PRODUCT INFORMATION DATA SHEET Electrochemicals Inc. 5630 Pioneer Creek Drive Maple Plain, Minnesota 55359 763-479-2008 Fax 763-479-3344 PRODUCT DESCRIPTION SHADOW * CONDUCTIVE COLLOID 2 Shadow Conductive Colloid 2 is a slightly alkaline aqueous dispersion of conductive colloids and proprietary additives used to make through-holes, and other vias, conductive for subsequent copper electroplating. Shadow Conductive Colloid 2 is environmentally advantageous as compared to other metalization processes. These benefits include, no metal chelators, less rinse water usage, and ease of operation. The Shadow Conductive Colloid 2 chemistry, and the other products/processes in the Shadow direct metalization process, are covered by several U.S. and foreign patents*. SOLUTION MAKE-UP Shadow Conductive Colloid 2 Deionized Water 31-63% v/v 69-37% v/v Mixing Instructions 1. The entire sump and upper process tray must be clean and free of any loose Shadow particles. 2. Before placing Shadow Conductive Colloid 2 into sump, the following must be done to ensure the proper concentration of solids in the working solution: If Shadow Conductive Colloid 2 is shipped in a 5 gallon container, mix well by shaking the pail for several minutes. If Shadow Conductive Colloid 2 is shipped in a 55 gallon container, mix well by recirculating the solution within the drum with a clean, dedicated electric drum pump for 10 minutes. *United States Patent # s 5,389,270; #5,476,580; #5,690,805; #5,725,807 IMPORTANT: THE INFORMATION PRESENTED HERE IS BELIEVED TO BE ACCURATE AND IS OFFERED ONLY AS A GUIDE. USERS SHOULD MAKE THEIR OWN TESTS TO DETERMINE THE SUITABILITY OF THESE PRODUCTS FOR THEIR OWN PARTICULAR PURPOSES. USER ASSUMES ALL RISK OF USE, STOARGE AND HANDLING OF THE PRODUCT. NO WARRANTY, EXPRESSED OR IMPLIED, IS MADE INCLUDING, BUT NOT LIMITED TO, IMPLIED WARRANTIES OF MERCHANTABILITY AND FITNESS FOR A PARTICULAR PURPOSE. NOTHING CONTAINED HEREIN SHALL BE CONSTRUED AS A LICENSE TO OPERATE UNDER, OR RECOMMENDATION TO INFRINGE, ANY PATENTS.
SHADOW Conductive Colloid 2 2 of 19 Mixing Instructions (cont d) 3. Carefully add Shadow Conductive Colloid 2 to the sump to prevent splashing. 4. Slowly add the DI Water while mixing from the recirculation pump if possible. Do not add DI water first. 5. Let the recirculation pump mix the bath for a minimum of 2 hours before sampling the bath for analysis. After analysis confirms the proper concentration, production may begin. OPERATING CONDITIONS Nominal Range Percent Solids 3.75% 2.5 to 5% ph* 8.8 8.0 to 9.2 Temperature 21.1 C (70 F) 15.5-26.6 C (60-80 F) Contact Time 30 seconds 20-40 seconds Filtration 100 micron 50-250 micron *A new bath will initially have a ph in the 9.7 to 10.2 range. This is normal. Do not attempt to adjust the ph down. -The use of immersion heaters in the Shadow Conductive Colloid 2 bath is NOT recommended. Running chilled water through a cooling coil is necessary due to the heat generated by the recirculation and lift pumps. -Filters must be cartridge-type stainless steel mesh only. -All of the nominal and range values given above may be modified by an Electrochemicals Sales/Technical Service Representative according to specific customer needs.
