ENPLATE Ni 434 E

High speed, stable, ammonia free electroless nickel process

INTRODUCTION ENPLATE Ni 434E is a high speed, extremely bright electroless nickel process with a moderate phosphorus content, designed for optimum bath performance. This process offers excellent high temperature stability. The ENPLATE Ni 434E process chemically deposits a uniform nickel-phosphorus alloy on a wide variety of substrates. The process contains no ammonia. The ENPLATE Ni 434E is supplied as three separate liquid concentrates. ENPLATE Ni 434E A and ENPLATE Ni 434E B are used for bath make-up and ENPLATE Ni 434E A and ENPLATE Ni 434E C are used for replenishment. ENPLATE Ni 434 E meets MIL-C-26074E, AMS 2404 and AMS 2405 specifications. Features of the ENPLATE Ni 434E process * * * * * Excellent stability/extended bath life Fast plating rate Effective bath performance at low surface area to volume ratio Superior brightness Ease in waste treatment of spent plating bath (ammonia free)

Issued Spsds

: 13 Sep 2001 : 07 Dec 1999

ENPLATE Ni 434E Technical data sheet Page 2 of 10

ENPLATE NI 434E PHYSICAL PROPERTIES Typical result Phosphorus Content, wt% Melting Point (eutectic) C Coefficient of Thermal Expansion. m /m/C Thermal Conductivity, cal/cm/sec/C Electrical Resistivity microhm-cm Magnetic Properties Hardness Vickers HV 100 100g load, 75 m deposit, steel As plated Heat treated @ 1 hr 400C Wear Properties Taber Abraser Wear test Taber Wear Index Wt. loss mg/1000 cycles As plated Heat treated @ 1hr. 400C Corrosion Related Properties Salt spray test* (ASTM B117) 35C 5% NaCl, 25m deposit, hours to first corrosion spot 2024 Aluminium 1010 carbon Steel Nitric Acid Test Conc. nitric acid 42 Be 30 sec room temp 25 m steel Hydrochloric Acid Test 50% HC1, 3 min, room temp 25m steel * 5.0 to 8.5 880 to 960 13 to 15 0.0105 to 0.0135 50 to 100 Slightly Magnetic

500 to 680 760 to 870

15 to 18 4 to 8

100 100 Fail **

Pass**

**

ASTM test is performed on a flat panel. More complex or rough parts may show initial spotting in fewer hours. ASTM B117 salt spray is primarily a porosity test and only effective as a screening tool to show the difference afforded by alternative processes. It is not, however, a quantitative corrosion test. Fail is indicated by any significant discoloration of the deposit.

EQUIPMENT Anodically protected stainless steel tanks are recommended. Polypropylene or polypropylene-lined tanks can also be used. Steam teflon super coils, or type 316 stainless steel electric immersion heaters may be used. Note: Electric heaters must be properly earthed (earth leakage) and equipped with over-temperature hazard protected, also low liquid level shut-off devices are recommended. In-tank filtration is recommended. Clean, low-pressure air agitation through bottom-mounted stainless steel, CPVC or polypropylene pipes is highly recommended. Clean air, free of oil and dirt is required; shop air should not be used.

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Exhaust ventilation is recommended to remove solution mist which is caused by agitation or gassing of the solution and which may contain nickel salts. The bath should be kept covered when it contains no work and is at or near operating temperature. FILTRATION Continuous filtration is recommended. To ensure smooth deposits continuous filtration through 5 micron filtration medium is required, (preferably gravity feed bag-type units). A minimum of 6 to 10 solution turnovers per hour is recommended for proper filtration. If continuous filtration is not feasible, the solution must be cooled at the end of the working period, then batch filtered through a 3 micron filtration medium before beginning the next days work. With or without continuous filtration, the tank and filtration equipment will require periodic leaching with 30% nitric acid followed by water rinse and a final deionised or distilled water rinse (with a small amount of potassium carbonate added). AGITATION Horizontal work rod agitation and/or air agitation using a low pressure blower are recommended. Agitation during heating avoids localised overheating which can result in bath plateout. CONTROL As with all electroless nickel solutions, successful plating requires maintaining proper solution control; temperature, pH agitation, filtration and chemistry. The use of automatic controllers/dosing units is strongly recommended. A complete information package on equipment for electroless nickel plating is available on request. Included is information on electroless nickel plating tanks, EN series electroless nickel controllers and ion exchange systems for the removal of nickel from electroless nickel rinses. SOLUTION PREPARATION ENPLATE Ni 434E is supplied as three separate liquid concentrates. ENPLATE Ni 434E A is used for makeup and replenishment, ENPLATE Ni 434E B is used only for make-up, and ENPLATE NI 434E C are used only for replenishment. COMPONENT PROPERTIES ENPLATE Ni 434E A Specific gravity Colour SOLUTION MAKE UP Make up additions ml per litre ENPLATE Ni 434E A ENPLATE Ni 434E B ENPLATE Ni 434E C Deionised or distilled water 60 150 790 1.27 Green ENPLATE Ni 434E B 1.19 Colourless ENPLATE Ni 434E C 1.29 Colourless

