NiClipse C. Ammonium chloride free

Transcription

1 NiClipse C NiClipse C is an acid zinc/nickel plating process that offers exceptional corrosion resistance, uniform alloy distribution and covering power, especially over cast substrates. NiClipse C deposits easily accept clear, yellow or black passivates. NiClipse C produces a fully bright deposit for rack or barrel applications. 1,000-3,000 hours to red rust in salt spray Uniform nickel content between 12 16% Produces ductile zinc nickel deposits Low temperature application Suitable for rack and barrel Can be full bright or semi-bright Ammonium chloride free PAVCO, Inc John Crosland Jr Drive Charlotte, NC Phone: Toll-free: or PAVCO INC ( ) Fax: Order Fax (for orders only)

2 2 Operating Parameters Rack: (12 16% Nickel alloy) Range Optimum Zinc: oz/gal (23-45 g/l) 3.7 oz/gal (28 g/l) Nickel: oz/gal (6 15 g/l) Not a control parameter Zinc to Nickel ratio: to to 1 Potassium chloride: oz/gal ( g/l) 37.4 oz/gal (280 g/l) Total chloride: oz/gal ( g/l) Not a control parameter Boric acid: oz/gal (18-25 g/l) 2.9 oz/gal (22 g/l) NiClipse C Starter 3-6 % 4 % NiClipse C 4-10% 6 % NiClipse C Brightener % 0.05% Temperature: F (22-30 C) 75 F (24 C) ph: Cathode current density: amps/ft 2 ( amps/dm 2 ) 20 amps/ft 2 (2.1 amps/dm 2 ) Anode current density, Zinc: amps/ ft 2 30 amps/ ft 2 ( amps/dm 2 ) (3.2 amps/dm 2 ) Operating Parameters Barrel: (12-16% Nickel alloy) Range Optimum Zinc: oz/gal (24-55 g/l) 4.7 oz/gal (35 g/l) Nickel: oz/gal (6-15 g/l) Not a control parameter Zinc to Nickel ratio to to 1 Potassium chloride: oz/gal ( g/l) 37.4 oz/gal (280 g/l) Total chloride: oz/gal ( g/l) Not a control parameter Boric acid: oz/gal (18-25 g/l) 2.9 oz/gal (22 g/l) NiClipse C Starter 3-6 % 4 % NiClipse C 4-10% 6 % NiClipse C Brightener % 0.05% Temperature: F (22-30 C) 75 F (24 C) ph: Cathode Current Density amps/ft amps/dm 2 Anode current density, Zinc amps/ ft 2 ( amps/dm 2 ) 5 amps/ft amps/dm 2 30 amps/ ft 2 (3.2 amps/dm 2 )

3 3 Maintenance of the Solution: NiClipse C NiClipse C Starter NiClipse C Brightener Consumption method/control Lost mainly by drag-out, add approximately 1 gal per 41# KCl (1L per 5 kg KCl) Lost mainly by drag out. Add approximately 1 gal per 61# KCl (1 L per 7.3 kg KCl) Electrolysis- rate depends on brightness requirement Typical feed rate (Rack) Typical feed rate (Barrel) 189 mls per KAH 380 mls per KAH 1 gal per 20 KAH 1 gal per 10 KAH 190 mls per KAH 283 mls per KAH 1 gal per 20 KAH 1 gal per 13 KAH mls per KAH mls per KAH 1 gal per KAH 1 gal per KAH Zn By Analysis (page 6) Controlled by rectification Ni By Analysis (page 7) Controlled by rectification Equipment: Tank: Anodes: Anode Baskets: Anode Bags: Anode Hooks: Anode Bars: Filtration: Rectifier: A polypropylene, PVC, or Koroseal lined tank is required. Anodes should be a mix of zinc slab anodes with sulfur free nickel chips. Use 4 zinc slabs per nickel basket. Zinc balls are NOT recommended and will cause failures. Titanium baskets are used for nickel chips. Avoid use of anode bags through adequate filtration. If anode bags are used, leach in 1% NiClipse C Starter overnight. Use polypro bags. Do not use hooks. Zinc slab anodes should be bolted directly to anode rail. Titanium baskets should be bolted to anode rail. Use copper anode bars, shielded with plastic or nickel plated. Use a 5-10 micron cartridge or plate filter. Filtration rate should be a minimum of 3 tank turnovers per hour. 3-5 tank turnovers per hour is recommended. Dual rectification is required for the NiClipse C system. Separate rectification, bussing, anode bars and anodes must be in place for the zinc and nickel anodes. Zinc anodes should be placed on a removable rail to facilitate removal from the tank during downtime. Nickel anodes do not require removal. The ratio of current to anodes should be approximately 4:1 zinc to nickel. Use up to 12 volts for rack, 15 volts for barrel. Temperature Control: Agitation: Exhaust: Salt Mixing Tank: Consistent temperature is necessary in order to maintain a constant alloy in the deposit. Automatic temperature control is mandatory to +/- 2 F (1 C). Titanium or PTFE is recommended. Uniform air agitation is mandatory for rack operations. Air supply must be free of oil. Supplement with cathode rod agitation at ft/min ( m/min). Recommended. Allows for quick dissolution of all salt and easy addition during continuous operation. Separate pump from filter pump. Pump intake should be at ½ solution height to minimize solids damage. A heating coil in this tank is good practice. The recommended volume is gallons.

