MICROFAB PB 200 High purity lead or lead-tin plating process for semiconductor applications

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1 High purity lead or lead-tin plating process for semiconductor applications MICROFAB PB 200 is a high-purity electroplating process which produces fine-grained pure lead or lead-rich tin/lead deposits. It is specially formulated for use in the fabrication of circuit patterns and bumps on semiconductor wafers. The process contains no fluoborates or formaldehyde. READ ENTIRE TECHNICAL DATA SHEET BE- FORE USING THIS PRODUCT. MATERIALS REQUIRED 1. MICROFAB PB 200 MAKE-UP is a highly-purified, ready-to-use solution containing 20 g/l (2.7 oz/gal) lead, 2 g/l (0.27) oz/gal) tin, 115 ml/l (14.7 oz/gal) free acid, and 40 ml/l (5.1 fl oz/gal) MICROFAB PB 200 REPLENISHER. 2. MICROFAB TIN CONCENTRATE is a high purity concentrate containing 300 g/l (40 oz/gal) tin. It provides the tin ion concentration for the operating solution. It also provides some of the acid required for optimum solution operation. 3. MICROFAB LEAD CONCENTRATE is a high purity concentrate containing 500 g/l (67 oz/gal) lead. It provides the lead ion concentration for the operating solution. It also provides some of the acid required for optimum solution operation. 4. MICROFAB NF ACID 70% is a high purity solution containing 942 g/l (125 oz/gal ) free acid. It provides acid for the operating solution and is necessary for solution stability and conductivity. 5. MICROFAB PB 200 REPLENISHER is a high purity, liquid concentrate for replenishment and stability of the plating solution. HOW TO USE MICROFAB PB 200 MAKE-UP 1. The plating tank, filter pump, anodes and anode bags must be properly leached with 10% v/v MICROFAB NF ACID 70% and thoroughly rinsed with deionized water. 2. Carefully add MICROFAB PB 200 MAKE-UP to the plating tank. 3. Check and adjust the solution temperature to 25 C (77 F). The plating solution is now ready for use. 2008, Enthone Inc. ssued: 20 July 2000 Spsds: 18 Jan 1995

2 Page 2 of 6 OPERATION Maintain the concentrations of tin (2+), lead (2+), and free acid ions by solution analysis (see ANALYSIS section) and additions of MICROFAB TIN CONCENTRATE, MICROFAB LEAD CONCENTRATE and MICROFAB PB300 NF ACID 70%, respectively. Maintain the temperature at an optimum of 25 C (77 F). The consumption rate of MICROFAB PB 200 REPLENISHER will be a function of the type of plating equipment used. However, the replenishment rate will normally be 1 to 3 ml per amp-hour. MICROFAB PB 200 REPLEN- ISHER contains grain refiners necessary to ensure a fine-grained, bondable deposit. EQUIPMENT Tank Material and Liners Rectifiers Anodes Pumps, Filtration and Filter Cartridges Agitation Temperature Control Use rigid PVC, CPVC, polypropylene, or Teflon-lined steel tanks with this solution. It should however be noted that this solution, contrary to fluoborate based solutions, does not dissolve glass and attacks metals only slowly. Titanium will not be attacked. Titanium parts can therefore be used without problems. NOTE: Avoid solution contact with the following materials: 316 stainless steel, Orlon, nylon, neoprene and cotton. Use a standard AC/DC power supply with an ampere output capacity sufficient to meet the requirements of the plating operation, with a maximum ripple of 5%. The use of an ampere-hour meter is strongly recommended. Insoluble anodes, platinized titanium, niobium or columbium anodes such as PERMANODES are recommended. Employ continuous filtration through modacrylic or polypropylene cartridges to ensure solution clarity. Moderate to vigorous agitation is essential to maintain uniform alloy distribution. Maintain the temperature at an optimum of 25 C (77 F). Ventilation Exhaust ventilation at the tank surface is recommended. Using the ACGIH manual "Industrial Ventilation," an A-4 class (rating) is recommended.