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To make up the required amount of operating solution, proceed as follows: 1. 2. 3. 4. Rinse tank thoroughly with deionised or distilled water. Partially fill tank with deionised or distilled water. Add the required amount of ENPLATE Ni 434E A and ENPLATE Ni 434E B, with air or mechanical agitation and fill to working volume with deionised or distilled water. Heat solution to 82 to 91C. Check solution pH. Adjust if necessary with dilute (~50%) potassium carbonate, or (~10%) sulphuric acid.

OPERATING CONDITIONS Solution parameters Temperature C pH Bath loading dm2/l Nickel concentration g/l * Up to 5.2 for aluminium alloys. PERFORMANCE Typical results Plating rate, m/h 88C Solution life, turnovers* Steel Aluminium * ** 17 to 20** microns/hour 8 7 to 8 Typical range 82 to 91 4.7 to 5.2* 0.25 to 2.45 5.2 to 6.0 Optimum value 88 4.9 to 5.2* 1.23 5.8

Turnover occurs when the original concentration of 5.8 g/l nickel metal has been replenished. Increasing the pH as the bath ages, i.e. Beginning at pH 4.7 gradually increasing to pH 5.2, will help to maintain the plating rate.

TEMPERATURE Faster plating rates are obtained at higher temperatures. Low temperatures should be used to retard pitting when heavy deposits are desired. Do not maintain the bath at operating temperature if work is not being processed. This will cause breakdown of the reducer and stabiliser components. Heating the bath above 91C is not recommended. pH pH may be adjusted upward by additions of dilute (~50%) calcined potassium carbonate solution. A high purity, 47% by weight, calcined potassium carbonate solution is available. Sulphuric acid, 10% by volume, may be used to lower pH. Make all additions slowly with constant stirring. When using potassium carbonate for pH adjustment, be especially careful to make additions slowly with stirring to prevent eruption of the bath due to carbon dioxide liberation. pH measurements should be made only after good agitation (and consistent bath temperature) to assure equilibrium concentration of the bath. Narrow range pH papers are recommended when measuring the pH at the tank side. Electrometric pH meters are recommended for accurate measurement of pH. In this case, the buffer and solution temperature must be equal before testing. Because potassium carbonate is used for pH adjustment, a white crystalline precipitate (potassium sulphate) can occur in the electroless nickel bath after approximately 7 to 8 metal turnovers. This is especially true during cooling of an electroless nickel solution and is indicative of an aged bath.

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Note: This precipitate is not a problem and a simple decanting procedure of the precipitate should be performed (together with filtration). If ammonia is not a problem in the effluent, ammonia solution may be used for pH adjustment in place of potassium carbonate if desired. The solution life will be extended (up to 10 metal turnovers) if ammonia is used and the precipitation of potassium sulphate will be prevented. RECOMMENDED PLATING PROCEDURES The quality of the finished product is generally dependent upon the original condition of the workpiece, pretreatment, and the condition and control of the plating solution. Generally, those involved in finishing operations have very little control over the condition of the workpiece as received. Therefore, proper pretreatment, and solution control are essential to minimse rejects and maximise production. CLEANING A water-break and scale-free surface is required for proper adhesion. Routine analysis of cleaners and descalers (acid salts) can minimise rejects. CLEANING SEQUENCE FOR STEEL Time (minutes) 1. 2. 3. ENBOND 808 Hot alkali soal cleaner COLD WATER RINSE (CWR) ENDOX 114 Room temperature electrolytic Periodic reverse cleaner (ending with an anodic cycle) CWR ACTANE 82 Acid dip CWR ENDOX 114 (as step 3 CWR HOT WATER RINSE (HWR) (if necessary, for pre-heating large items) ELECTROLESS NICKEL PLATE 5.0 1.0 2.0

4. 5. 6. 7. 8. 9. 10.

1.0 0.5 to 1.0 1.0 2.0 1.0

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CLEANING SEQUENCE FOR COPPER ALLOYS Time (minutes) 1. ENBOND 160 or ENBOND Z 72 Soak clean COLD WATER (CWR) EBOND 160 Cathodic cleaner ENPLATE AD 485 Mild etch CWR SULPHURIC ACID DIP (10% by volume) CWR ELECTROLESS NICKEL PLATE Promote deposition by cathodic pulse 5.0

2. 3. or 4. 5. 6. 7.