4 4 Rack Bath Make Up 1,000 Gallons (3,785 L): 1. Prepare a lined tank by leaching it with 5% hydrochloric acid for a period of hours. 2. Rinse the tank clean with water. 3. Fill the lined tank with 600 gallons (2271L) of water. 4. Add 487 pounds (221 kilograms) of anhydrous zinc chloride and mix well. For liquid zinc chloride, use 51 gallons (194 L) of 62.5% liquid zinc chloride. 5. Add 253 pounds (115 kilograms) of nickel chloride (hexahydrate) and mix well. For liquid nickel chloride, use 42 gallons (160 L ). 6. Add 90% of the required boric acid. For 1,000 gallons, add 165 pounds (75 kilograms) of boric acid and mix well. 7. Add 90% of the required potassium chloride. For 1,000 gallons, add 2142 pounds (972 kilograms) of potassium chloride and mix well. 8. Add 40 gallons (151 L) of NiClipse C Starter and 60 gallons (227 L) NiClipse C. Mix well. 9. Heat the bath at F (32-38 C) for faster dissolution. 10. Analyze the bath chemistry. Additions of boric acid and potassium chloride will be required at this point. 11. Adjust the ph to 5.4 with hydrochloric acid. It takes about 1.5% hydrochloric acid to adjust ph. Allow solution to mix 8 hours to equilibrate and form the proper nickel complex. Re-adjust ph after 8 hours and let the solution to cool down. 12. Hang zinc and nickel anodes in the bath. 13. Add water to the final working level, mix thoroughly, and analyze the bath. Make adjustments if necessary. Add 0.5 gallon (1.9 liter) NiClipse C Brightener before plating. v Liquid zinc chloride at 62.5% contains 9.45 #/gal of zinc chloride (1134 g/l). v Liquid nickel chloride contains 6#/gal of nickel chloride (720 g/l). Barrel Bath Make Up 1,000 Gallons (3,785 L): 1. Prepare a lined tank by leaching it with 5% hydrochloric acid for a period of hours. 2. Rinse the tank clean with water. 3. Fill the lined tank with 600 gallons (2271L) of water. 4. Add 610 pounds (277 kilograms) of anhydrous zinc chloride and mix well. For liquid zinc chloride, use 64 gallons (243L) of 62.5% liquid zinc chloride. 5. Add 320 pounds (145 kilograms) of nickel chloride (hexahydrate) and mix well. For liquid nickel chloride, use 54 gallons (202L) 6. Add 90% of the required boric acid. For 1,000 gallons, add 165 pounds (75 kilograms) of boric acid and mix well. 7. Add 90% of the required potassium chloride. For 1,000 gallons, add 2142 pounds (972 kilograms) of potassium chloride and mix well. 8. Add 40 gallons (151 L) of NiClipse C Starter and 60 gallons (227 L) NiClipse C. Mix well. 9. Heat the bath at F (32-38 C) for faster dissolution. 10. Analyze the bath chemistry. Additions of boric acid and potassium chloride will be required at this point. 11. Adjust the ph to 5.4 with hydrochloric acid. It takes about 1.5% hydrochloric acid to adjust ph. Allow solution to mix 8 hours to equilibrate and form the proper nickel complex. Re-adjust ph after

