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OPC COPPER NCA

High Deposition Rate Electroless Copper Plating Solution for MID Board OPC Copper NCA

2011.5.11

Research，Metal Finishing

OKUNO CHEMICAL INDUSTRIES CO., LTD. JAPAN

1 Feature of OPC Copper NCA

2 Bath Composition

3 Application, Control Method

?Application method, control method and analysis method of stabilizer 4 Performance Comparison with Build Copper

?Deposition rate, change in bath stability and appearance at continuous usage ? Evaluation of Resistance to Cr

?Influence on film appearance, deposition rate, stress and film properties 5 Quality Confirmation at Usage of Copper Chloride you provided

? Deposition rate, change in bath stability and appearance at continuous usage ? Summary

Content of Introduction for OPC Copper NCA

OPC ＣＯＰＰＥＲ NCA － Electroless Copper Plating Solution

1. Feature of OPC Copper NCA

OPC ＣＯＰＰＥＲ NCA － Electroless Copper Plating Solution

1. Feature of OPC Copper NCA

① Friendly to work environment Cyanide-free

e lectroless copper plating solution

② By simple analysis method, analysis control of

stabilizer is applicable.

③ High deposition rate

④ Good in bath stability

⑤ Stable film appearance and physical properties

2．Bath Composition of OPC Copper NCA

OPC ＣＯＰＰＥＲ NCA － Electroless Copper Plating Solution

2-1．Bath Composition

1 2 3 4 R-H R-N

Cu ○ - - ○ - -

HCHO - - - - ○ -

EDTA - ○ ○ - - -

NaOH - ○ ○ - - ○ Additives - - - ○ - -

OPC Copper NCA-1 (Cu 100.0 g/L)

Electroless Copper R-Ｎ (NaOH 240g/L)

Electroless Copper R-Ｈ (HCHO 340g/L)

○；Contain、－；Not contain

3．Application and Control Methods

of OPC Copper NCA

3-1．Application Method

Products Concentration

Replenishm

ent OPC Copper NCA　-1

OPC Copper NCA　-3

OPC Copper NCA　-4

10ml/L (Cu 1.0g)

3.7ml

0.4ml

(HCHO 240g/L containing)

（NaOH 340g/L containing)

25ｍｌ/L

250ml/L

4ml/L

9ml/L

Making-up

OPC Copper NCA　-1 OPC Copper NCA　-2 OPC Copper NCA　-3 OPC Copper NCA　-4 Electroless Copper R-H Electroless Copper R-H Electroless Copper R-N

OPC ＣＯＰＰＥＲ NCA － Electroless Copper Plating Solution

3-2. Control Method

※ Analysis and replenishment control by automatic

replenishment equipment

80 ～ 120 %

100%

Stabilizer Concentration

1.8 ～

2.6 g/L 2.2 g/L ※ Formaldehyde 6.0 ～ 8.0 g/L 7.0 g/L ※ Sodium Hydroxide 2.2 ～ 2.8 g/L 2.5 g/L ※ Copper Concentration Control Range Standard Item

OPC ＣＯＰＰＥＲ NCA － Electroless Copper Plating Solution

3-3. Analysis Control Method of Stabilizer

Used apparatuses, chemicals

① Spectrophotometer ② Separating funnel ③ 10ml whole pipette ④ Ethyl acetate 10ml

⑤100g/L NaCl solution 10ml ⑥ Using solution 10ml

After extraction [solvent is ethyl acetate] of stabilizer by separating funnel,

measured absorbancy at 281 nm by spectrophotometer.

Stabilizer Concentration （%）＝ Absorbancy × 555 + 5

Can analyze stabilizer concentration by simple method Analysis Method

Stabilizer Control Range

80%～120%

OPC ＣＯＰＰＥＲ NCA － Electroless Copper Plating Solution

In lacking of stabilizer by 10%, Replenish OPC Copper NCA-4 0.4ml/L

4．Performance Comparison

with Build Copper

4-1. Treatment Process for PC/ABS Co-injection Moldings

1.8g/L

K〔Au(CN)2〕

100ml/L Flash Gold 330B 15 min.

85℃

150ml/L Flash Gold 330A

Electroless Gold Plating

2 min.

