NIPOSIT PM-980 W Semi-Bright Electroless Nickel Process For Industrial Finishing Applications

Transcription

1 Technical Data Sheet NIPOSIT PM-980 W Semi-Bright Electroless Nickel Process For Industrial Finishing Applications Regional Product Availability Description North America The NIPOSIT PM-980 W process is specifically formulated to autocatalytically deposit semi-bright nickel, 4 5% phosphorous alloys from an alkaline solution. The NIPOSIT PM-980 W process deposits an adherent coating on properly-prepared plastic substrates that serve as a base for subsequent electrolytic plating. The resulting deposit will exhibit excellent bond strength, with a finish reproducing the base surface finish, and is capable of withstanding high electroplating current density without burn-off. Advantages Lead-free, cadmium-free formulation ELV and RoHS compliant Extremely long solution life Self ph regulating Exceptional chemical stability High tolerance to metallic contamination Low temperature process Fine grained, pit-free deposits Deposit Properties Phosphorous Content (wt %): 4 5 Density (g/cm 3 ): 7.9 Applicable Specifications: ASTM B-733, Mil-C-26074E and AMS 2404A Bath Make-Up Chemicals Required Metric (U.S.) Deionized water ml/l (80.0% v/v) NIPOSIT PM ml/l (14.5% v/v) Ammonium hydroxide ~ 30 ml/ (~3.0 % v/v) (SG 0.88) Make-Up Procedure 1. Add deionized water to process tank. 2. Add NIPOSIT PM-980 and mix thoroughly. 3. Dilute to volume with deionized water. 4. Start pump(s) and allow solution to recirculate for 15 minutes. 5. Analyze nickel content and adjust to 3.4 g/l (0.45 oz./gal.) with NIPOSIT PM Measure ph and adjust to 9.0 using 500 ml/l (50%) ammonium hydroxide or 100 ml/l (10%) sulfuric acid. Note: Sodium hypophosphite concentration upon bath make-up is normally higher than a working solution. The sodium hypophosphite will decrease over time to the recommended concentration. Page 1 of 8 NIPOSIT TM PM-980 W / Interconnect Technologies September 2014

2 Bath Operation Bath Operation Metric Parameter Range Recommended Nickel Metal g/l 3.4 g/l Sodium Hypophosphite g/l 22 g/l Temperature C 30 C ph Loading Factor dm 2 /l 1.0 dm 2 /l Agitation Mild air agitation and mechanical part agitation are recommended Deposition Rate Dependent upon time and temperature Bath Operation U.S. Parameter Range Recommended Nickel Metal oz./gal oz./gal. Sodium Hypophosphite oz./gal. 2.9 oz./gal. Temperature F 85 F ph Loading Factor ft. 2 /gal. 0.4 ft. 2 /gal. Agitation Mild air agitation and mechanical part agitation are recommended Deposition Rate Dependent upon time and temperature Bath Maintenance Nickel Metal To ensure correct operation of the NIPOSIT PM-980 electroless nickel plating bath, the solution concentration should be maintained between 95 and 100% activity. Nickel metal is maintained using NIPOSIT PM-80 A. 1.5 ml/l (0.15% v/v) NIPOSIT PM-980 A will raise the nickel metal concentration by 0.2 g/l (0.027 oz./gal.). Percent activity is normally determined by measuring the nickel metal concentration in accordance with the following procedure. I. Equipment a) 10 ml Class A volumetric pipette b) 250 Erlenmeyer flask c) 25 ml and 100 ml graduated cylinder d) 50 ml burette e) Laboratory spatula f) Mortar and pestle II. III. Reagents a) Murexide indicator in a mortar, add 5g Murexide to 100g NaCl; pestle to mix thoroughly b) Concentrated ammonium hydroxide Titrant EDTA Solution, M Page 2 of 8 NIPOSIT TM PM-980 W / Interconnect Technologies September 2014