SHADOW Conductive Colloid 2 3 of 19 IMPORTANT CONSIDERATIONS Storage Conditions of Concentrate in Drum Store the Shadow Conductive Colloid 2 drum between 10 C and 32 C (50 F - 90 F). Do not allow the Shadow Conductive Colloid 2 to freeze or overheat. Both of these conditions can destroy the stability of the colloid. Generalized Start-up Procedure for Shadow conveyorized process. (Always refer to the specific Process/Operation Manual for the Shadow line for the exact Start-Up procedures.) Part 1 1. Check the entire line for chemical or water leaks and perform a safety check. 2. Check the solution level of each process tank. Adjust solution level with DI water. 3. Take the PVA rollers from the water they have been soaking in and thoroughly squeeze out the excess water. Install the PVA rollers after the Shadow module making sure the rollers are replaced to the exact position they were taken from. The rollers will be removed once the operation ends for the day. They should be soaked in deionized water overnight to maintain softness and integrity. Do not let the Shadow PVA rollers dry out. 4. Turn on the power at the main control panel. 5. Turn on all mixing and flood pumps. 6. Turn on all heaters. 7. Let the solutions warm up and continue to allow Shadow Conductive Colloid to MIX for approx. 60 min. 8. Take samples and analyze according to the analysis schedule. 9. Check all spray nozzles on the line. Clean and adjust if necessary. 10. Check all flood levels and spray pressures. Part 2 1. Replenish solutions, as determined by the analysis, to their operating parameters. 2. Record all adds/dumps in a designated replenishment record book. 3. Turn on the dryers and allow them to achieve proper temperature. 4. Run dummy panels. Run 10-12 full size panels through the entire line. This will properly wet and soak the PVA rollers with the Shadow solution. 5. Check PVA roller operation for consistency of Shadow coating on the board surface. 6. Run an etch rate weight loss coupon through the line.
SHADOW Conductive Colloid 2 4 of 19 IMPORTANT CONSIDERATIONS (part 2 cont d.) 7. Adjust microetch line speed, temperature, or concentration accordingly. 8. Turn on the ultrasonic unit in the Cleaner/Conditioner. 9. Run a test panel through the Shadow line and have it acid copper flash plated for 10 minutes at 25 ASF (2.7A/dm 2 ). Inspect panel for voids. If no voids are found, proceed with production. Record the plating results. If voids are found, check the Shadow trouble shooting guide or call your Electrochemicals Sales or Technical Representative. 10. Remember to write down all part numbers and corresponding square footages in the logbook. Even rework panels have to be counted to maintain an accurate number for square footage bath lives. 11. During Shadow production, line operators should periodically check the following items: -Check control display to ensure that all pumps/heaters are operational. -Check to see that all flood solutions are at proper operating levels. -Check pressure gauges, ensure proper readings. -Confirm proper conveyor tracking by observing several panels transported through the line. Cleanliness of the Shadow Conductive Colloid 2 module process equipment is important to the operation and performance of the process. Generalized Shut-down Procedure for Shadow conveyorized process. (Always refer to the specific Process/Operation Manual for the Shadow line for the exact SHUT-DOWN procedures.) 1. Make sure all panels have exited the machine. After all production is through the line, turn off all modules, sprays, heaters, and dryers. 2. After Shadow drains to main sump, remove all of the Shadow PVA rollers and squeeze the excess solution back to the flood chamber. Soak the PVA rollers overnight in fresh DI water only. It is important that PVA rollers from different process steps not be soaked together. (Change the DI water daily.) 3. Remove, clean, rinse, and re-install any other rollers as needed. 4. Dump all rinse sumps (including Fixer Rinse) and refill with water. 5. Dump the Antitarnish. Clean and refill the sump according to the procedure outlined in your specific Process/Operation Manual. 6. Wipe down the machine. Clean any chemical deposits or build-up. 7. Perform a safety check of the entire line.