↓ Water Rinsing

50ml/L

ICP Nicoron GM-NP-1E

15 min. 85℃

120ml/L ICP Nicoron GM-NP-ME Electroless Nickel Plating

2 min. ↓ Water Rinsing 1 min. 32℃

200ml/L

ICP Accera

Catalyzing 30 sec. 25℃ 100ml/L 35% Hydrochloric Acid

Pre-dipping 2 min. ↓ Water Rinsing 3 h. 60℃

OPC Copper NCA or Build Copper

Electroless Copper Plating

3 min. ↓ Water Rinsing 2ml/L

CR-200

5 min. 50℃

50ml/L 35% Hydrochloric Acid

Neutralization 3 min. ↓Dragging-out, Water Rinsing

4ml/L

Top Shut XO

180ml/L 98% Sulfuric Acid 20 min.

75℃

440g/L Chromic Anhydride

Etching

2 min.

↓Water Rinsing

20g/L

98% Sulfuric Acid

5 min. 50℃

10ml/L Top Placon GR Surface Conditioning Dipping Time

Bath Temp. Bath Composition at Making-up Fresh Bath

Steps

＜Treatment Condition ＞

? We measured plating film thickness on co-Injection molding by fluorescent X-ray analyzer.

? As dummy specimen, we used rolled copper sheet （0.5dm 2 /L ）.

4-2．Deposition Rate of OPC Copper NCA

Deposition Rate of OPC Coppe r NCA and Build Coppe r on Co-de position Moldings

2 4 6 8 10 12 14 16 18 20 0

60 120

180

Dipping Time (min.)

F i l m T h i c k n e s s 〔μm 〕

OPC Co ppe r NCA Bu ild Co ppe r

Deposition Rate

OPC Copper NCA

5.9μm/ｈ

Build Copper 5.3μm/ｈ

OPC Copper NCA has high deposition rate.

4-3. Bath Stability (Copper deposition on beaker bottom at continuous usage)

OPC Copper NCA

0MTO 5MTO 10MTO

No copper deposition on beaker→Good bath stability

Build Copper

0MTO 5MTO 10MTO

Copper deposited→Bath stability decreased

0MTO 5MTO 10MTO

OPC カッパーNCA Build Copper 〔Magnification : 100 times 〕

0MTO 5MTO 10MTO

OPC Copper NCA 〔Magnification : 100 times 〕

4-4．Film Appearance at Continuous Usage 〔after electroless copper plating 〕

No influence on plating appearance by usage

Confirmed nodule from 0 MTO and bright appearance

0MTO 5MTO 10MTO

OPC カッパーNCA

Build Copper

0MTO 5MTO 10MTO

OPC Copper NCA 4-5．Appearance Change at Continuous Usage 〔after electroless gold plating 〕

No appearance change by continuous usage

No appearance change by continuous usage (bright appearance)

Total replenishment

amount of OPC Copper NCA-4 at 10 MTO ： 10ml/L

Replenishment amount of OPC Copper NCA-4 per 1 MTO ： 1.0ml/L

（Equivalent to 25% as stabilizer）

4． Performance Comparison with Build Copper

?Evaluation of

Resistance to Cr

Cr in neutralizer (Add 500ppm Cr6+ to neutralizer)

0 0.2 0.4 0.6 0.8 1 1.2 200

400

600

800

1000

Wave Length 〔ｎｍ〕

A B S 4-6．Valence of Cr dragged-in to Electroless Copper

Cr3+　500ppm (CrCl3)

0 0.5 1 1.5 2 2.5 200

400 600

800 1000

Wave Length 〔ｎｍ〕

ＡＢＳ Cr6+　10ppm (CrO3)

0 0.5 1 1.5 2 200

400 600

800 1000

Wave Length 〔nm〕

A B S

Valence of Cr in Neutralizer

From absorbancy measurement result, we found that all Cr6+ dragged-in to neutralizer

bath was reduced to Cr3+.

All Cr dragged-in to electroless copper plating

bath is dragged-in as Cr3+. Has high correlation

576nm

409nm 577nm

416nm 354nm

OPC ＣＯＰＰＥＲ NCA － Electroless Copper Plating Solution

Neutralizer Composition CR-200 2ml/L 35%-HCl 50ml/L

0ppm 5ppm 10ppm 20ppm

OPC Copper NCA 〔Magnification : 100 times 〕

Build Copper 〔Magnification : 100 times 〕

0ppm 5ppm 10ppm 20ppm

4-7．Film Appearance 〔after electroless copper plating 〕

Brightness increased slightly. Less influence of Cr3+ dragging-in on appearance

According to increase in Cr3+ concentration, nodule increased and brightness increased widely.

4-8．Film Appearance 〔after electroless gold plating 〕

Build Copper

0ppm 5ppm 10ppm 20ppm

OPC Copper NCA

By dragging-in of Cr3, no formation of crack and stepping, brightness increased slightly

By dragging-in of Cr3, no formation of crack and stepping, brightness increased widely