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DIPSOL OF AMERICA, INC. TECHNICAL DATA SHEET

DIPSOL IZA-2500 Ammonia Free Acid Zinc Nickel Alloy Plating for Rack Application

TDS IZA-2500 (REVISION V).DOC

Rev. , 4/10/2017

DIPSOL OF AMERICA, INC. TECHNICAL DATA SHEET

Contents 1.1 SCOPE OF APPLICATION 1.2 PRODUCT FEATURES 1.3 CHEMICAL PROPERTIES 1.4 OPERATING INSTRUCTIONS 1.5 MAKE UP AND MAINTENANCE 1.6 ANALYSIS METHOD AND PROCEDURE 1.7 SUPPLIMENTAL DATA 1.8 HULL CELL 1.9 WASTE TREATMENT 1.10 SPECIAL HANDLING INSTRUCTIONS

1 1 1 2 4 9 10 17 17 18

The information presented herein was prepared by technically knowledgeable personnel, and to the best of our knowledge, is true and accurate. It is not intended to be all-inclusive, and the manner and conditions of use and handling may involve other or additional considerations. All previous revisions are obsolete.

TDS IZA-2500 (REVISION V).DOC

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DIPSOL OF AMERICA, INC. TECHNICAL DATA SHEET

1.1 SCOPE OF APPLICATION DIPSOL IZA-2500 is the latest advanced high Acid Zinc Nickel technology that does not contain boron or ammonia. It is a chloride-based plating process, for rack application that provides consistent 12-18% nickel in the deposit. The deposit from DIPSOL IZA-2500 has excellent adhesion, bending and corrosion resistance properties that exceed the requirement of the automotive industry. It has excellent thickness distribution for fasteners and casting applications.

1.2 PRODUCT FEATURES DIPSOL IZA-2500 system offers the following features: • • • • • • • • •

• •

Ammonia and boron free Provides four to five times the corrosion resistance in salt spray test compared to zinc deposits. Easy to control solution. Two rectification system is preferred but the bath can be controlled with one rectifier. Low foaming Has excellent adhesion and corrosion resistance in high temperature applications. Accepts different types of chromate conversion coatings (clear, iridescent and black), which can be easily applied to enhance appearance and corrosion resistance. Silver appearance with brightness Deposit consists of 12-18% nickel 2 In standard solution, plating speed is approximately 0.30-0.45 µm/min at 1.5 A/dm (9.3 ASF) in the cathode current density area. Hardness of deposit is HV250-350 in the Vickers Hardness scale. DIPSOL IZA-2500 has superior covering power and throwing power and provides excellent corrosion resistance on many complicated-shaped parts.

1.3 CHEMICAL PROPERTIES Name of Product Component IZA-2500 A IZA-2500 B IZA-2500 C IZA-2500 D

Utilization Purpose Carrier solution for make-up and replenishment Brightener solution for make-up and replenishment Complexor solution for make- up and replenishment Buffering liquid for make-up and replenishment

TDS IZA-2500 (REVISION V).DOC

Physical Properties

Specific Gravity (25ºC)

Light Yellow/Yellow Liquid

1.02

Clear/Light yellow Liquid

0.99

Clear/Light Yellow Liquid

1.07

Clear Colorless Liquid

1.20

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DIPSOL OF AMERICA, INC. TECHNICAL DATA SHEET

1.4 OPERATING INSTRUCTIONS 1.4.1 Standard Operating Process Soak

Water Rinse

→

Water Rinse

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→

Water Rinse

Water Rinse

Water Rinse

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→

→

Water Rinse

Electroclean

DIPSOL IZA-2500

→

Electroclean

→

Water Rinse

→

→

→

→

Water Rinse

Water Rinse

→

→

Water Rinse

Water Rinse

Trivalent Chromate

Water Rinse

→

→

Water Rinse

Water Rinse

→

→

Activation

Acid Pickling

→

→

Water Rinse

→

Activation

→

Water Rinse

→

Dryer

1.4.2 Operating Conditions Optimum

Range

pH

5.4

5.2-5.6

Zn/Ni Ratio

1.6

1.5-1.7

Temperature

35 C º (95 F)

Cathode Current Density

1.5 A/dm (13.9 ASF)

Anode Current Density

4 A/dm and above (37.0 ASF and above)

º

º

30 – 40 C º (86 - 104 F) 2

2

2

0.5 – 2.0 A/dm (4.6 – 18.5 ASF) 2

4 A/dm and above (37.0 ASF and above)

Anodes*

Sulfur-free nickel and zinc metal anodes

Filtration

Continuous filtration is necessary (2-3 turnovers/hr).