SHADOW Conductive Colloid 2 5 of 19 RECOMMENDED PROCESS CYCLE Module Process Step 1 Shadow Cleaner/Conditioner III or IV 2 Rinse 3 Shadow Conductive Colloid 2 4 Shadow Fixer 5 Rinse 6 Dry 7 Cu-Prep II microetch 8 Rinse 9 Shadow Antitarnish 10 Rinse 11 Final Dry BATH OPERATION AND MAINTENANCE Shadow Conductive Colloid 2 is controlled by percent solids and ph analysis. Replenishment is based on percent solids. Other less frequent analyses are the copper concentration and settling test. A typical analysis schedule follows: Test Procedure Upon Make-up Daily Weekly PH Yes Yes % Solids Yes Yes Copper Settling Bath life of the Shadow Conductive Colloid 2 depends on several factors such as: 1. Copper concentration Yes Yes 2. Drag in, or introduction, of contaminants (e.g. Cleaner/Conditioner) 3. Rate of replenishment (usage) 4. Cleanliness and maintenance of equipment 5. ph maintenance
SHADOW Conductive Colloid 2 6 of 19 BATH OPERATION AND MAINTENANCE Replenishment based on Percent Solids: To raise the solids by 0.1%, add 60 ml of Shadow Conductive Colloid 2 per gallon of bath (15.8 ml/l). Replenishment based on ph: To raise ph by 0.1 units, add 0.8 ml of conc. ammonium hydroxide per gallon of bath (0.2 ml/l). IMPORTANT NOTE: The concentrated ammonium hydroxide (28%) must be diluted at least 3:1 with DI water and mixed well before slowly adding to the Shadow sump while the Shadow solution is mixing. Important: Make sure that the Shadow Conductive Colloid 2 is thoroughly mixed in the container before making any adds. Shake the pail for several minutes to ensure the product is uniform in consistency before pouring any solution from the container. Daily Maintenance, Shadow Module: 1. Clean Shadow filter. 2. Rinse excess Shadow off rollers. 3. Check fluid head or nozzles for clogs. 4. Check condition of PVA rollers. Replace if wear is evident. Monthly Maintenance, Shadow Module: 1. Clean all rollers. Remove one section of rollers at a time and note the exact roller configuration. Important: all rollers must be replaced in the proper location. 2. Remove and thoroughly clean the fluid head or sparger nozzles and bars. 3. Scrap out any dried Shadow from the flood chamber. 4. Replace Shadow PVA rollers a minimum of every six months.
SHADOW Conductive Colloid 2 7 of 19 SHADOW TROUBLESHOOTING GUIDE I. VOIDS POSSIBLE CAUSE CORRECTIVE ACTION 1. Fixer is too aggressive 1A. Slow down Fixer solution flow. 1B. Analyze and adjust Fixer as needed. 1C. Check temperature in Fixer. 2. Insufficient Conditioning 2A. Check volume of work through Cleaner/Conditioner bath. Rebatch if required. 3. Low Flow Rate Through Flood Bars or Low Flood Level in the Shadow Chamber 2B. Check Cleaner/Conditioner operation, including consistent flood level and dam rollers. 3A. Check for clogging in the heads. 3B. Check for cracks in the plumbing near the slots/holes in the heads. 3C. Check delivery pumps for problems. 3D. Check for excess sludge in the sump, clean if necessary. 4. Shadow Bath Contaminated 4A. Check copper concentration (maintain at <700 ppm). 4B. Check for foaming in the Shadow bath. 4C. Check Shadow entry rollers and Cleaner/Conditioner rinse operation. 4D. Check for cooling coil for leaks. 5. Low Solids in Shadow Bath 5A. Analyze and add Shadow Conductive Colloid as required.
SHADOW Conductive Colloid 2 8 of 19 I. VOIDS (cont d) 6. Shadow Not Dried Completely before Microetch 7. Too Much Water in PVA Rollers After Soaking/Cleaning 6A. Check to see if dryer is on. 6B. Check dryer temperature (>140 F, 60 C). 6C. Check hoses from blower to oven and hot air knifes. 6D. Check blower operation. 6E. Make sure dryer covers are in place. 6F. Check blower intake filters. 8. Large Particulate in Shadow Bath 8A. Filter bath. 6G. Check heating elements for consistent operation. 7A. Soak in DI water as needed, squeeze out all excess water, re-saturate with Shadow. Run 15 20 dummy panels before production. 9. Plasma Ash Present 9A. Remove ash prior to Shadow process with additional burn or permanganate. 9B. Modify plasma parameters. 10. Microetch Too Aggressive 10A. Lower etch rate to 20 30 microinches (0.51 0.76 microns). When using Fixer, lower etch rate to 15 22 microinches (0.38 0.55 microns.) 10B. Lower spray pressure to 20 40 psi (1.0 2.7 bar). 11. Acid Copper Preclean Problems 11A. Avoid strong alkaline contact before plating. 11B. Use only Electrochemicals recommended cleaners. 11C. Limit exposure in the pre-plate 10% sulfuric acid prior to a maximum of 5 minutes. 12. Voids After Rework 12A. Run panels through the entire Shadow line anytime resist has been stripped.
