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ACID COPPER SULFATE SOLUTIONS AND OPERATION
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The preferred industrial process uses an acid copper sulfate solution containing copper sulfate, sulfuric acid, chloride ion, and organic additives.
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Solution Makeup by Current Density Using the proper additives, the resultant copper is fine-grained with tensile strengths of 50,000 lb/in.2 (345 MPa), a minimum of 10 percent elongation, and a 1.2 surface-to-hole thickness ratio (see Table 29.4).
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Agitation Air (vigorous) is agitated from an oil-free source at 70 to 80 F. Or e-ductors (airless high-volume, low-pressure circulation). Filtration The operation is continuous through a 3 to 10 mm filter to control solution clarity and deposit smoothness. Carbon treatment New baths do not require activated carbon purification. Circulation through a carbon-packed filter tube is recommended to control organic contamination; for design and number, consult with supplier. The need for batch carbon treatment is indicated by corner cracking after reflow; dull, pink deposits; and haze, haloing, or comet trails around the PTH. Carbon-treat about every 1,500 (Ah) per gal. The following is the procedure for batch carbon treatment. 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. Pump to the storage tank. Clean out the plating tank. Rinse and clean the tank. Leach with 10 percent H2SO4. Adjust the agitators. Clean the anodes. Heat the solution to 120 F. Add 1 or 2 qt of hydrogen peroxide (35 percent per 100 gal of solution). Dilute with 2 pt water, using low-stabilized peroxide. Air-agitate or mix for 1 hour. Maintain heat at 120 or 140 F. Add 3 or 5 lb. powdered or granular carbon per 100 gal. of solution. For a specific carbon source, seek recommendations from your supplier. Mix for 1 to 2 hour. Pump back to plating tank promptly or within 4 hours. Analyze and adjust. Dummy plate at 10 A/ft2 for 6 hours. Panels should be matte and dull. Replenish with additive. Follow supplier instructions for electrolyzing and start-up.
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Contaminants In general, acid copper tolerates both organic and metallic contaminants. Organic residues may come from cleaners, resists, and certain sulfur compounds. Dye systems usually are more resistant than dye-free systems with respect to certain cleaner constituents.
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Metals should be kept at these maximums: chromium, 25 ppm; tin, 300 ppm; antimony, 25 ppm. Nickel, lead, and arsenic may also cause roughness and other problems.
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Bath Composition
Copper sulfate is the source of metal. Low copper will cause deposit burning; high copper will cause roughness and decreased hole-to-surface thickness ratios or throwing power. Sulfuric acid increases the solution conductivity, allowing the use of high currents at low voltages. However, an excess of sulfuric acid lowers the plating rate, whereas low acid reduces holeto-surface ratio (throwing power). Chloride ion (Cl ) should be controlled at 60 to 80 ppm. Below 30 ppm, deposits will be dull, striated, coarse, and step-plated. Above 120 ppm, deposits will be coarse-grained and dull. The anodes will become polarized, causing plating to stop. Excess chloride is reduced by bath dilution or by dragout. Additive components analysis and control are critical for consistent product quality. The primary analytical tool is CVS, and the Hull cell continues to be a useful complementary tool. Excessive or insufficient additive will cause deposit burning and corner cracking. This condition can be judged by metallographic cross-sectioning and etching. Optimum-quality plated metal is fine-grained and equiaxed (nondirectional) and shows no laminations or columnar patterns. Concerning water quality, the use of DI water and contamination-free materials such as low chloride and iron will give added control and improved deposit quality.
29.6.3.2 Temperature. Optimum throwing power and surface-to-hole ratios are obtained by operating at room temperature (i.e., 70 to 80 F). Lower temperatures cause brittleness, burning, and thin plating. Higher temperatures cause haze in low-current-density areas and reduced throwing power. Cooling coils may be necessary during a hot summer or under heavy operation. 29.6.3.3 Deposition Rate. A thickness of 0.001 in. (1.0 mil) of copper deposits in 54 min. at 20 A/ft2, in 21 min. at 50 A/ft2. 29.6.3.4 Hull Cell. Operation at 2 A will show the presence of organic contamination, chloride concentration, and overall bath condition. However, an optimum Hull cell panel is only a small indication that the bath is in good operating condition, since test results are not always related to production problems. More reliable results are obtained by adjusting the bath before Hull cell testing. See Sec. 29.12.4 for procedures on Hull cell.
Cross-Sectioning Results Troubleshooting Sectioning with etching provides information on the plated copper that explains PTH quality in terms of processing factors. Besides showing the overall quality, cross-sectioning gives information on thickness and on possible problems, such as drilling, cracking, blowholes, and multilayer smear. Copper deposits with columnar or laminar patterns indicate inferior copper properties. Cross sections of optimum copper deposits are fine-grained and equiaxed (structureless) upon etching.
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