* Note: Initially use Ni:Zn anode ratio at 2:1 and adjust later based on solution chemistry.

TDS IZA-2500 (REVISION V).DOC

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→

Water Rinse

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DIPSOL OF AMERICA, INC. TECHNICAL DATA SHEET 1.4.3 Equipment Item

Contents

Tank

Steel lined with PVC, Polyethylene. Rubber lined tank is not recommended.

Exhaust

Should be well-ventilated.

Filter

The filter should have the capacity to turn over plating solution at least 2-3 times per hour. Micron size is (10-20) microns

Thermo Controller

Maintain solution temperature between 30 - 40˚C (86 – 104˚F).

Anodes

Sulfur and Carbon Free Nickel anodes with Zinc slabs. Steel anodes cannot be used.

Anode Bag

Anode bags are recommended. Material: Saran 205 or 701

Rectifier

12-15 V, 3 phase full wave rectifier is usually satisfactory. Capacity should hold the total quantity of plating solution. Similar material to process tank.

Spare Tank Cathode Rocker & Air agitation

Necessary for solution agitation

Eductor

To maintain metal concentration in entire plating solution

1.4.4 Standard Operating Parameters Make-up

Acid Zn-Ni Alloy Plating

Component

Concentration

ZnCl2 NiCl2•6H2O KCl IZA-2500A

73.0 g/L (9.7 oz/gal) 89.0 g/L (11.9 oz/gal) 160 g/L (21.4 oz/gal) 30 ml/L 1.0 ml/L

IZA-2500B

Tank Material Basket

35ºC (30-40) 95ºF (86-104)

(Not Required for Matte Application)

IZA-2500C IZA-2500D Agitation Filtration Dryer

Temperature

10 ml/L 225 ml/L Required Continuous filtration, 2-3 turnovers/hour

80ºC (80-120ºC) for 20 minutes (minimum 5 minutes) 176ºF (176-248ºF) Plating Bath

Steel lined with PVC, Polyethylene. Rubber lined tank is not recommended.

PP or PVC coated stainless steel basket is recommended (Barrel)

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DIPSOL OF AMERICA, INC. TECHNICAL DATA SHEET

1.5 MAKE UP AND MAINTENANCE 1.5.1 Make-Up Make-up of the solution should be done according to the following procedure using city water. When using well water or industrial water, please contact DIPSOL OF AMERICA in advance. DIPSOL IZA-2500 A. Fill plating tank 35% of its capacity with water and dissolve the necessary quantity of zinc chloride, nickel chloride, and potassium chloride. If it is necessary to do a carbon treatment at this point, please adjust pH to 5.5-5.7 using hydrochloric acid and thoroughly dissolve the added components. B. Add the required amount of IZA-2500D and mix well. C. Fill plating tank to 90% of its final capacity with water and mix we well for 20min. D. Perform carbon treatment (active carbon 0.5-1g/L) for 24 hours and zinc dust treatment (0.5-1.og/L) for 2-4 hours. Both carbon and zinc dust treatment can be done together. E. Add the required amount of IZA-2500C, IZA-2500A and IZA-2500B and mix well. F. Fill bath to final volume with city water and mix well. G. Adjust pH by using hydrochloric acid or sodium hydroxide and mix well. H. Take a 500 mL sample of the well-mixed solution to perform hull cell testing to confirm bath is operating optimally.

1.5.2 Solution Composition

Zinc Nickel

*1

Chlorides IZA-2500A IZA-2500B IZA-2500C IZA-2500D

Optimum 35.0 g/L (4.6 oz/gal) 22.0 g/L (2.9 oz/gal) 140 g/L (18.7 oz/gal) 30.0 ml/L 1.0 ml/L 10 ml/L 225 ml/L

Range 30-40 g/L (4.0-5.3 oz/gal) 17-27 g/L (2.3-3.6 oz/gal) 130-170 g/L (17.4-22.7 oz/gal) 20-40 ml/L 0.5-1.5 ml/L 7.5-12.5 ml/L 140-240 ml/L

Note: *1. For DIPSOL IZB-256Y, a higher nickel deposit is recommended to get a darker appearance. Low nickel in the deposit may cause iridescence.