5 5 8 hours and let the solution to cool down. 12. Hang zinc and nickel anodes in the bath. 13. Add water to the final working level, mix thoroughly, and analyze the bath. Make adjustments if necessary. Add 0.5 gallon (1.9 liter) NiClipse C Brightener before plating. v Liquid zinc chloride at 62.5% contains 9.45 #/gal of zinc chloride (1134 g/l). v Liquid nickel chloride contains 6#/gal of nickel chloride (720 g/l). NiClipse C Operating Tips: CRITICAL: Successful operation of this process requires the ability to determine the nickel composition of the alloy deposit. You must have X-Ray Fluorescence analytical capability and it needs to be set up for analysis of zinc nickel thickness and composition. Standards for zinc nickel alloy with varying thickness and composition are required. 30 second measurements are recommended. Consistent temperature control is critical. Alloy composition will fluctuate with temperature. Temperature must be maintained within +/- 2 F (1 C). Separate coils for heating and cooling may be needed. Bright finishes are best obtained at 12-16% nickel alloy. If alloy composition is incorrect, check and adjust chemistry first. Alloy composition will fluctuate with agitation. Increased agitation will suppress nickel deposition. To obtain uniform alloy and brightness in rack operation, uniform agitation is mandatory. Due to the high chloride levels in the bath, it is recommended that the solution be continuously agitated and temperature must be maintained above 68 F (20 C) at all times. This will prevent crystallization of salts in the tank blocking the air sparger. If crystallization does occur, turn air off and temporarily raise temperature to 110 F (43 C) to aid in clearing air lines. Operation at recommended temperature (75 F/24 C) provides optimal low current density (LCD) performance in both rack and barrel applications. Exceeding recommended temperature will cause LCD darkness. Each 1 oz/gal (7.5 g/l) nickel requires about 3% NiClipse C. Low will cause poor alloy uniformity. NiClipse C Booster may be added to improve LCD coverage in baths with higher metal concentrations. Use up to 1 %, as excess NiClipse C Booster will increase stress in the deposit and could generate blistering. Nickel and total chlorides are not controlled parameters, use Zinc to Nickel ratio and potassium chloride instead respectively. Single rectification can be used in barrel operations with sufficient dragout to prevent zinc metal growth. In these cases, liquid nickel chloride is fed by amp-hour dosing. Consult your Pavco representative to determine if this may fit your application.

6 6 Analysis Procedures: Zinc Analysis: Reagents 1. Eriochrome Black T indicator M EDTA solution 3. ph 10 Buffer solution To make this solution: a. Add mls of ammonium hydroxide to a 1 liter volumetric flask. b. Add 70 g of ammonium chloride to the flask. c. Bring to volume with de-ionized water and mix well. 4. 1M KCN solution To make this solution: a. Add 65 g of potassium cyanide to a 1 liter volumetric flask b. Bring to volume with de-ionized water and mix well. 5. 8% formaldehyde Procedure 1. Pipette a 2 ml sample of the bath into a 250 ml Erlenmeyer flask. 2. Add 100 mls of de-ionized water 3. Add 10 mls of KCN solution, 10 mls of buffer solution and 15 mls of 8% formaldehyde. 4. Add ~ 0.1g of Eriochrome Black T indicator and titrate with 0.1M EDTA solution to a light blue endpoint. Calculations Zn g/l = mls of EDTA x 3.27 Zn oz/gal = Zn g/l x 0.13 Boric acid: Equipment 150 ml beaker 5 ml pipette Reagents De-ionized water Dilute sulfuric acid 1N sodium hydroxide Mannitol Procedure Note: Make sure all the boric acid is in solution before proceeding with this analysis. Heat the sample to put all the boric acid in solution. 1. Pipette a 5 ml bath sample into a 150ml beaker and add 20ml of D.I. water. Add a Teflon coated magnetic stir bar and mix solution on stir plate throughout procedure. 2. Using a ph meter, adjust ph of solution to , using either sodium hydroxide or Sulfuric acid. Record final ph. 3. Add 2g mannitol. (Excess mannitol is necessary at all times.) 4. Slowly titrate the solution with 1N sodium hydroxide until original ph is reached. Calculation oz/gal H 3BO 3 = mls NaOH x 1.82 Nickel Analysis: by AA method Consult your Pavco representative for the recommended procedure.

