ZINC PLATING SYSTEMS NH4 Zn/Co
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1 Zinc Plating Systems is an acid zinc cobalt electroplating process which produces a zinc alloy containing % (by weight) cobalt. Deposits from the process provide corrosion resistance unmatched by conventional zinc deposits. is characterized by ease of control, consistent day-to-day operation, extreme high temperature tolerance, and good chromate receptivity. Mirror bright finish Excellent corrosion resistance Temperature tolerance up to 120 F (49 C) Excellent chromate receptivity Ease of plating bath control Excellent adhesion and ductility Pavco Inc John Crosland Jr. Dr. Charlotte, NC Phone Fax Toll Free
2 Pavco Page 2 Operating Parameters Barrel Operation Zinc: Potassium chloride: Ammonium chloride: Range oz/gal g/l oz/gal g/l 4-8 oz/gal g/l Cobalt oz/gal g/l Current Density: 1-15 amps/ft 2 Rack Operation Zinc: Potassium chloride: Ammonium chloride: Cobalt amps/dm oz/gal g/l oz/gal g/l 4-8 oz/gal g/l oz/gal g/l Current Density: 1-80 amps/ft amps/dm 2 Optimum 3 oz/gal 22.5 g/l 18 oz/gal 130 g/l 6 oz/gal 45 g/l 0.4 oz/gal 3 g/l 3.5 oz/gal 26 g/l 18 oz/gal 130 g/l 6 oz/gal 18 g/l Zn - Co Starter NH 4 2-6% 4 % 0.4 oz/gal 3 g/l ZCL BRT II % 0.2% ZCL Zn/Co ESP 0.5-3% 1% ph: Temperature: F C Anode to Cathode Area: 1:1 minimum 90 F 32 C
3 Pavco Page 3 Equipment Tank: A polypropylene, PVC, or Koroseal lined tank is required. Anodes: Use Special High Grade (SHG 99.99% pure) zinc balls or slabs Anode Baskets: Titanium baskets are required. Keep the baskets filled with zinc anodes all the time and not to exceed 9 volts on the rectifier. Anode Bags: Nylon or polypropylene bags are required for rack operations. Anode S-Hooks: Nickel plated S-hooks. Anode Bars: Use copper anode bars, preferably shielded with plastic. Filtration: Use a 5-15 micron cartridge packed with a non - cellulose filter aid or activated carbon. Filtration speed should be at least 1 tank turnover per hour. Sand filters have been found to work quite satisfactorily. Rectifier: Up to 12 volts Temperature: The is tolerant to temperatures ranging from F (18 49 C). Control: A titanium heat exchanger is recommended for heating. Ventilation: Recommended Agitation: Air agitation is mandatory for rack operations. Optional Equipment Automatic ph controller Automatic brightener feeder Automatic temperature control
4 Pavco Page 4 Maintenance of the Solution Zinc Potassium Chloride By analysis By drag-out & analysis Ammonium Chloride By drag-out & analysis Starter ZCL BRT II By drag-out & analysis 1 gal / 20,000 30,000 amp hrs (1 l / 5,000 8,000 amp hrs) Bath Makeup per 1000 gallons (3785 l) 1. Prepare a lined tank by leaching it with 5% hydrochloric acid for hours. 2. Rinse the tank 3. Fill the lined tank with 500 gallons (2000 liters) of water. 4. Add 45 gallons (170 liters) of 62.5% liquid zinc chloride and mix well to dissolve. 5. Add 375 pounds (170 kg) of ammonium chloride and mix well to dissolve. 6. Add 1125 pounds (510 kg) of potassium chloride and mix well to dissolve. 7. Add 90 pounds of cobalt chloride (40 kg) and mix well to dissolve 8. Hang slab anodes or zinc filled titanium anode baskets in the bath. 9. Add 40 gallons of Zn - Co Starter NH Add 0.5 gallons of ZCL BRT II 11. Add 10 gallons of Smart Zn/Co ESP 12. Add warm water to the 1000 gallon (3785 l) level. Analytical Procedures Zinc Reagents 1. Acetate Buffer -To makeup, dissolve: a)180 grams of sodium acetate b) 30 ml of acetic acid c) Add de-ionized water to make one liter 2. Xylenol Orange Indicator-To make this indicator liquid: a) One gram of Xylenol Orange b) Dissolved in 1 liter of de-ionized water M EDTA Solution Procedure 1. Into a 400 ml beaker pipette a 5 ml bath sample. CAUTION: Fumes are poisonous if using this method with a cyanide bath. 2. Add 150 mls de-ionized water. 3. Add 50 ml acetate buffer. 4. Add indicator 5. Titrate with 0.1 M EDTA until the color changes from red to yellow Calculation: ml of titration.176 = zinc in oz/gal ml of titration 1.32 = zinc in g/l