SHADOW Conductive Colloid 2 9 of 19 II. WEDGE VOIDS 1. Oxide/Postdip Problems 1A. Contact oxide/treatment supplier. Reduced oxide or double treat required. 2. Lamination/Cure Parameters to Meet Specifications 2A. Adjust lamination cycle parameters to meet vendors specifications. 3. Wedges From Desmear 3A. Adjust time, temperature and concentrations to eliminate wedges. 3B. Institute post drill baking. 4. Drilling Nailheading 4A. Adjust feeds and speeds. 4B. Lower hits per bit. 4C. Improve backup and/or entry material. 4D. Lower stack height. 5. Poor Plating 5A. Contact plating chemistry supplier. 6. Microetch Rate Too High 6A. Maintain recommended etch rate. 7. Poor Plating Rectifiers 7A. Check ripple and noise level. (use an oscilloscope, not a volt meter). III. GLASS VOIDS 1. Drilling Gouges 1A. Adjust feeds and speeds, check spindle turnout and collets. 1B. Lower hits per bit. 1C. Improve backup and/or entry material. 1D. Lower stack height. 2. Resin Starvation Around Glass Bundles 2A. Contact laminate supplier. IV. ICD S / POST SEPARATION 2B. Adjust resin content in prepreg and/or lamination cycle, if applicable. 1. Drill Smear on Post 1A. Check desmear operation. Increase resin removal in desmear process. 2. Improper Microetching in Shadow Line 2A. Check for plugged nozzles. 2B. Check pressure through nozzles. 2C. Check etch rate. 2D. Check filters, replace if necessary.
SHADOW Conductive Colloid 2 10 of 19 V. CORNER CONTAMINATION (Thick Shadow at knee of hole) 1. Burrs 1A. Improve drilling/deburr process 2. Drill Smear 2A. Increase resin removal in desmear. 3. Air Knives / PVA Rollers 3A. Check operation of air knives. 3B. Check operation of PVA rollers. 4. Microetch 4A. Ensure proper microetch operation. VI. SURFACE CONTAMINATION 1. Dried Shadow on Panel 1A. Clean rollers, making sure that all dried Shadow is removed. 1B. Check operation of microetch. 1C. Check for dried Shadow particles on PVA rollers. 1D. Filter Conductive Colloid to remove all debris. 2. Streaks on panels 2A. Ensure PVA rollers are wet. VII. OXIDATION 2B. Check microetch operation. 1. Antitarnish 1A. Dump and remake antitarnish. VIII. ROUGH PLATING OR PITTING 1. Shadow residue on rollers (Line is not clean.) 1B. Check PVA or chamois roller operation prior to final dry. 1C. Check antitarnish and following rinse for plugged nozzles. 1A. Clean the Shadow line. 2. Antitarnish 2A. Clean out antitarnish chamber as recommended to remove mold. IX. PLUGGED HOLES 1. Drill Debris / Excessive Burrs 1A. Check backup and entry material. 1B. Improve deburr / high pressure rinse. 2. Particulate in Shadow bath 2A. Filter solution and clean out sump.
SHADOW Conductive Colloid 2 11 of 19 X. POOR DRY FILM ADHESION 1. Stains on Surface 1A. Check antitarnish. 1B. Check dryer operation. 1C. Clean Shadow line. 2. Poor Topography 2A. Check Cu-Prep II etch rate.
