Pretreatment of iron-based substrates for electroless plating

Patent metadata

Field	Value
Publication number	US-10577692-B2
Application number	US-201715398809-A
Country	US
Kind code	B2
Filing date	Jan 5, 2017
Priority date	Jan 5, 2017
Publication date	Mar 3, 2020
Grant date	Mar 3, 2020

Abstract

A method of electrolessly plating an iron-based substrate, including immersing an iron-based substrate in an acidic solution, immersing the iron-based substrate in a basic complexing solution, immersing the iron-based substrate in a catalytic metal solution including a catalytic metal, and immersing the iron-based substrate in an electroless nickel plating solution or an electroless cobalt plating solution.

First claim

What is claimed is:

1. A method of electrolessly plating a cast iron substrate, comprising:
immersing the cast iron substrate in an acidic solution;
immersing the cast iron substrate subsequently in a basic complexing solution containing sodium potassium tartrate (KNaC 4 H 4 O 6 ) or sodium citrate (Na 3 C 6 H 5 O 7 ) having a concentration in the range of about 30 g/L to about 100 g/L that prevents reformation of oxides on the surface of the substrate after immersing the cast iron substrate in the acidic solution;
immersing the cast iron substrate directly in a catalytic metal solution including a catalytic metal without rinsing the cast iron substrate after immersing the cast iron substrate in the basic complexing solution; and
immersing the cast iron substrate subsequently in an electroless nickel plating solution or an electroless cobalt plating solution.

2. The method of claim 1 , wherein the acidic solution is a hydrochloric acid solution.

3. The method of claim 2 , wherein the hydrochloric acid solution has a concentration in the range of about 5% to about 20% by weight hydrochloric acid.

4. The method of claim 3 , wherein the hydrochloric acid solution is a 10% hydrochloric acid solution by weight.

5. The method of claim 1 , wherein the basic complexing solution is a potassium sodium tartrate solution or sodium citrate solution with a pH in the range of above 7 to about 9.

6. The method of claim 5 , further comprising maintaining the pH of the potassium sodium tartrate solution or sodium citrate solution at a pH of about 8 with a 2 molar sodium hydroxide solution or a hydrochloric acid solution to prevent re-oxidation.

7. The method of claim 1 , wherein the catalytic metal is palladium.

8. The method of claim 7 , wherein the catalytic metal solution contains 55 ppm Pd from dissolved PdSO 4 and a sulfuric acid solution.

9. The method of claim 1 , further comprising rinsing the cast iron substrate with deionized water after immersion in the catalytic metal solution.

10. The method of claim 1 , wherein the electroless nickel plating solution is used and includes a hydrated nickel sulfate salt, and sodium hypophosphite (NaH 2 PO 2 ), dimethylamine borane (DMAB), or sodium borohydride (NaBH 4 ).

11. A method of nickel plating a cast iron substrate, comprising:
immersing the cast iron substrate, wherein the cast iron substrate does not form a protective oxide coating, in a 10% by weight hydrochloric acidic solution;
immersing the cast iron substrate subsequently in a basic complexing solution containing sodium potassium tartrate (KNaC 4 H 4 O 6 ) or sodium citrate (Na 3 C 6 H 5 O 7 ) with a pH of about 8 and having a concentration in the range of about 30 g/L to about 100 g/L of the sodium potassium tartrate or sodium citrate for about 5 minutes to about 10 minutes that prevents reformation of oxides on the surface of and—the substrate after immersing the cast iron substrate in the acidic solution—is inserted in its place;
immersing the cast iron substrate subsequently in a catalytic metal solution including dissolved PdSO 4 and a sulfuric acid solution without rinsing the cast iron substrate after immersing the cast iron substrate in the basic complexing solution, wherein the catalytic metal solution forms up to a monolayer of palladium on the cast iron substrate surface; and
immersing the cast iron substrate subsequently in an electroless nickel plating solution prepared using a nickel sulfate salt and sodium hypophosphite (NaH 2 PO 2 ).

12. The method of claim 11 , further comprising subsequently rinsing the cast iron substrate in deionized water after immersion in the catalytic metal solution.

13. The method of claim 12 , wherein the cast iron substrate is immersed in the electroless nickel plating solution for about 1 hour, where the electroless nickel plating solution is maintained at a temperature of about 95° C. for the 1 hour.

14. The method of claim 11 , wherein the cast iron substrate is immersed in the catalytic metal solution for a duration of about 2 minutes.

15. The method of claim 11 , wherein the cast iron substrate is immersed in the 10% by weight hydrochloric acidic solution for a duration of about 5 minutes.

16. A method of nickel plating a cast iron substrate, comprising:
immersing an cast iron substrate in a 10% by weight hydrochloric acidic solution, wherein the cast iron substrate does not form a protective oxide coating;
immersing the cast iron substrate subsequently in a potassium sodium tartrate solution with a pH of about 8 and a concentration in the range of about 30 g/L to about 100 g/L of the potassium sodium tartrate;
immersing the cast iron substrate subsequently directly in a catalytic metal solution including about 25 ppm to about 75 ppm Pd from dissolved PdSO 4 and a sulfuric acid solution without rinsing the cast iron substrate after immersing the cast iron substrate in the potassium sodium tartrate solution, wherein the catalytic metal solution forms up to a monolayer of palladium directly on the cast iron substrate surface without using a nickel strike coating or silver as the catalytic metal; and
immersing the cast iron substrate in subsequently an electroless nickel plating solution at a temperature in the range of about 20° C. to about 95° C., where the electroless nickel plating solution is prepared using a hydrated nickel sulfate salt (NiSO 4 ) and sodium hypophosphite (NaH 2 PO 2 ), dimethylamine borane (DMAB), or sodium borohydride (NaBH 4 ).

17. The method of claim 16 , further comprising rinsing the cast iron substrate with deionized water after immersion in the catalytic metal solution and before immersing the cast iron substrate in an electroless nickel plating solution.

18. The method of claim 16 , wherein nickel plating is formed on the cast iron substrate by the electroless nickel plating solution, and the nickel plating has a phosphorus content of about 1 weight % to about 20 weight %.

19. The method of claim 18 , further comprising heat treating the nickel plating.

Assignees

• IBM

Inventors

• Dimilia Doreen D
• Luo Yu
• Nowak Janusz J
• Romankiw Lubomyr T

Classifications

• C23C18/1844

  with use of organic or inorganic compounds other than metals, first · CPC title

• C23C18/168

  Control of temperature, e.g. temperature of bath, substrate · CPC title

• C23C18/34 Primary

  using reducing agents · CPC title

• C23C18/36

  using hypophosphites · CPC title

• C23C18/1637

  metallic substrate · CPC title