3 Page 3 of 6 CONTROL The following analytical procedures are recommended for use by personnel who have been trained to use laboratory practices which are considered safe and prudent by chemical industry standards. Such practices include suitable personal protective equipment, the use of proper equipment, the use of proper methods of handling all chemicals and proper laboratory procedures. Use only analytical reagent grade chemicals and deionized or distilled water in the following analytical procedures. CAUTION: The following procedures involve the use of potentially hazardous chemicals. Consult manufacturer's material safety data sheets and follow the appropriate safety precautions. Equipment Needed ANALYSES FOR MICROFAB PB 200 PLATING PROCESSES 1 2 ml pipet 1 5 ml pipet 1 5 ml graduated cylinder 1 10 ml graduated cylinder 1 10 ml pipet 1 20 ml pipet 1 50 ml graduated cylinder 3 50 ml burets ml Erlenmeyer flask ml Erlenmeyer flasks ml Erlenmeyer flask Reagents Needed M EDTA Ethylene-diamine-tetra-acetic Acid, Disodium Salt, Dihydrate (EDTA Na 2 2H 2 O) solution - Dissolve 21.4 grams of EDTA and 6 grams of sodium hydroxide (NaOH), AR grade, in 500 ml of water. Cool and dilute to one liter in a volumetric flask. Standardize against a zinc solution of known concentration M Zinc Chloride (ZnCl 2 ) - Add 10 ml HCl, conc. into about 500 ml H2O in a one-liter volumetric flask. Dissolve 7.8 grams of ZnCl 2 in this solution and dilute to volume with water. Standardize against M EDTA solution. 0.1 N Potassium Iodate (KlO 3 ) - Dry the crystals of KlO3, AR grade, to constant weight at 180 C. Dissolve grams KlO3 in about 200 ml of water containing 1 gram of sodium hydroxide (NaOH) and 23 grams potassium iodide (Kl). Dilute to one liter in a volumetric flask. Standardization not necessary if KlO 3 was weighed on an analytical balance. 1.0 N Sodium Hydroxide (NaOH) - Weigh 40 grams NaOH, AR grade, and dissolve in water. Dilute to one liter in a volumetric flask. Standardize against a H 2 SO 4 acid solution of known concentration. Eriochrome Black T: - Grind together 1 gram Eriochrome Black T with 99 grams sodium chloride. Starch Solution - Purchase 50% Hydrochloric acid (HCl) - Add 500 ml HCl, conc. 37%, to 500 ml water cautiously with stirring. Never add water to acid. 1M Rochelle salt (potassium sodium tartrate) - Dissolve 28 grams Rochelle salt in water and dilute to 100 ml with water. Buffer Solution (NH 4 Cl-NH 4 OH) - Dissolve 125 grams of NH 4 Cl in 500 ml of 29% NH 4 OH solution and dilute to one liter with 29% NH 4 OH solution. 30% Hydrogen peroxide (H2O2) - Purchase 20% Triethanolamine - Dilute 20 ml of triethanolamine to 100 ml with water. Mix well. Phenolphthalein Indicator - Dissolve 0.1 gram of phenolphthalein in 50 ml ethanol. Adjust final volume to 100 ml.

4 Page 4 of 6 Procedure ANALYSIS FOR LEAD 1. Pipet 10 ml of working solution into a 250 ml Erlenmeyer flask. 2. Add about 75 ml of water. 3. Add 3 ml of 1M Rochelle salt, 1 ml 30% H 2 O 2 and 3 ml 20% Triethanolamine. Mix after each addition. 4. Pipet 20 ml M EDTA into the Erlenmeyer flask. Mix. 5. Add 10 ml NH 4 Cl-NH 4 OH buffer. Mix. 6. Add enough Eriochrome Black T to produce a medium intensity blue color and titrate immediately to a red purple end point with M ZnCl 2. Calculation [(ml EDTA x M EDTA) minus (ml ZnCl 2 x M ZnCl 2 )] = g/l lead in solution. Replenishment For each g/l low by analysis, add 2 ml of MICROFAB LEAD CONCENTRATE per liter of working solution. ANALYSIS FOR TIN Procedure 1. Pipet 5 ml of working solution into a 250 ml Erlenmeyer flask. 2. Add 50 ml of water and 50 ml of 50% HCl. 3. Add 5 ml of starch solution. 4. Titrate with 0.1 N KI0 3 to a dark blue-brown color that persists for 30 seconds after swirling. Calculation ml KI0 3 titrated x N KI0 3 x = g/l tin in solution Replenishment For each g/l low, add 3.5 ml of MICROFAB TIN CONCENTRATE per liter of working solution. ANALYSIS FOR MICROFAB PB300 NF ACID 70% Procedure 1. Pipet a 10 ml sample of the operating solution into a 500 ml Erlenmeyer flask. 2. Add 100 ml of deionized water and ten drops of phenolphthalein indicator solution. 3. Titrate with 1.0 N sodium hydroxide solution until the first hint of a persistent purple color. Calculation ml NaOH titrated x N NaOH x 9.81 = g/l MICROFAB PB300 NF ACID 70% in solution. Replenishment For each ml low by analysis, add 1 ml of MICROFAB PB300 NF ACID 70% per liter of working solution.