SHADOW Conductive Colloid 2 12 of 19 EQUIPMENT Tanks and Process Modules polypropylene, PVC and other plastics Conveyor Rollers PVA, EPDM, Neoprene and other chemically resistant rubbers, PVC and other plastics Filters stainless steel mesh only Cooling Coils titanium, stainless steel WASTE TREATMENT Batch Waste Treatment Outline for Shadow Conductive Colloid 2: The spent Shadow Conductive Colloid 2 bath may contain approximately 0.4 to 1.0 gram/liter copper complexed by ammonia. The initial part of the waste treatment of the spent Shadow Conductive Colloid bath is recommended as a batch process up to step 3. After step 3, the solution can be slowly bled into a copper metal waste stream such as an ion-resin bed or a DTC-(sodium diethyldithiocarbamate) type precipitation tank after the proper ph adjustments are made according to the process used. 1. Dilute the spent bath by 50% with water. 2. Slowly, add dilute sulfuric acid to ph 1.8 and mix for one hour. Monitor ph and readjust as needed. 3. Filter out precipitated graphite. Bleed the clear supernatant into a metals waste stream or continue to batch treat. If supernatant is not clear, continue filtering before continuing. 4. To the filtered solution, raise the ph to 8.5 with dilute NaOH solution. Let mix for one hour. The ph MUST BE MONITORED and kept at exactly ph 8.5. 5. Filter precipitated copper. 6. Check the copper concentration in the solution. A metal precipitant (such as DTC) may have to be added at this point. Follow directions of the DTC or metal precipitant supplier. Dispose of the solids and filtered solutions in accordance with all federal, state and local regulations. SAFETY Consult the Material Safety Data Sheet for safety, health and environmental information. Shadow Conductive Colloid 2 is a mildly alkaline solution, normal caution such as the use of safety goggles, rubber gloves, etc. should be exercised during handling. In the event of eye contact, flush with copious amounts of water and see a physician.
SHADOW Conductive Colloid 2 13 of 19 ANALYSIS PROCEDURE NUMBER: AP.4101.02 PAGE: 1 of 1 I. PROCEDURE DESCRIPTION: Gravimetric procedure to determine Percent Solids in a Shadow bath. II. EQUIPMENT & SETTINGS A. Aluminum dish (Fisher Cat# 08-732 or VWR Cat# 25433-008) B. Infrared Lamp, 250 watt C. Analytical Balance (0.001g capacity) III. REAGENTS A. None IV. PROCEDURE A. Weigh the aluminum dish on the analytical balance. Record as (A). B. Place a 5 ml sample of Shadow bath into the aluminum dish. Record the weight as (B). C. Place the sample under the infrared lamp. The lamp height should be 3-5 inches from the sample. (Adjust lamp height to obtain 110 C 125 C. This can be checked by placing a thermometer under the lamp for a minimum of 10 minutes.) D. Turn lamp on and allow to evaporate for 30 minutes. E. Place the dish on a clean, dry surface for approximately 30 seconds. F. Place the cooled dish on the balance and record the weight as (C). V. CALCULATIONS A. Percent Solids = C A B A x 100 Naformátováno PROCEDURE NUMBER: AP.4101.01 PAGE: 1 of 1 I. PROCEDURE DESCRIPTION: Gravimetric procedure to determine Percent Solids in the Shadow Conductive Colloid 2 bath. II. EQUIPMENT & SETTINGS A. Aluminum dish (Fisher Cat# 08-732 or VWR Cat# 25433-008)
SHADOW Conductive Colloid 2 14 of 19 B. Infrared Lamp, 250 watt C. Analytical Balance (0.001g capacity) III. REAGENTS A. None IV. PROCEDURE A. Weigh the aluminum dish on the analytical balance. Record as (A). B. Place a 5 ml sample of Shadow bath into the aluminum dish. Record the weight as (B). C. Place the sample under the infrared lamp. The lamp height should be 3-5 inches from the sample. (Adjust lamp height to obtain 110 o C 125 o C. This can be checked by placing a thermometer under the lamp for a minimum of 10 minutes.) D. Turn lamp on and allow to evaporate for 30 minutes. E. Place the dish on a clean, dry surface for approximately 30 seconds. F. Place the cooled dish on the balance and record the weight as (C). V. CALCULATIONS A. Percent Solids = C A B A x 100
