As a requirment in my project, I have to synthesize Formamidinium bromide (FABr). According to the protocols which are mentioned in the articles, I've synthesized this material but I think there is an error in my work?
Does anyone has the experience of this synthesis?
Because in the articles, the authors don't express all the steps, I want to know if there is any critical strategy during the synthesis of FABr and specially in the purification stage of this process.
I would appreciate if you point out a reliable article which has mentioned all the stages of this synthesis with it's details.
Synthesis of formamidinium iodide (FAI) FAI was synthesized via the reaction of FA(OAc) with an excess of hydrogen iodide (57%) upon stirring in an ice bath for 2 h. Subsequently, the solution was dried in a rotary evaporator under vacuum and mild heating (50 °C). The crude product was washed with diethyl ether and recrystallized from ethanol. After drying in a vacuum oven (overnight at 55 °C) a white powder was obtained. Single crystals of FAI, grown via the diffusion of diethyl ether into an ethanol solution of FAI, were used for structure determination (Supplementary Figure 1, for crystallography tables see Supplementary Tables 1–4). The overall purity of the obtained FAI material was confirmed by X-ray powder diffraction (see attachment)
@Sandeep Chandrashekharappa
Thanks for your attention, but the article which you've mentioned was not relevant to what I'm searching for.
@Jürgen Wintner
Thanks for your response. I've actually synthesized FAI, but the challenge is when I do the same procedure for synthesizing FABr, the process fails. And also I didn't find something beneficial in the article which you've send in order to approach to my answer.
Jürgen Wintner For the stirring process in ice bath, do we need vacuum condition for the entire 2 hours or just ambient condition?
Dear Reads Nima Tabatabaei Rezaei,
Have you tried the way I propose to go ahead for the same? Just try it.Somebody has done and successfully got some very interesting synthesis results.
Because of the good thermal stability and superior carrier transport characteristics of formamidinium lead trihalide perovskite HC(NH2)2PbX3 (FAPbX3) has been considered to be a better optoelectronic material than conventional CH3NH3PbX3 (MAPbX3). The FAPbBr3 photodetector’s responsivity to two-photon absorption with an 800-nm excitation source can reach 0.07 A W−1, which is four orders of magnitude higher than that of its MAPbBr3 counterparts. Materials such as Formamidine acetate, lead bromide (PbBr2, > 98%) and hydrobromic acid (48 wt% in water), Gamma-butyrolactone (GBL) and N,N-dimethylformamide (DMF) may required for synthesis.
Formamidinium iodide (FAI) and formamidinium bromide (FABr) can be synthesised by dissolving formamidinium acetate powder in a 2x molar excess of 57%w/w hydroiodic acid (for FAI) or 48%w/w hydrobromic acid (for FABr). FABr can be synthesized by slowly dropping 10 mL hydrobromic acid into 50 mmol (5.205 g) formamidine acetate in a flask, accompanied by continuous stirring at 0 °C for 2 h under argon atmosphere. The product FABr was formed once the solvent was removed using a rotary evaporator at 70 °C. The crude white powder was dissolved in ethanol and subsequently reprecipitated in diethyl ether. Then, the filtered product was dried at 60 °C in a vacuum oven for 24 h for further use.
Ashish
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