7 7 Total Chloride Analysis: Equipment ml Erlenmeyer flask 2. 1 ml pipette Reagents 1. De-Ionized water 2. Dextrin/Calcium carbonate buffer (mixed 1to1 by weight) 3. Dichlorofluorescein indicator N silver nitrate solution Procedure 1. Pipette a 1 ml sample of the bath into a 250 ml Erlenmeyer flask. 2. Add approx. 50 mls of de-ionized water. 3. Add one scoop - approx. 2 grams of buffer. 4. Add 0.5 ml of dichlorofluorescein indicator. 5. Swirl the flask to mix thoroughly. 6. Titrate the solution with N silver nitrate until the color changes from yellow to pink. 7. Record the titration. Calculation Total chlorides in oz/gal = mls silver nitrate x Zn metal X = oz/gal chloride in zinc chloride = A Ni metal X = oz/gal chloride in nickel chloride = B Analyze for NiClipse C with the procedure below. NiClipse C = C Potassium chloride in oz/gal = [total chloride - (A+B+C * 0.21+C * 0.20)] X 2.1 Alternative analysis procedure to calculate potassium chloride is available. Please contact Pavco Technical Department Determination of NiClipse C Reagents 1. 30% Potassium Iodide Solution 2. 10% Sulfuric Acid 3. Copper Sulfate 5-hydrate solution (50g/L) N Sodium Thiosulfate 5. Starch Solution Procedure 1. Pipet 5 mls bath sample into a 100ml beaker. 2. Add 20 mls of the copper sulfate 5-hydrate solution. 3. Raise the ph to 11 using 50% NaOH, and stir for 10 minutes. 4. Filter the solution through # 41 filter paper into a 500 ml Erlenmeyer flask and rinse the filter paper thoroughly (until you have 200 mls in the flask). 5. Add 10ml 10% sulfuric acid and 20ml 30% potassium iodide solution. 6. Add 1 ml starch indicator. Titrate with 0.1N sodium thiosulfate to a milky-white endpoint. 7. Use the graph and calculation to determine the % of NiClipse C. Calculation: % NiClipse C = (mls thiosulfate X.68)

8 8 Hull Cell Testing: A 2 Amp, 5 minute, air agitated (steel) hull cell is recommended for rack applications. A 1 Amp, 10 minute cathode rod agitated panel is recommended for barrel applications. It may be necessary to plate panels for minutes in order to get sufficient thickness in low current density areas, for a more accurate alloy reading by XRF. A 2 amp, 10 minute, air agitated (steel) Toshi cell is recommended to measure covering power. Troubleshooting Chart: Problem Cause Possible Solution Low Nickel alloy Low ph Increase to 5.4 using NiClipse C in 0.2% increments. Low nickel, high Zn:Ni ratio Low temperature Excessive agitation High zinc Increase current through nickel anodes. Add nickel anodes or liquid nickel chloride. Raise temperature. Reduce air. Review anode distribution. Reduce current in Zn anodes if possible. Dilute bath. High Nickel alloy High temperature Reduce temperature. High Nickel, low Zn:Ni ratio Dull Deposit Low Nickel Analyze and adjust. Low NiClipse C Brightener Low Potassium chloride Reduce current through nickel anodes to adjust ratio, add zinc chloride or liquid zinc chloride. Adjust with 0.025% increments of NiClipse C Brightener. Adjust concentration, it will increase Ni alloy in the deposit.

