Lead (II) acetate trihydrate (99.0–103%), lead (II) chloride (reagent grade, 99%), hydrobromic acid 47% in water, hydroiodic acid 57% in water (stabilized with 1.5% hypophosphorous acid), methylamine 40% in water were purchased from Alfa Aesar. Hydrochloric acid 37% in water was purchased from Sigma Aldrich. The compounds were synthesized as powders according to literature procedure20 . In the case of MAPbCl3 a quantity of 37% HCl double with respect to literature procedure was necessary to dissolve the solid PbCl2. All the syntheses gave crystalline precipitates that were collected on a Büchner funnel under suction. In the case of MAPbI3 the filtration was performed while the solution was still hot (T > 45–50 °C) to avoid the formation of (MA)4PbI6∙2H2O21 . After filtration, the solids were left under suction for at least 30 min to let them dry. MAPbCl3 and MAPbBr3 were then washed with acetone to remove the last traces of the mother solutions and left under suction for additional 30 min. The washing with acetone was not possible in the case of MAPbI3, which immediately decomposes in contact with the solvent, probably because of the traces of water present in the same. So after drying under suction, it was purified by keeping it in vacuum at 100 °C overnight.
Hydroiodic acid
Manufactured by Thermo Fisher Scientific
Hydroiodic acid is a colorless, fuming, and corrosive liquid. It is a strong acid composed of hydrogen and iodine. Hydroiodic acid is commonly used in various industrial and laboratory applications, where its acidic properties are required.
Automatically generated - may contain errors
Lab products found in correlation
Diethyl ether, by Merck Group (2 mentions)
Methanol, by Thermo Fisher Scientific (2 mentions)
Methylamine ch3nh2, by Thermo Fisher Scientific (2 mentions)
Methylamine, by Merck Group (2 mentions)
Hydrochloric acid (hcl), by Merck Group (1 mentions)
Lead 2 acetate trihydrate, by Thermo Fisher Scientific (1 mentions)
Methylamine, by Thermo Fisher Scientific (1 mentions)
Hydrobromic acid, by Thermo Fisher Scientific (1 mentions)
Lead 2 chloride, by Thermo Fisher Scientific (1 mentions)
Absolute ethanol, by Merck Group (1 mentions)
Diethyl ether, by Thermo Fisher Scientific (1 mentions)
Pbcl2, by Merck Group (1 mentions)
Lead 2 iodide, by Merck Group (1 mentions)
Lead 2 oxide, by Merck Group (1 mentions)
N n dimethylformamide dmf dimethyl sulfoxide dmso, by Merck Group (1 mentions)
Hypophosphorous acid h3po2, by Merck Group (1 mentions)
Phenylethylammonium iodide peai, by Greatcell Solar (1 mentions)
Dimethyl sulfoxide (dmso), by Merck Group (1 mentions)
Ethanol, by Thermo Fisher Scientific (1 mentions)
N n dimethylformamide (dmf), by Merck Group (1 mentions)
11 protocols using hydroiodic acid
1
Synthesis and Purification of Methylammonium Lead Halide Perovskites
2
Synthesis of Methyl Ammonium Iodide
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
CH3NH3I was synthesized as our previous literature. Methylamine (CH3NH2) (13.5 mL, 40 wt% in aqueous solution, Alfa Aesar) and hydroiodic acid (HI) (15.0 mL, 57 wt% in water, Alfa Aesar) were stirred at 0°C under nitrogen atmosphere for 2 h. After the reaction, the solvent of the solution was evaporated using a rotary evaporator. A white powder, methyl ammonium iodide (CH3NH3I), was generated by the reaction. The precipitate was washed with diethyl ether (Sigma–Aldrich) three times and dried at 60°C in a vacuum oven overnight1 (link)3 (link)7 (link)25 (link).