3 Bath Maintenance (cont d) IV. Procedure a) Cool a sample of working solution to C (59 77 F). b) Pipette 10 ml of solution into a 250 ml Erlenmeyer flask. c) Add 100 ml of deionized water. d) Add 15 ml of ammonium hydroxide. e) Add two spatula tips (about 0.2 g) of murexide indicator. The solution color should change to a yellow brown. Excess indicator can obscure the endpoint. f) Titrate immediately with M EDTA until the solution changes to a deep blue violet endpoint. V. Calculation Nickel Metal g/l = ml Titrant x Molarity of Titrant x Nickel Metal oz./gal. = ml Titrant x Molartity of Titrant x Sodium Hypophosphite Sodium hypophosphite is maintained by additions of NIPOSIT PM-980 B according to nickel metal analysis. A daily analytical check of the sodium hypophosphite concentration should be made using the method described in the analytical procedure below. 1.5 ml/l (0.15% v/v) NIPOSIT PM-980 B will raise the sodium hypophosphite concentration by 1.2 g/l (0.16 oz/gal). I. Equipment a) 250 ml glass-s stoppered iodine flask b) 5 ml Class A transfer pipette c) 50 ml Class A transfer pipette d) 25 ml graduated cylinder e) 50 ml burette II. III. IV. Reagents a) Iodine solution, 0.1N (0.05M) b) Standard starch indicator, 1% c) Hydrochloric acid solution, 50% v/v Titrant Sodium thiosulfate solution, 0.1N (0.1M) Procedure a) Cool a sample of working solution to C (59 77 F). b) Pipette a 5.0 ml sample of the cooled electroless nickel working solution into a 250 ml iodine flask. c) Add 30 ml of 50% hydrochloric acid (must be room temperature) to the flask. d) Pipette 50.0 ml of 0.1N iodine solution into the flask. Immediately stopper the flask and pour water around the stopper to seal. Place flask in a dark place for 30 ±1 minutes between C (65 75 F). Page 3 of 8 NIPOSIT TM PM-980 W / Interconnect Technologies September 2014

4 Bath Maintenance (cont d) e) Titrate with 0.1N sodium thiosulfate solution until a pale yellow color is observed. f) Add approximately 2 ml of starch indicator. The solution color must turn blue upon addition of starch. If the solution is colorless, the sample has been over titrated and the procedure must be repeated. g) Continue to titrate with sodium thiosulfate to a colorless endpoint. Note: The endpoint appears slowly so care must be taken to avoid over-titration. V. Calculation Sodium Hypophosphite g/l = [(50 x Normality of Iodine) - (ml Titrant x Normality)] x Sodium Hypophosphite oz./gal. = [(50 x Normality of Iodine) - (ml Titrant x Normality)] x 1.41 ph The ph of the NIPOSIT PM-980 W solution should be maintained between 8.5 and 9.5. The ph measurements should always be made at room temperature. To raise the ph of the solution, add a 500 ml/l (50% v/v) solution of reagent grade ammonium hydroxide. To lower the ph, add a 100 ml/l (10% v/v) solution of reagent grade sulfuric acid. Use extreme caution when mixing and handling sulfuric acid solutions, as the reaction is exothermic (heat producing). Always add acid to water and mix thoroughly during addition. Allow this mixture to cool to room temperature before making additions to the plating solution. When making ph adjustments at operating temperature, add small, frequent amounts of ph adjuster over the entire solution surface area. IMPORTANT! To maintain bath stability over a weekend or extended shutdown, adjust the ph to approximately 9.0 with ammonium hydroxide at the end of the last working day. Bath Temperature Loading Factor Operating temperature of the electroless nickel solution should be maintained at C (75 95 F). Temperatures below 24 C (75 F) will result in an impractically slow plating rate while temperatures above 35 C (95 F) may result in accelerated tank plateout and/or decomposition of certain bath constituents. If the solution is maintained at operating temperature during extended periods when no work is being processed, thermal decomposition of the reducing agent may occur, resulting in excessive consumption of chemicals and an unnecessary loss in economy of operation. The workload to solution volume ratio (loading factor) of the NIPOSIT PM-980 W process should be maintained between dm 2 /liter ( ft 2 /gal.). The process has been designed to tolerate large variations in loading factor; however, continual underloading (<0.25 dm 2 /liter, 0.1 ft 2 /gal.) will result in low plating rates and eventual overstabilization while overloading (>2.5 dm 2 /liter, 0.5 ft 2 /gal.) will cause low initial plating rates and may lead to instability of the process. Recommended Control Schedule Analysis of Procedure Frequency Nickel Metal Volumetric Daily Sodium Hypophosphite Volumetric Daily ph Electrometric Hourly Temperature Hourly Metallic Contamination Atomic Absorption As Required Page 4 of 8 NIPOSIT TM PM-980 W / Interconnect Technologies September 2014