1.0 1.0 1.0 1.0 0.5 to 1.0 1.0

CLEANING AND PREPARATION SEQUENCE FOR ALUMINIUM Time (minutes) 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. ENBOND NS-35 COLD WATER RINSE (CWR) ACTANE 70/NITRIC/SULPHURIC ACID SOLUTION Smut remover CWR ALUMON EN Zincate process CWR 50% NITRIC ACID STRIP CWR ACTANE 70 CWR ALUMON EN (can be a repeat of step 5) CWR ENPLATE AL 100 ELECTROLESS NICKEL STRIKE BATH (Optional - particularly useful for castings) CWR ELECTROLESS NICKEL PLATE 5.0 1.0 0.5 to 1.0 1.0 1.0 to 2.0 1.0 1.0 1.0 0.25 1.0 0.3 to 0.5 1.0

14. 15.

1.0

The delay between cleaning and plating should be the minimum possible. PLATING After proper preparation, parts to be electroless nickel plated are simply immersed in the ENPLATE Ni 434E operating solution for the required time to obtain the desired thickness. REPLENISHMENT Replenishment (see table over) is based on percent nickel activity of the solution. Analysis is required to determine the proper amount of replenishment chemicals. The ENPLATE Ni 434E process is maintained by additions of ENPLATE Ni 434E A and ENPLATE Ni 434E C at a 1:1 ratio. The amount of replenishment chemicals required Can be determined by a simple nickel titration. * For optimum results the nickel concentration should not be allowed to fall below 5.3 g/l.

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The maximum recommended additions (at any one time) should not exceed 10 percent of the original metal content of the operating solution. If additions greater than 10 percent are required, they should be accomplished incrementally between workloads. All replenishment additions should be made with agitation.

ENPLATE NI 434 E REPLENISHMENT SCHEDULE Additions ml/l Ni 434E A Ni 434E C 1.5 3.0 4.5 6.0 7.5 9.0 10.5 12.0 13.5 15.0 16.5 18.0 1.5 3.0 4.5 6.0 7.5 9.0 10.5 12.0 13.5 15.0 16.5 18.0 Remarks Ni concentration g/l % activity 5.8 5.6 5.5 5.3 5.2 5.1 4.9 4.7 4.6 4.5 4.4 4.2 4.1 100 97.5 95.0 92.5 90.0 87.5 85.0 82.5 80.0 77.5 75.0 72.5 70.0

ml EDTA ** titrated 8.5 8.3 8.1 7.9 7.7 7.5 7.2 7.0 6.9 6.7 6.4 6.2 6.0 * **

Replenishment additions should never exceed 10% of the original make-up. When a 5 ml sample is titrated with a 0.0575M EDTA solution.

ANALYTICAL CONTROL Control of the ENPLATE Ni 434E bath is based on the rapid and accurate analysis for nickel metal content as follows: ANALYSIS FOR NICKEL METAL Apparatus needed 5 ml pipette 50 ml burette with 0.1 ml graduations 250 ml erlenmeyer flask Reagents needed 0.0575M EDTA solution: Dissolve 21.4 grams of EDTA - Na2 (disodium ethylene diamine-tetra-acetate) and 6.0 grams of AR grade sodium hydroxide in deionised or distilled water. Allow to cool and dilute to exactly 1 litre with deionised or distilled water using a volumetric flask. Murexide Indicator: Mix 0.2 gram of Murexide (acid ammonium purpurate) with 100 grams of sodium chloride. Grind together with a mortar and pestle. AR grade ammonium hydroxide.

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PROCEDURES 1. 2. With a safety pipette, transfer a 5 ml sample of the bath into the 250 ml Erlenmeyer flask. Add approximately 50 ml deionised or distilled water, 10 ml AR grade ammonium hydroxide, and a "pinch" of murexide indicator. Only sufficient murexide indicator should be added to develop a pale straw colour; too much indicator obscures the end point. Titrate with the EDTA solution to a blue-purple end point.

3.