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DIPSOL OF AMERICA, INC. TECHNICAL DATA SHEET 1.5.3 Maintenance The plating solution should be maintained by periodic analysis of Zn, Ni, and Total Chlorides, as well as through Hull Cell testing.

1.5.3.1 IZA-2500A (Carrier Solution)* DIPSOL IZA-2500A is a carrier solution used for make-up and replenishment and should be replenished at a rate of 200 mL/KAH.

1.5.3.2 IZA-2500B (Brightener)* DIPSOL IZA-2500B is a brightener solution used for make-up and replenishment and should be replenished at a rate of 375 ml/KAH.

1.5.3.3 IZA-2500C (Complexor)* DIPSOL IZA-2500C is a complexor solution used for make-up and replenishment and should be replenished at a rate of 60 ml/KAH.

1.5.3.4 IZA-2500D (Buffering Salt)* DIPSOL IZA-2500D is a buffering salt solution used for make-up and replenishment and should be replenished at a rate of 270 ml/L KAH. *Note: These components are to be adjusted according to amounts lost to drag-out.

1.5.3.5 Bath Temperature o

º

Maintaining the bath temperature at 35 C (95 F) is very important to produce good parts. During cold weather months, if the bath temperature gets colder you might see crystallization in the plating solution, o raising the bath temperature to 35 C will dissolve back the crystalize.

1.5.3.6 Anode Current Density A. One Rectifier 2 Set anode current density to be higher than 4A/dm Zn and Ni anode surface ratio should be Zn:Ni=1:4 This ratio is a guideline. Please adjust the number of anodes in order to be able to maintain Zn and Ni concentration within the recommended range. B. Two Rectifiers There isn’t a specific anode current density. Place the anodes in a way the parts won’t have thickness distribution issues. The current ration between Zn anode and Ni anode should be 7:3-6:4. The Zn anodes need to be out of the plating solution when the bath is in idle state. The following are some examples of negative effects from leaving the Zn anodes in the tank. 1. Zn anode dissolves in the bath. Zn concentration rises in the bath. 2. Raise Voltage Ni ion in the bath substitutes on to the Zn anodes and passivates the surface of Zn anodes. Using passiveted anodes will raise the voltage and the results of it may cause the appropriate current to not be applied. 3. Breaks down brightener component (Dipsol IZA-2500B) in the bath and creates appearance (dullness) issue. 4. Raise pH in the bath. Need to adjust pH with diluted HCl

TDS IZA-2500 (REVISION V).DOC

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DIPSOL OF AMERICA, INC. TECHNICAL DATA SHEET Example of One Rectifier System

Example of Wrong Set Up

TDS IZA-2500 (REVISION V).DOC

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DIPSOL OF AMERICA, INC. TECHNICAL DATA SHEET Example of Two Rectifier System

TDS IZA-2500 (REVISION V).DOC

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DIPSOL OF AMERICA, INC. TECHNICAL DATA SHEET 1.5.3.7 Impurities, Effect, and Countermeasure Impurity

Limit (mg/L)

Total Chromium Ion

4

Pb

0.5

Cu

20

Fe

200

Co

4

Organics

-

Effect Reduce in Brightness Excess Brightness in HCD area Appearance Issue on LCD area Adhesion Issue • Decrease in Corrosion Performance • Darkness in LCD • Reduced Covering Power Adhesion Issue Low Ni Alloy Reduce in Brightness • Reduced Brightness • Pitting, Haziness • Roughness • Reduce Bendability

Countermeasure • Zinc Dust Treatment • Dummy Plate • •

Zinc Dust Treatment Dummy Plate

• Zinc Dust Treatment • Dummy Plate Increase Drag Out Dummy Plate Carbon Treatment