5 Replenishment Schedule Nickel Metal (100 liter bath) % Activity Nickel Concentration NIPOSIT PM-980 A NIPOSIT PM-980 B NIPOSIT PM-980 W 105% 3.6 g/l None None None 100% 3.4 g/l None None None 95% 3.2 g/l 0.15 liters 0.15 liters 0.07 liters 90% 3.0 g/l 0.30 liters 0.30 liters 0.14 liters 85% 2.8 g/l 0.45 liters 0.45 liters 0.21 liters 80% 2.6 g/l 0.60 liters 0.60 liters 0.28 liters 75% 2.4 g/l 0.75 liters 0.75 liters 0.35 liters Replenishment Schedule Nickel Metal (100 gallon bath) % Activity Nickel Concentration NIPOSIT PM-980 A NIPOSIT PM-980 B NIPOSIT PM-980 W 105% 0.48 oz./gal. None None None 100% 0.45 oz./gal. None None None 95% 0.43 oz./gal. 0.6 quarts 0.6 quarts 0.28 quarts 90% 0.40 oz./gal. 1.2 quarts 1.2 quarts 0.56 quarts 85% 0.37 oz./gal. 1.8 quarts 1.8 quarts 0.84 quarts 80% 0.35 oz./gal. 2.4 quarts 2.4 quarts 1.12 quarts 75% 0.32 oz./gal. 3.0 quarts 3.0 quarts 1.40 quarts Replenishment Usually it is sufficient to make the standard additions of NIPOSIT PM-980 A, B and W to hold nickel and sodium hypophosphite in the working range. If an extra addition of sodium hypophosphite is required, then use the tables below for the recommended addition. Replenishment Schedule Sodium Hypophosphite (100 liter bath) % Activity Sodium Hypophosphite Concentration NIPOSIT PM-980 B 105% 23.0 g/l None 100% 22.0 g/l None 95% 21.0 g/l liters 90% 20.0 g/l liters 85% 19.0 g/l liters 80% 18.0 g/l liters 75% 17.0 g/l liters Replenishment Schedule Sodium Hypophosphite (100 gallon bath) % Activity Sodium Hypophosphite Concentration NIPOSIT PM-980 B 105% 3.07 oz./gal. None 100% 2.93 oz./gal. None 95% 2.80 oz./gal. 0.5 quarts 90% 2.67 oz./gal. 1.0 quarts 85% 2.53 oz./gal. 1.5 quarts 80% 2.40 oz./gal. 2.0 quarts 75% 2.26 oz./gal. 2.5 quarts Page 5 of 8 NIPOSIT TM PM-980 W / Interconnect Technologies September 2014

6 Replenishment (cont d) 1. NIPOSIT PM-980 W should be maintained according to the nickel metals analysis. Replenishment should be according to the schedule tables above. 2. Analyze at the bath working volume only. 3. Add NIPOSIT PM-980 A, B and W slowly with vigorous agitation. 4. Never add replenishers to the bath directly over heaters or parts being processed. 5. Do not make additions of more than 20% v/v (ca 0.7 g/l Ni) at one time. If a larger addition is required, add the replenishers in increments of 10% v/v while plating work in the solution. Failure to observe this procedure may result in an overstabilized solution, producing skip-plate or edge pullback on processed parts. Equipment Tanks: Suitable heat-resistant, stress-relieved natural polypropylene or 316 stainless steel (17/11/2.5 Cr-Ni-Mo stainless) with anodic protection. Heaters: Racks: Filtration: Agitation: Exhaust: Immersion heaters (PVDF clad panel or anodically protected stainless steel) or external stainless steel steam heat exchangers may be used. Temperature controllers with ±1 C capability should be employed. Stainless steel or plastic coated. Continuous solution filtration is essential. All filtration system components which contact the plating solution should be constructed of heat-resistant plastic. For filtration, 3 10 micron woven polypropylene cartridges or filter bags with a flow rate of three times tank volume per hour are preferred. Soak the cartridge or bags well before use to remove any residual release agents. Mechanical agitation. Lip extraction recommended. All process tanks should be equipped with an exhaust system to remove spray and steam. Process tanks should be covered when not in use to avoid contamination and evaporation losses. Equipment Preparation I. Tanks and Ancillary Equipment Prior to makeup, the process tank and ancillary equipment should be thoroughly stripped and conditioned according to the procedure outlined below. II. III. Stripping Solution Nitric Acid: 300 ml/l (30% v/v) Conditioning Solution Ammonium Hydroxide: 20 ml/l (2% v/v) Page 6 of 8 NIPOSIT TM PM-980 W / Interconnect Technologies September 2014

