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Persulfates Ammonium, sodium, and potassium persulfates modified by certain catalysts have been adopted for the etching of copper in PC manufacturing. Continuous regenerative systems and a batch system using ammonium persulfate are no longer used.Wide use is made of persulfates as a microetch for innerlayer oxide coating and copper electroless and plating processes. Persulfate solutions allow all common types of resists on boards including solder, tin, tin/nickel, screened inks, and photosensitive films. Formulations of ammonium persulfate catalyzed with mercuric chloride are no longer used, primarily because of environmental issues, costs, and improved alternatives. In general, persulfate etchants are unstable and will exhibit decomposition, lower etch rates vs. copper content, and lower useful copper capacity. 34.4.4.1 Chemistry. Ammonium, potassium, and persulfates are stable salts of persulfuric acid (H2S2O8). When these salts are dissolved in water, the persulfate ion (S2O82 ) is formed. It is the most powerful oxidant of the commonly used peroxy compounds. During copper etching, persulfate oxidizes metallic copper to cupric ion as shown: Cu + Na2S2O8 CuSO4 + Na2SO4 (34.12)

Persulfate solutions hydrolyze to form peroxy monosulfate ion (HSO41 ) and, subsequently, hydrogen peroxide and oxygen. This hydrolysis is acid catalyzed and accounts for the instability of acidic persulfate etching solutions. Ammonium persulfate solution, normally made up at 20 percent, is acidic. Hydrolysis reactions and etchant use cause a reduction of the pH from 4 to 2. The persulfate concentration is lowered, and hydrated cupric ammonium sulfate [CuSO4 (NH4)2SO4 6H2O] is formed. This precipitate may interfere with etching. Solid persulfate compounds are stable and do not deteriorate if stored dry in closed containers. Solution makeup composition includes various catalysts, including organic matter and transition metals (Fe, Cr, Cu, Pb, Ag, etc.). Materials for storage must be chosen carefully. Persulfates should not be mixed with reducing agents or oxidizable organics. The useful capacity of the etchant is about 7 oz/gal copper at 100 to 130 F. Above 5 oz/gal of copper, it is necessary to keep the solutions at 130 F to prevent salt crystallization. The etch rate of a solution containing 7 oz/gal of dissolved copper is 0.00027 in/min at 118 F. 34.4.4.2 Batch Operation. Sodium persulfate is preferred because it has minimal disposal problems and somewhat higher copper capacity and etch rates. A composition of 3 lb/gal sodium persulfate with 15 ppm of HgCl2, 1 gal of proprietary additive, and 57 ml/gal of H3PO4 has been successfully used for batch-type spray etching.27 Etch rates vary throughout bath life and range from 0.0018 to 0.0006 in/min for copper content of 0 to 7 oz/gal. Prepared solutions must be aged for 16 to 72 h before etching when proprietary additives are used. 34.4.4.3 Problems with Persulfates

1. Low etch rates. Since the solution may decompose, it will be necessary to replace the bath. If solution is new, add more catalyst and check for iron contamination. 2. Salt crystallization. Salts crystallize on the board and cause streaks, damage the solder plate, and plug the spray nozzles or filters. When copper content is high, blue salts may precipitate. 3. White films on solder surface. This may occur normally or when the lead content in the solder plate is too high. 4. Black film on solder. This condition can result when the solder alloy is high in tin. If solder reflow or component soldering is to follow, activate by tin immersion or with solder brighteners. Adjust phosphoric acid content in etchant and solder-plating conditions. 5. Spontaneous decomposition of etch solution. This breakdown is due to contaminated, overheated, or idle solutions. Ammonium persulfate etchants are unstable, especially at higher temperatures. At about 150 F, the solution decomposes quickly. Use it soon after mixing.

Remember that no one sees your notes but you. It s perfectly acceptable to mark up the notes any way you please. Just make sure you know what your marks mean. In general, the simpler your system, the better it works. On my notes, I ve marked when to ask a question, turn to a speci c audience member, or hand out samples.

6 Disposal The exhausted etchant consists mainly of ammonium or sodium and copper sulfate with a pH of about 2 Two methods for disposal are: Electrolytic disposition of the copper on the surface of passivated 300 series stainless steel is one disposal method The spent etchant is acidified with sulfuric acid prior to electrolysis Once the copper has been removed, the remaining solution can be diluted, neutralized, checked, and discarded The copper can be removed from the cathode Spent sodium persulfate can be treated with caustic soda Addition of aluminum or iron machine turnings to a slightly acidified solution is another practical but possibly more difficult means of removing the dissolved copper The reaction, especially in the presence of chloride ions, will be violent, and considerable heat will be given off if the solutions are not diluted 344.