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1 E2S Denver Convention Center Denver, Colorado Paul Brezovec, CEF, CTC Michael Miller, CTC Testing Room Temperature Ionic Liquid Solutions for Depot Repair of Aluminum Coatings Wednesday, June 16, 2010

2 Outline A. Background of need B. Problem with incumbent coating C. Reason for ionic liquids as electrolytes D. Safety issues 2

3 Background Need to repair aluminum (Al) coatings a) Pure (> 99%) Al coating electrodeposit b) Steel part surfaces c) Coating is not all within the line of sight There would be two major requirements: a) The repair process would comply with facility environment, safety and occupational health (ESOH) b) The coating would conform with MIL-DTL-83488, Detail Specification Coating, Aluminum, High Purity 3

4 Incumbent Aluminum Coating The incumbent Al coating is electrodeposited on the part by original equipment manufacturers It serves as a cadmium coating replacement The Al coating itself is considered to be safe However, adopting this Al coating technology poses processing issues for a repair facility Uses an aluminum organyl and salt in an aromatic solvent electrolyte, which is air/moisture sensitive Ignites spontaneously in air Requires stringent controls to eliminate moisture contact, and mitigate the fire hazard in the facility 4

5 Ionic Liquid: Definition An ionic liquid (IL) is a salt in the liquid state Discussion will be limited to a room-temperature IL (RTIL) which has a melting point that is less than 100 C For example, BMIM-PF 6 is an RTIL; table salt is not Source: Wikipedia sodium (Na + ) chloride (Cl - ) Table Salt (NaCl) Crystal Melting Point = 801 C Source: Wikipedia 1-butyl-3-methylimidazolium (BMIM + ) hexafluorophosphate (PF 6- ) Ionic Liquid (BMIM-PF 6 ) Melting Point = 11 C 5

6 Example RTIL Anions/Cations Cations Alkylated imidazolium Alkylpyridinium Dialkylpyrrolidinium / Dialkylpiperidinium Tetraalkylammonium Tetraalkylphosphonium Anions Trifluoroacetate Bromide (Cl ) Chloride (Br ) Hexafluorophosphate Tri-fluoromethane sulfonate Tricyanomethide Tetrafluoroborate Trialkylsulfonium RTIL anion/cation pairings Bis(trifluoromethyl sulfonyl)imide They are used to dissolve metal salts and additives for electroplating They become the electrolyte in place of an aqueous solution 6

7 RTIL Features Negligible vapor pressure Non-flammable Remain liquid within a wide temperature range Other properties may be tailored by the anion/cation selection Physicochemical properties Electrochemical properties Instances of existing equipment used for conversion to RTIL-based processing but expect some equipment modifications 7

8 Claimed Plating Opportunities Inert 1 H IIA IIIA IVA VA VIA VIIA He 2 Li Be B C N O F Ne 3 Na Mg IIIB IVB VB VIB VIIB VIIIB IB IIB Al Si P S Cl Ar K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn Fr Ra Ac Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr = As Metal = As Alloy = As Metal and Alloy Reference: Endres, F., A.P. Abbott, and D.R, MacFarlane, Ed., Electrodeposition from Ionic Liquids, Wiley-VCH, Weinheim, Germany, Opportunity of new plating alloys (e.g., Nb) Plating of active elements (e.g., Mg, Mo, Ta, Ti) Quality of plating is not quantitatively reported 8

9 Select Al Electroplating in RTIL Options based on the research literature Cation Dialkyimidazolium Tetraalkylammonium Tetraalkylphosphonium Dialkylpyrrolidinium Anion Chloride Bis(trifluoromethylsulfonyl)imide ( TFSI ) Down-select, based on commercial availability 1-ethyl,3-methylimidazolium chloride ([EMIM]Cl) 9

10 Electroplating Al in [EMIM]Cl Aluminum chloride (AlCl 3 ) dissolves in [EMIM]Cl, forming [EMIM]chloroaluminates: [EMIM]Cl + AlCl 3 [EMIM]AlCl 4, and [EMIM]AlCl 4 + AlCl 3 [EMIM]Al 2 Cl 7 Electrolyte is supplied pre-mixed Al plates (Al ) when there are more dissolved Al atoms than EMIM molecules: 4[EMIM]Al 2 Cl 7 + 3e Al + 4[EMIM]AlCl 4 + 3AlCl 4 100% plating efficiency at 4 amperes/decimeter 2 (A/dm 2 ), claimed 10

11 Al Plating from RTIL Electrolyte Overview: 1. Remove soils/corrosion products/plating from surfaces 2. Activate the substrate (standard method); dry 3. Electroplate Al onto the activated areas: Pure Al anodes Elevated electrolyte temperature improves activity Mechanical agitation Current density of 4 A/dm 2 (example) 4. Rinse and dry plating; Inspect the plating quality 11

12 Safety Considerations 1. Water (H 2 O) contamination Reacts with chloroaluminate (AlCl 4 ) anions: AlCl 4 + H 2 O AlOCl 2 + 2HCl Liberates hydrogen chloride (HCl) gas Forms oxychloroaluminate (AlOCl 2 ) ) Slows plating rate; requires AlCl 3 additions Build-up of AlOCl 2 requires recycling Design limits H 2 O contamination Process allows for < 0.1 % H 2 O by weight 12

13 Safety Considerations (continued) 2. Voltage excursion above ~2.7 volts Chloride anion oxidize to chlorine at anode 4AlCl 4 2Al 2 Cl 7 + Cl 2 + 2e. 3. Electrolyte handling Electrolyte is a superacid Personal protective equipment required Face shield, goggles Nitrile gloves with elbow extension 13

14 Summary 1. A method to repair electroplated aluminum is a option using a near-commercial RTIL electrolyte, [EMIM]Cl-AlCl The specification for pure aluminum deposits, MIL-DTL-83488, may apply. 3. Compliance with ESOH requirements require further hands-on review, including designs for container covers. 14

15 Contacts Paul Brezovec, CEF Concurrent Technologies Corporation 100 CTC Drive Johnstown, PA Ph: (814) Michael Miller Concurrent Technologies Corporation th Avenue Largo, FL Ph: (727)

16 Putting ideas into action. SM CTC

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