Dummy Plating 2 2 Anode current density should be above 4A/dm and cathode current density should be 0.5-2A/dm Zinc and Carbon Treatment 2 Apply on filter (per 1m of filter) 1000g of Zn Dust 500g of carbon for 2-4 hours or add 0.3-0.6g/L of Zinc or carbon into the plating tank and circulate for 2-4hours and filter to remove it

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DIPSOL OF AMERICA, INC. TECHNICAL DATA SHEET

1.6 ANALYSIS METHOD AND PROCEDURE Sample Preparation: Pipette 10ml of plating solution into a 100ml volumetric flask. (Solution A) If precipitation appears please add 2-3 drops of sulfuric acid. (Only for Zn and Ni analysis)

1.6.1 Zinc and Nickel Metal Analysis A. B. C. D. E. F. G. H. I.

Pipette 10 mL of solution A into a 250 mL Erlenmeyer flask. Fill the flask with 100 mL of deionized water. Add 15-20 mL of pH 10 buffer solution to the flask. Add Murexide indicator and mix well to dissolve. Titrate using 0.1 M EDTA until the color turns violet. Record the volume of EDTA used as (a). Prepare a clean 250ml Erlenmeyer flask and pipette 10ml of solution A into it. Fill the flask with 50ml of deionized water. Add 15-20ml of pH 10 buffer solution to the flask Add 15ml of 0.1M EDTA and add 2ml of 10% 2,3-Dimercapto-1-propanol (To make 10% 2,3-Dimercapto-1-propanol, add 10g of 2,3-Dimercapto-1-propanol into 100ml of ethanol.) J. Add Eriochrome Black T indicator K. Titrate using 0.05mol/L MgCl2 solution until the color turns reddish purple. Record the volume of MgCl2 used as (b).

Calculation: Y= ((b) /2)-(15-(a)) Zinc (g/L)= Y x 6.54 Zinc (oz/gal)= Y x 0.87 Nickel (g/L)= 5.87 x ((a)-Y) Nickel (oz/gal)=0.78 x((a)-Y)

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DIPSOL OF AMERICA, INC. TECHNICAL DATA SHEET 1.6.2 Total Chloride Analysis A. B. C. D.

Pipette 2 mL of solution A into a 250 mL Erlenmeyer flask. Fill the flask with 25 mL of deionized water. Add 2 mL of sodium chromate indicator to the flask. The solution should be yellow. Titrate with 0.1 M silver nitrate until the color turns brick red. Record the volume of silver nitric used as (c).

Calculation: Total Chlorides (g/L)= (c) x 17.8 or Total Chlorides (oz/gal)= (c) x 2.38

1.7 SUPPLIMENTAL DATA 1.7.1 Effect of Zn

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DIPSOL OF AMERICA, INC. TECHNICAL DATA SHEET 1.7.2 Effect of Ni

1.7.3 Effect of Total Chloride

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DIPSOL OF AMERICA, INC. TECHNICAL DATA SHEET 1.7.4 Effect of pH

1.7.5 Effect of Bath Temperature

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DIPSOL OF AMERICA, INC. TECHNICAL DATA SHEET 1.7.6 Effect of IZA-2500A

1.7.7 Effect of IZA-2500B

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DIPSOL OF AMERICA, INC. TECHNICAL DATA SHEET 1.7.8 Effect of IZA-2500C

1.7.9 Effect of IZA-2500D

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DIPSOL OF AMERICA, INC. TECHNICAL DATA SHEET

1.7.10 Parameter Variation: Effect on Performance Category

Brightness

Plating Speed

Adhesion

Bendability

Ni Alloy

Covering Power

Burning

Skip Plating

Ni (Optimal 22g/L)

Zn (Optimal 35g/L)

High

Low

Changing of Zinc concentration has a strong effect on the deposit appearance and its Ni deposition. When Zinc concentration increase by 5g/L, Ni co-deposition goes down from 14% to 13%. When Ni codeposition goes down, the brightness of LCD goes down. On the other hand, when Zinc concentration decrease by 5g/L, Ni co-deposition goes up from 14% to15%. One of the key factors of operating this bath is to control the Zinc concentration. High Low

Fluctuating Nickel concentration by 5g/L won’t show a big effect on appearance, plating speed, and Ni codeposition. Higher Ni (above 17%) will show Ni stain on LCD area.