SHADOW Conductive Colloid 2 15 of 19 PROCEDURE NUMBER: AP.102.02 PAGE: 1 of 1 I. PROCEDURE DESCRIPTION: Procedure to determine ph in a Shadow bath. II. EQUIPMENT & SETTINGS A. ph Meter III. REAGENTS A. ph 7 Buffer Solution B. ph 10 Buffer Solution IV. PROCEDURE A. Standardize the ph meter with fresh 7 and 10 ph buffer solutions. B. Measure the ph of the solution with the meter. C. Record the result. V. CALCULATIONS A. None PROCEDURE NUMBER: AP.102.01 PAGE: 1 of 1 I. PROCEDURE DESCRIPTION: Procedure to determine ph in the Shadow Conductive Colloid 2 bath. II. EQUIPMENT & SETTINGS A. ph Meter III. REAGENTS A.pH 7 Buffer Solution B. ph 10 Buffer Solution IV. PROCEDURE A.Standardize the ph meter with fresh 7 and 10 ph buffer solutions. B.Measure the ph of the solution with the meter. C. Record the result. Naformátováno: Odrážky a číslování Naformátováno: Odrážky a číslování V. CALCULATIONS
SHADOW Conductive Colloid 2 16 of 19 A. None
SHADOW Conductive Colloid 2 17 of 19 PROCEDURE NUMBER: AP.4304.01 PAGE: 1 of 1 I. PROCEDURE DESCRIPTION: Procedure to determine Settling in the Shadow Conductive Colloid 2 bath. II. EQUIPMENT & SETTINGS A. 100 ml Glass Graduated Cylinder III. REAGENTS A. None IV. PROCEDURE A. Take a sample from the Shadow sump that has been recirculating for at least two hours. B. Fill the 100 ml glass graduated cylinder with Shadow to 100 ml mark. Tilt the cylinder while pouring slowly. This will prevent the Shadow from obscuring the solution level on one side. When nearing the mark, stand the cylinder upright making sure the bottom of the meniscus is at the 100 ml mark. C. Place the cylinder in an area where it can remain undisturbed for 24 hours. D. After 24 hours, measure the amount of water (top layer) that has separated from the colloid. E. Record the volume in ml as percent settling. V. CALCULATIONS A. None
SHADOW Conductive Colloid 2 18 of 19 PROCEDURE NUMBER: AP.2102.03 PAGE: 1 of 2 I. PROCEDURE DESCRIPTION: Titrimetric procedure to determine Copper concentration in the Shadow Conductive Colloid bath. II. EQUIPMENT & SETTINGS A. 250 ml beaker B. 500 ml Erlenmeyer flask C. 25 or 50 ml burette D. 10 ml class A pipette E. Glass Fiber filter paper Whatman 934-AH (125 mm) (or equivalent) Whatman No. 1827-125, Fisher Cat# 09-873J F. Buchner-type funnel and flask sized for 125 mm paper, aspirator needed G. 50 ml Graduated cylinder III. REAGENTS A. 0.01 M EDTA - Add 3.7224 grams of disodium EDTA salt to 1 liter of DI water and dissolve. B. Nitric Acid, 75% v/v Add 750 ml of concentrated nitric acid slowly to 250 ml of DI water. Dilute to a volume of 1 liter. C. Ammonium Hydroxide, conc. D. Methanol A.C.S. reagent grade E. PAN Indicator, 0.1% Solution - Dissolve 0.1 grams of PAN Indicator, 1-(2-pyridylazo) 2 naphthol, in 100 ml of ACS grade methanol. IV. PROCEDURE A. Pipette 10 ml of the Shadow Conductive Colloid sample into a 250 ml beaker. B. Add about 50 ml of DI water to the beaker and mix.
SHADOW Conductive Colloid 2 19 of 19 PROCEDURE NUMBER: AP.2102.03 PAGE: 2 of 2 C. Add 10 ml of the 75% nitric acid solution to the beaker and mix. Let the beaker stand for 10 minutes. D. Filter the solution into a 500 ml flask using the glass fiber filter. Wash the precipitate with 20 30 ml of DI water. Re-filter, if needed, until the solution is clear. E. Add about 20 ml of ammonium hydroxide and mix. F. Add about 20 ml of methanol and mix. G. Add about 3 drops of PAN indicator and titrate with 0.01 M EDTA to the first color change. V. CALCULATIONS A. g/l copper = (ml of EDTA) (M of EDTA) (63.54) 10 ml sample