5 Page 5 of 6 PRECAUTIONARY INFORMATION DANGER! MICROFAB PB 200 MAKE-UP, MICROFAB TIN CONCENTRATE, MICROFAB LEAD CONCENTRATE, MICROFAB PB300 NF ACID 70% AND THE OPERATING SOLUTION CONTAIN METHANE SULFONIC ACID, WHICH MAY CAUSE SEVERE BURNS, BLINDNESS. HAZARDS: MICROFAB PB 200 MAKE-UP, MICROFAB TIN CONCENTRATE, MICROFAB LEAD CONCENTRATE, MICROFAB PB300 NF ACID 70% and the operating solution contain methane sulfonic acid which upon contact may cause severe burns to skin and eyes, possible blindness. Inhalation of vapors or mist from the operating solution may cause severe irritation or burns to respiratory tract. Ingestion may cause burns of mouth, throat, esophagus and stomach. Contact with most metals will generate hydrogen, a highly flammable and explosive gas. May react violently with water. MICROFAB LEAD CONCENTRATE contains lead. Over exposure to lead can cause lead poisoning; damage to blood-forming, nervous, urinary, and reproductive systems. MICROFAB PB 200 REPLENISHER may cause irritation to skin, eyes, and gastro-intestinal tract. Do not get in eyes, on skin, or on clothing. Do not inhale or take internally. FIRST AID: In case of contact of MICROFAB PB 200 MAKE-UP, MICROFAB TIN CONCENTRATE, MICROFAB LEAD CONCENTRATE, MICROFAB PB300 NF ACID 70%, MICROFAB PB 200 REPLENISHER or the operating solution with skin or eyes, flush with plenty of clean, cool water for 15 minutes; for eyes get immediate medical attention. Remove contaminated clothing and shoes. HANDLING INFORMATION: When preparing or adding to the operating solution, always add MICROFAB PB 200 MAKE-UP, MICROFAB TIN CONCENTRATE, MICROFAB LEAD CONCENTRATE, MICROFAB NF ACID, MICROFAB PB 200 REPLENISHER slowly and cautiously. Do not get in eyes, on skin, or on clothing. Avoid breathing vapors or mist. Do not take internally. When handling MICROFAB PB 200 MAKE-UP, MICROFAB TIN CONCENTRATE, MICROFAB LEAD CONCENTRATE, MICROFAB NF ACID, MICROFAB PB 200 REPLENISHER or the operating solution, wear protective clothing, chemical safety goggles, respirator, face shield and Neoprene, PVC, or nitrile rubber gloves. Avoid contact with alkalis and any other foreign materials. Exhaust ventilation is recommended to remove vapors or mist that may be generated during Make-Up and Operation. CONTAINER INFORMATION: Keep containers tightly closed. Store indoors in a cool, dry area away from alkalis. Loosen closure cautiously when opening. Wash thoroughly after handling. Do not reuse containers, wash before disposal. Improper disposal or reuse of container may be dangerous and illegal. REFER TO MSDS FOR FURTHER SAFETY AND HANDLING INFORMATION

6 Page 6 of 6 MATERIAL SAFETY DATA SHEETS For more detailed information on the toxicological properties of the products described herein, reference can be made to the Material Safety Data Sheet (MSDS) for each product. If you do not have the proper MSDS, it can be requested from: Enthone Inc., attention: Regulatory Affairs Department, 350 Frontage Road, West Haven, CT For emergency assistance call CHEMTREC (800) WARRANTY AND DISCLAIMER The information presented herein is to the best of our knowledge true and accurate and all recommendations and suggestions appearing in this bulletin covering the use of our products are based upon information believed to be reliable. However, since the conditions of use are beyond our control, this information is given on the express condition and agreement that Enthone Inc. will not be liable to any person in contract, tort (including negligence), strict liability or otherwise for any claims, damages or losses whatsoever. Nothing herein shall be deemed a recommendation to use any product or process in violation of any existing patent rights and no warranties, expressed or implied, are made regarding the information, product, processes, recommendations, description and safety notations contained herein. The above includes proprietary information of Enthone Inc. and is furnished to you for your use solely on products or processes supplied by us to you. CUSTOMER ORDER CENTERS UNITED STATES Enthone Inc. 350 Frontage Road West Haven, Connecticut (800) Fax (203) ctchemorders@enthone.com MEXICO Enthone de Mexico S.A. de C.V. Norte 59 No Col. Industrial Vallejo Mexico, D.F. ( ) Fax ( ) BRAZIL Cookson Electronics Brasil Ltda. Av José Odorizzi, 650 Sao Bernardo do Campo SP CEP Brazil (011-55) Fax (011-55) vendas@enthone.com enthone.com Enthone Inc. Registered Trademark of Enthone Inc. Trademark of Enthone Inc. 19 Dec 2012_US TDS Last Page