Total Chloride (Optimal 140g/L)

High Low

The chloride concentration will strongly influence the appearance and Nickel co-deposition. Increasing the chloride by 5g/L will change Ni co-deposition from 14% to 15%. On the other hand, when the chloride concentration goes down by 5g/L, Ni co-deposition will go down from 14% to 13%. Lowering the Ni codeposition will reduce brightness on LCD area.

Bath Temp. o (Optimal 35 C)

PH (Optimal 5.4)

High Low

Change of pH will have a strong effect on appearance, plating speed, and Ni co-deposition. When pH goes up by 0.1, Ni co-deposition goes down from14% to 13% and thickness will go up by 5%. Lowering pH by 0.1, will increase Ni co-deposition from 14% to 15% and thickness will be reduced by 5%. High Low o

Bath temp. has a strong effect on Ni co-deposition. When the temp. goes up by 5 C, Ni co-deposition goes o up from 14% to 15%. When the bath temp. goes down by 5 C, Ni co-deposition goes down from 14% to 13%.

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IZA-2500B (Optimal 1.0ml/L)

IZA-2500A (Optimal 30ml/L)

DIPSOL OF AMERICA, INC. TECHNICAL DATA SHEET High

Low

There isn’t a direct correlation with the concentration of IZA-2500A against appearance, plating speed, and Ni co-deposition. When the concentration drops below 10ml/L, covering power will reduce, and the brightness will reduce on the HCD area . High Low

Adding IZA-2500B will brighten up the HCD area. When the concentration of the brightener becomes below 0.2ml/L, the appearance will become dull (gray appearance). The concentration of IZA-2500B doesn’t directly have an effect on the plating speed and Ni co-deposition. High amount of IZA-2500B in the bath (above 2ml/L) will reduce the bendability of the deposit.

IZA-2500C (Optimal 10ml/L)

High Low

The concentration of IZA-2500C has a strong influence on appearance and Nickel co-deposition. When IZA-2500C concentration goes down by 5ml/L, Ni co-deposition is reduced from 14% to 12%. When Ni codeposition gets lower, the brightness of LCD is reduced. Increasing IZA-2500C concentration by 5ml/L, Ni co-deposition goes up from 14% to 15.5%. IZA-2500C helps to improve ductility so for those parts that require ductility, there is an option to set optimal concentration to 15ml/L.

IZA-2500D (Optimal 225ml/L)

High Low

Fluctuation of IZA-2500D concentration has a strong effect on appearance, plating speed, and Ni codeposition. When the concentration goes down by 40ml/L, Ni co-deposition drops from 14% to 13%. On the other hand, when concentration goes up by 40ml/L, Ni co-deposition goes up from 14% to 15%. When the concentration of IZA-2500D is low, Ni co-deposition on the HCD area drops and nickel hydroxide will deposit on the HCD area.

TDS IZA-2500 (REVISION V).DOC

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DIPSOL OF AMERICA, INC. TECHNICAL DATA SHEET

1.8 HULL CELL The hull cell is taken under the following condition. o Long Hull Cell, Zn or Ni anodes, 1A- 10min at 35 C Solution agitation with magnetic stirrer at 700 rpm Hull Cell Appearance without IZA-2500B

Hull Cell Appearance with IZA-2500B

Thickness (um) Ni Alloy (%)

2cm from HCD Edge

5 cm from HCD Edge

5.5-7.0 14.0-15.5

2.0-3.0 14.5-16.5

1.9 WASTE TREATMENT Neutralization of the solution is necessary to adhere to acceptable local standard for effluent pH may be required. DIPSOL IZA-2500 process is free of chromates, cyanides, fluorides, and phenolic compounds. All surface active agents are biodegradable. Removal of metallic hydroxides may be required.

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DIPSOL OF AMERICA, INC. TECHNICAL DATA SHEET

1.10 SPECIAL HANDLING INSTRUCTIONS Wear protective gloves and goggles when handling these products. In case of contact with solution, immediately flush skin with plenty of water. Store products in a cool, dry place in a sealed container, due to their hygroscopic properties. The use, handling, and storage of this product may involve certain hazards. Please refer to the Safety Data Sheet for additional hazard information.

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