5 Pavco Page 5 Analytical Procedures Cont d Total Chloride - Free Chloride Reagents 1. Buffer (Mix dextrin and calcium carbonate in a 1:1 ratio) 2. Chloride Indicator Dissolve: a) 0.2 g of Dichlorofluorescein b) 70 mls of methyl alcohol c) De-ionized water to make 100 mls N silver nitrate solution Procedure 1. Pipette a 1 ml sample of zinc chloride plating bath into a 250 ml Erlenmeyer Flask 2. Add 100 mls of de-ionized water. 3. Add one scoop, approximately 2g, of buffer. 4. Add 1 ml of indicator 5. Titrate with 0.153N silver nitrate until the color changes from yellow to pink Calculation 1. mls of Silver Nitrate x = oz/gal total chloride (A) A x 7.49 = g/l total chloride (Am) 2. Zinc in oz/gal x = oz/gal chloride associated with the zinc metal (B) B x 7.49 = g/l chloride associated with the zinc metal (Bm) 3. A - B = oz/gal free chloride (C) Am - Bm = g/l free chloride (Cm) Iron Test and Treatment per 1,000 gallons (3785 l) Procedure 1. Into a 100 ml beaker add 30 ml of clear bath sample (if the sample is not clear, filter it). 2. Add 1 ml of 3.5% hydrogen peroxide 3. Determine the concentration of the iron in the bath by the intensity of the color change. No change - no iron Slight precipitate - moderate iron Heavy precipitate - high iron 4. If the test indicates moderate or high iron, or if barrel spots are present, treat the bath for iron as follows: Dilute one pint (500 ml) of 35% or 50% hydrogen peroxide to 1 gallon (3.785 L) with water. Mix this diluted peroxide throughout the plating bath. Repeat steps 1 to 4 until the majority of the iron is precipitated. Filter out the precipitated iron..cobalt Analysis 1 Analyze the cobalt in the bath via atomic absorption. Use the procedure as provided by your AA supplier. 2. The cobalt in the bath should measure in the range of 1,500-3,000 ppm. This correlates to.2-.4 oz/gal ( g/l) cobalt in the bath Calculation: ppm Co/7,500= Cobalt in oz/gal ppm Co/ 1,000= Cobalt in g/l
6 Pavco Page 6 Normal Panel Normal Low Current Density Problem High ph Low total chloride Low ZCL BRT II High Current Density Problem Black Burn Gray Low Zinc, Low Ammonium chloride, High ph, Low Zn - Co Starter NH 4, Low temperature Chromium Contamination Blister Chromium contamination Skip Control Panel Hull Cell Panel Observe From Left to Right Area 1 High Current Density Area 2 Mid Current Density Area 3 Low Current Density Metal Contamination Problem Blackish Discoloration Metallic Contamination (either copper or cadmium) of the plating bath or the bright dip ener Problem Low ZCL BRT II Semi High and Low Current Density Problem Frost Low Zn - Co Starter NH 4 Low ZCL BRT II Gray
7 Pavco Page 7 Iron Problem Black Discoloration High Iron (Black color shows up after the bright dip or chromate) Pavco, Inc. s Hull Cell Scale 1 AMPS. 2 AMPS. 3 AMPS. 5 AMPS. TOTAL CURRENT 3 AMPS. 5 AMPS. PANEL EDGE GM./1000 ML. 7.8 ML./1000 ML. AMPS./SQ. FT. 267 ML. OR 534 ML. HULL CELL OR 267 ml Hull Cell Agitation Mechanical or Air Temperature 90 F, 32 C Current & Time 2 amps/5 minutes 2 GM/267 ML. HULL CELL = 1 OZ./GAL. = 6.25 LBS./100 GAL. 2 ML./267 ML. HULL CELL = 0.96 FL. OZ./GAL. = 6 PTS./100 GAL. 4 GM. 534 ML. HULL CELL = 1 OZ./GAL. = 6.25 LBS./100 GAL. 4 ML./534 ML. HULL CELL = 0.96 FL. OZ./GAL. = 6 PTS./100 GAL. CU. FT. X 7.48 = GAL. GM/L X = OZ./GAL. OZ./GAL. X 7.5 = GM/LITER GAL. X 3785 = ML. A/SQ. FT. X = A/SQ. DM. PANEL AMPS./SQ. FT ML. HULL CELL