7 Equipment Preparation (cont d) IV. Procedure a) Transfer any remaining spent electroless nickel solution to a separate holding tank. b) Remove filter. Thoroughly wash down the process tank and ancillary equipment with tap water. Circulate water through filtration system. Any residual plating solution remaining in the tank will shorten the life and effectiveness of the stripping solution. c) Discard water. d) Add stripping solution to the process tank. Recirculate through pump(s) and filtration system for approximately 3 hours. e) Allow the stripping solution to remain in the tank overnight, or until all metallic nickel has been stripped and heaters and pump(s) have been re-passivated. f) Transfer the stripping solution into an appropriate holding tank. g) Thoroughly rinse process tank with tap water. Circulate water through the filtration system. h) Discard water. i) Insert filter. Add conditioning solution to the process tank and recirculate through pump(s) and filtration system for approximately 30 minutes. j) Check ph of conditioning solution. If the ph is less than 7.0, add additional ammonium hydroxide and continue recirculation. Repeat procedure until conditioning solution ph is greater than 7.0. k) Discard conditioning solution. l) Thoroughly rinse process tank, all pump(s) and the filtration system with tap water. m) Discard water. n) As a final rinse, use deionized water as above. Note: Appropriate safety equipment must be worn during the entire procedure Product Data Associated Products For the specific Product Data values, please refer to the Certificate of Analysis provided with the shipments of the products(s). NIPOSIT PM-980 NIPOSIT PM-980 A NIPOSIT PM-980 B NIPOSIT PM-980 W Page 7 of 8 NIPOSIT TM PM-980 W / Interconnect Technologies September 2014

8 Handling Precautions Before using this product, associated generic chemicals or the analytical reagents required for its control, consult the supplier's Material Safety Data Sheet (MSDS)/Safety Data Sheet (SDS) for details on material hazards, recommended handling precautions and product storage. CAUTION! Keep combustible and/or flammable products and their vapors away from heat, sparks, flames and other sources of ignition including static discharge. Processing or operating at temperatures near or above product flashpoint may pose a fire hazard. Use appropriate grounding and bonding techniques to manage static discharge hazards. CAUTION! Failure to maintain proper volume level when using immersion heaters can expose tank and solution to excessive heat resulting in a possible combustion hazard, particularly when plastic tanks are used. Storage Disposal Considerations Store products in tightly closed original containers at temperatures recommended on the product label. Dispose in accordance with all local, state (provincial) and federal regulations. Empty containers may contain hazardous residues. This material and its container must be disposed in a safe and legal manner. It is the user's responsibility to verify that treatment and disposal procedures comply with local, state (provincial) and federal regulations. Contact your Dow Electronic Materials Technical Representative for more information. Product Stewardship Customer Notice Dow has a fundamental concern for all who make, distribute, and use its products, and for the environment in which we live. This concern is the basis for our product stewardship philosophy by which we assess the safety, health, and environmental information on our products and then take appropriate steps to protect employee and public health and our environment. The success of our product stewardship program rests with each and every individual involved with Dow products - from the initial concept and research, to manufacture, use, sale, disposal, and recycle of each product. Dow strongly encourages its customers to review both their manufacturing processes and their applications of Dow products from the standpoint of human health and environmental quality to ensure that Dow products are not used in ways for which they are not intended or tested. Dow personnel are available to answer your questions and to provide reasonable technical support. Dow product literature, including safety data sheets, should be consulted prior to use of Dow products. Current safety data sheets are available from Dow. For Industrial Use Only. This information is based on our experience and is, to the best of our knowledge, true and accurate. However, since conditions for use and handling of products are beyond our control, we make no guarantee or warranty, expressed or implied, regarding the information, the use, handling, storage or possession of the products, or the applications of any process described herein or the results sought to be obtained. Nothing herein shall be construed as a recommendation to use any product in violation of any patent rights. Contact: North America: Taiwan: China: (+86) Hong Kong: (+852) Korea: (+82) Japan: (+81) Europe: (+41)(0) NOTICE: No freedom from infringement of any patent owned by Dow or others is to be inferred. Because use conditions and applicable laws may differ from one location to another and may change with time, Customer is responsible for determining whether products and the information in this document are appropriate for Customer's use and for ensuring that Customer's workplace and disposal practices are in compliance with applicable laws and other government enactments. The product shown in this literature may not be available for sale and/or available in all geographies where Dow is represented. The claims made may not have been approved for use in all countries. Dow assumes no obligation or liability for the information in this document. References to Dow or the Company mean the Dow legal entity selling the products to Customer unless otherwise expressly noted. NO WARRANTIES ARE GIVEN; ALL IMPLIED WARRANTIES OF MERCHANTABILITY OR FITNESS FOR A PARTICULAR PURPOSE ARE EXPRESSLY EXCLUDED. Page 8 of 8 NIPOSIT TM PM-980 W / Interconnect Technologies September 2014