9 9 Organic contamination Low NiClipse C Starter Carbon treatment. Adjust with 0.2% increments of NiClipse C Starter. Dark Low CD Copper, lead > 5 ppm Check by AA, dummy at 1-2 ASF to remove. High temperature Low NiClipse C Starter Low NiClipse C Reduce temperature and raise nickel or increase ph to maintain alloy. Add 0.5% increments of NiClipse C Starter. Adjust concentration. Burning Low boric acid Analyze and adjust. Low temperature Low zinc level Adjust temperature to the proper range. Analyze and adjust zinc & nickel. High ph Reduce ph to 5.6. Low NiClipse C Poor Agitation Excessive plating current High NiClipse C Booster Test and adjust. Improve air flow or uniformity. Reduce current density. Stop adds, check concentration and adjust with increments of 0.5%. Poor LCD coverage High temperature Reduce and maintain temperature at 75F. Low chloride High Zinc Poor anode contact Low NiClipse C Booster Excessive agitation Poor preparation or rework Electrical problems High NiClipse C Starter, low NiClipse C Raise chloride. Cut solution to reduce Zinc. Correct anode contact (use tong testers to confirm contact). Add NiClipse C Booster in 0.2% increments. Reduce agitation. Check preparation. Check connections. Zinc metal growth High temperature Lower temperature. Low ph Maintain at 5.6. Increase NiClipse C by 1% increments. Non-uniform alloy ph out of range Check and adjust ph to 5.6. Low NiClipse C Low NiClipse C Starter Non-uniform agitation Poor temperature control Add NiClipse C in 1% increments. Add 0.5% increments of NiClipse C Starter. Check and clean air sparger. Redesign sparger if needed. Hazy at MCD Low Potassium chloride Analyze and adjust. Blistering Low NiClipse C Analyze and adjust. Check cooling system and ensure sufficient solution agitation.

10 10 High nickel alloy High NiClipse C Brightener High NiClipse C Booster Check all bath parameters and adjust. Plate out excess brightener. Stop adds, increase NiClipse C with 0.5% increments. Roughness Particulates in solutions Inspect filtration and improve as needed. Add or change anode bags. Waste Treatment: Dispose of the concentrate or solutions thereof according to local waste treatment regulations. Safety: Handling Pavco mandates that the following safety equipment be used when handling chemicals in an electroplating environment: safety glasses, face shield, plastic or rubber apron, rubber gloves and safety shoes. Chemicals should only be handled by trained and experienced personnel. Storage Store Pavco products in a clean, well ventilated room which temperature remains above 45 F (7 C). Pavco products should remain in their original container with the lid or cap tightened. Drum pumps or pails must be clean prior to dispensing Pavco products to prevent contamination. If any NiClipse C product freezes during shipment or storage, warm the product and mix it well before use. Emergency Procedures - Refer to the MSDS for detailed emergency procedures. Eye Contact Seek immediate medical attention. Flush the eyes with water for 15 minutes. Skin Contact Remove all contaminated clothing. Wash the skin with soap and water. Seek medical attention. Inhalation Remove the person to an area with fresh air. Seek medical attention if necessary. Ingestion Seek immediate medical attention. Spill Dike the area to contain the spill. Refer to the MSDS for clean-up. Notify the proper authorities if required. *NOTE: Refer to the MSDS for detailed emergency medical procedures. Product Description & Shipping: NiClipse C Starter (ZN5005) is a brown liquid with a specific gravity between 1.0 and 1.1 and a ph less than 7.5. NiClipse C (ZN5010) is a colorless to slightly yellow liquid with a specific gravity between 1.0 and 1.1 and a ph greater than 8.5 NiClipse C Brightener (ZN5015R) is a clear colorless liquid with a specific gravity between 0.98 and 1.03 and a ph less than 6.5. NiClipse C Booster (ZN5035) is a pale yellow liquid with a specific gravity between 1.10 and 1.20 and a ph less than 9.5. All NiClipse C products are available in 5 gallon containers or 55 gallon drums. Revision Date: 05/09/2017 WARRANTY AND DISCLAIMER Technical information and recommendations contained herein are believed to be reliable, however, the accuracy or completeness thereof is not guaranteed. No statement or recommendation shall constitute a representation unless set forth in an agreement in writing by the seller and manufacturer. NO WARRANTY OR MERCHANTABILITY OR WARRANTY OF FITNESS FOR A PARTICULAR PURPOSE IS MADE. The following warranty is made in lieu of any other warranties, express, implied, or statutory. Products are warranted to be free from defects on material and workmanship at the time sold. The sole obligation of the seller and manufacturer under this warranty shall be to replace any product defective at the time sold. Under no circumstances shall the manufacturer or seller be liable for any loss, damage, expense, direct or consequential, arising out of the use of or inability to use the product. Materials shall not be returned to the seller or manufacturer without express written permission. No information or suggestions given by us shall be deemed to be a recommendation to use any product in conflict with any existing patent rights.