Synthesis of tris(2,2'-bipyridine) ruthenium(II) tetrafluoroborate. Encyclopedia of radio electronics and electrical engineering
Encyclopedia of radio electronics and electrical engineering / Ham Radio Technologies
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Method modified by Jonathan Breitzer and George Lisensky using the following source: John A. Broomhead, Charles G. Young "Inorganic Synthesis" 28, 338-340 (1990)
The coordination complex between the transparent tin oxide electrode and the active metal electrode emits light when an external voltage is applied. Coating too thin a layer of [Ru(bipyridine)3](BF4)2-polyvinyl alcohol will result in a short circuit and no light emission; a coating that is too thick will have too high an electrical resistance and will also result in no radiation.
DryingRuCl3 (enough for 35 preparations)
Rub about 3 g of technical RuCl33H2About in a mortar and pestle and dry the resulting powder in an oven at a temperature of 100 ° C for several hours. The color should change from dark black to dark brown.
Preparation of NaH2PO2from H3PO2(enough for 35 preparations)
Hypophosphorous acid is monobasic (two hydrogen atoms are connected directly to a phosphorus atom) with a dissociation constant of 1,1. Be careful when working! Pour 6 ml of water into a beaker, add 10 ml of 50% H3Ro2 and stir with a magnetic stirrer.
Carefully add the NaOH pellets until the pH of the solution is 6-8. Approximately 3,9 g of NaOH will be required. The resulting solution is approximately a 6 molar NaH solution2PO2.
Preparation of the Ru(II) complex
Dissolve 0,083 g (0,40 mmol) RuCl3· 3H2O in 8 ml of water in a 30 ml beaker fitted with a magnetic stirrer. Add 0,188 g (1,204 mmol) 2,2'-dipyridyl and 0,44 ml NaH2PO2. Cover the beaker with a glass slide and heat under reflux for 30 minutes. Maintain volume by adding water as needed.
Add 0,333 g NaBF4dissolved in 1,5 ml of water. Let the solution cool to room temperature and then cool it on ice until crystals form.
Collect the material obtained by suction filtration and wash it with cold ethanol. Air dry.
[Ru(bipyridine)3](BF4)2 can be applied to manufacturing organic light emitting diode.
Materials
Ruthenium(III) chloride trihydrate (Aldrich 20,622-9)
Hypophosphorous acid, 50% (vol.) aqueous solution (Aldrich 21,490-6)
Sodium hydroxide
2,2'-dipyridyl (Aldrich D21,630-5)
Sodium tetrafluoroborate (Aldrich 20,221-5)
ethanol
Drying oven
pH indicator paper
Mortar and pestle, small beaker, glass slide, suction flask, Hirsch funnel
Publication: cxem.net
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