8 Pavco Page 8 Trouble Shooting Chart Problem Cause Solution High current density burn Low zinc level Add zinc chloride High current density area bright-dips black, or barrel work exhibits Low current density are dull or hazy Poor low current density coverage High current Low ammonium chloride Low temperature Reduce current Add ammonium chloride Raise temperature High iron High ph Low total chloride Treat for iron with diluted hydrogen peroxide Reduce ph Add potassium or ammonium chloride Metallic or organic contamination High ph Low chloride Treat with zinc dust or carbon Reduce ph Add Potassium or Ammonium Chloride Low/High ZCL BRT II Metallic contamination High zinc level (>6oz/gal or 45 g/l) Excess peroxide added Organic contamination Check BRT II level in hull cell Treat with zinc dust Dilute the bath Electrolyze bath Treat with carbon
9 Pavco Page 9 Trouble Shooting Chart Cont d Problem Cause Solution Low current density area bright dips black Metallic contamination Treat with zinc dust Overall Haze Low ZCL BRT II Inadequate agitation Poor cleaning Work rusting before plating Poor bright dip Blue bright chromate out of balance or contaminated Temperature too high Add ZCL BRT II Increase agitation Improve cleaning Acidify rinses Remake bright dip; try HCl instead of nitric acid Remake chromate Decrease temperature Overall Dullness Low ZCL BRT II Metallic contamination High temperature temperature too high ph too low Organic contamination Add ZCL BRT II Treat with zinc dust Decrease temperature decrease temperature Raise ph Treat with carbon Slow Plating Speed Low zinc level Add zinc chloride Low chloride level Add potassium or ammonium chloride Weak pickle or pickling problem Low temperature Low current Smut formation in pickling Add more hydrochloric acid to the pickle or make a new pickle Raise temperature Increase current Add PavPrep to the pickle
10 Pavco Page 10 Trouble Shooting Chart Cont d Problem Cause Solution Roughness Inadequate filtration Improve filtration Low anode area Increase anode area Particles from anodes Bag the anodes Current too high Lower the current Blistering Poor cleaning &/or pickling Improve pre-treatment Organic contamination Treat with carbon Metallic contamination Treat with zinc dust Chromium contamination Treat with peroxide High current Lower current High ZCL BRT II Hold ZCL BRT II Flaking or star dusting High ZCL BRT II Hold ZCL BRT II Current interruption Check all contacts High current Lower current High ph Reduce ph
11 Pavco Page 11 Waste Treatment Dispose of the concentrates 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 Smart Zn/Co Starter or BRT freeze 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 m 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. Product Description & Shipping Zn - Co Starter NH 4 (CO650) is a clear amber liquid. The specific gravity is between 1.0 and 1.1 with a ph of greater than 8 ZCL BRT II (ZB 710) is a clear liquid. The specific gravity is between 1.0 and 1.1 with a ph less than 6. Both products are available in in 5 gallon containers, 55 gallon drums, or 275 gallon totes Revision Date: 11/9/09 Revision Number: 6 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.
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