Calculation ml EDTA x 0.675 = g/l of nickel metal Replenishment Nickel metal content should be maintained at an average range of 5.3 - 6.3 g/l. For each 1 g/l of nickel metal to be replenished, add 10 ml/l of ENPLATE Ni 434E A and 10 ml of ENPLATE Ni 434E C. Check the pH of the solution and adjust, if necessary. ANALYSIS FOR HYPOPHOSPHITE Normally, replenishment additions of ENPLATE Ni 434E based on the analysis for nickel metal will keep the concentration of reducer at its proper level. However, the consumption of reducer may not always be at the same rate; therefore, it is advisable to run occasional analyses to ensure that it is in the recommended range (26.5 to 29 g/l). If it is not within the recommended range, replenish using ENPLATE Ni 434E C as outlined below. Apparatus needed 250 ml glass stoppered iodine flask 2 ml pipette 50 ml pipette 5 ml dropping pipette 25 ml graduate 50 ml burette Reagents needed 0.10N Iodine solution 50% v/v Hydrochloric Acid 0.10N sodium thiosulphate (Na2S2O3)* * These are available as ready-to-use solutions or as measured concentrates your local laboratory chemical supply house. in ampoules from

PROCEDURE 1. 2. 3. 4. With a safety pipette, transfer a 2 ml sample of the solution into a stoppered iodine flask. Add 25 ml of 50% v/v hydrochloric acid. With a safety pipette, transfer 50 ml of the 0.10N standard iodine solution into the flask. Stopper the flask and set in the dark for exactly 30 minutes. Solution temperature should be 20 2C. Titrate with 0.10N sodium thiosulphate until the solution is faintly yellow-brown. Add a few millilitres of Starch solution and continue titration to the disappearance of the blue-mauve coloration.

Calculation (50 ....ml Thiosulphate) x 2.65 = g/l hypophosphite

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REPLENISHMENT Reducer should be maintained at 26.5 to 29 g/l. For every 1 g/l low add 2 ml/l of ENPLATE Ni 434E C. STRIPPING ENSTRIP EN 79 and ENSTRIP EN 86 are non-cyanide, alkaline strippers utilising advanced technology. They dissolve electroless nickel deposits up to 125 m thick from steel by immersion. These products are particularly effective in removing high phosphorus deposits that could be difficult to remove with other strippers. The expected stripping rate will range from 10 to 15 m/h. Solution life will vary depending upon method and condition of operation, but should hold nickel metal at the level of 15 to 30 g/l of ENSTRIP EN 79 or ENSTRIP EN 86. ENSTRIP EN 79 and ENSTRIP EN 86 are also effective in stripping electroless nickel deposits from copper, and copper alloys, stainless steel, kovar, and some nickel based alloys. Proper cleaning of the part is required before stripping. Soak cleaning followed by reactivation of the deposit surface with 50% hcl is recommended for parts that are carbonised and oxidised due to storage or extended service. Cathodic activation in ACTANE 82 using carbon anodes is recommended for aged or heavily oxidised deposits. SOLDERABILITY Soldering to ENPLATE Ni 434E can be effectively accomplished with a fully active flux. Direct soldering to electroless nickel is difficult, particularly as the deposit ages and forms oxides on the surface. If direct soldering is desired, this should be done as soon as possible after plating. WASTE TREATMENT Operating solutions of ENPLATE Ni 434E contain nickel and are very slightly acidic. Before disposing of the spent solution, the nickel should be removed and the pH adjusted to the regulated limits. A customer bulletin is available detailing nickel removal. Be sure to consult local agencies with regard to regulations concerning pH limits and nickel bearing sludge disposal. PRECAUTIONARY INFORMATION CAUTION ENPLATE Ni 434E A, Ni 434E B, Ni 434E C and ENPLATE Ni 434E operating solution may cause irritation. HAZARD ENPLATE Ni 434E A, contains nickel sulphate, sensitivity to nickel may cause skin irritation. ENPLATE Ni 434E B, and ENPLATE Ni 434E C contain hypophosphite and may cause irritation. Heating dried salts to temperatures over 245C may produce toxic and flammable phosphine gas. HANDLING INFORMATION Always wear chemical safety goggles, rubber gloves, and protective clothing when handling ENPLATE Ni 434E A, B and C and the ENPLATE Ni 434E operating solutions. Exhaust ventilation is recommended to remove mist or vapours that may be generated during make up and operation. Wash thoroughly after handling.

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CONTAINER INFORMATION Keep containers tightly closed. Store indoors in a cool dry, frost free area away from acids, salts, or oxidisers. Loosen closure cautiously when opening. Do not re-use containers. Wash before disposal. Improper disposal or re-use of containers may be dangerous and illegal. HANDLING AND SAFETY INSTRUCTIONS For detailed information consult the material safety data sheets for this product. Please read material safety data sheets carefully before using this product. DISCLAIMER All recommendations and suggestions in this bulletin concerning the use of our products are based upon tests and data believed to be reliable. Since the actual use by others is beyond our control, no guarantee expressed or implied, is made by Enthone, its subsidiaries of distributors, as to the effects of such use or results to be obtained, nor is any information to be construed as a recommendation to infringe any patent. ADDRESSES
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