3
Synthesis of Chiral Organic Ammonium Halide Salts
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
1.2 mmol of organic amine (R- and S-MBA > 98%; Sigma-Aldrich, St. Louis, MO) and 1.3 mmol of hydroiodic acid in the form of an aqueous solution (57 wt% stabilized with 1.5% hypophosphorous acid; Alfa Aesar, Ward Hill, MA) were mixed with 0.5 mL of absolute ethanol (Merk, Darmstadt, Germany). After vigorous stirring for 12 h, the solution was fully evaporated at 80 °C in a vacuum to synthesize the chiral organic ammonium halide salts.
4
Synthesis and Purification of Methylammonium Iodide and Anhydrous Europium Iodide
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Methylammonium iodide (CH3NH3I) was synthesized and purified based on the method proposed by J. H. Im.54 (link) All chemicals were used as received. Methylammonium iodide (CH3NH3I) was synthesized by mixing methylamine (CH3NH2) (27.8 mL, 0.273 mol, 40 wt% in methanol, Alfa Aesar) and hydroiodic acid (HI) (30 mL, 0.227 mol, 57 wt% in water, Alfa Aesar) in a 250 mL round-bottom flask, and stirring the mixture in an ice-water bath for 2 h. The yellowish raw product obtained by evaporating the solvent was recrystallized three times from a mixture of diethyl ether and ethanol. After filtration, the solid was collected in a dark container and dried at 60 °C in a vacuum oven overnight. Anhydrous EuI2 was synthesized and purified based on the method proposed by Chengpeng D.55 (link) Anhydrous EuI2 was prepared by dissolving europium oxide (Eu2O3) and ammonium iodide (NH4I) into HI to form a transparent solution. We obtained a dense solid after we evaporated the solution. Then the solid was placed into a quartz tube for vacuum dehydration in a tube heating furnace, until it was completely dehydrated. After that, the dehydrated solid was sintered until the solid turned to transparent melt. Eventually, anhydrous EuI2 in bulk polycrystalline was obtained.
5
Synthesis of Methylammonium Iodide
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Methylammonium iodide (CH3NH3I) was synthesized by the method described by Lee et al. (3 (link)). A concentrated aqueous solution of hydroiodic acid [15.0 ml, 57 weight % (wt %) in water; Alfa Aesar] was reacted with methylamine (CH3NH2) (13.5 ml, 40 wt % in aqueous solution; Alfa Aesar) at 0°C for 2 hours with constant stirring under nitrogen atmosphere. Methylammonium iodide was crystallized by removing the solvent using a rotary evaporator. The generated white powder was washed three times with diethyl ether (Alfa Aesar) and then dried in a vacuum overnight.
6
Methylammonium Iodide Synthesis and Purification
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Methylammonium iodide (MAI) was synthesized by reacting 10 ml of hydroiodic acid (57 wt.% in water, Alfa Aesar) with 24 ml of methylamine (33 wt.% in ethanol, Sigma-Aldrich) in ice bath under nitrogen atmosphere with constant stirring. After reacting for 2 h, the resulting white powder of MAI was collected by rotary evaporator at 50 °C. The MAI was dissolved into ethanol and evaporated for further purification. This step was repeated two times, and the MAI powder was finally collected and dried in a vacuum oven at 60 °C for 30 h. Poly(3,4-ethylenedioxythiophene):poly(p-styrene sulfonate) (PEDOT:PSS, Clevios AI 4083) and [6,6]-phenyl-C60-butyric acid methylester (PC60BM) were bought from Heraeus (Germany) and Nichem Fine Technology Co. Ltd. (Taiwan), respectively. To prepare MAPbI3 − xClx (30 wt.%) precursor solution, MAI and PbCl2 (Sigma-Aldrich) were dissolved into N,N-dimethylformamide (DMF) solvent with a molar ratio of 1:1 under constant stirring. The concentration of PC60BM solution was 20 mg/ml in chlorobenzene.
7
Synthesis and Purification of Methylammonium Iodide
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
MAI was synthesized
in our lab. Methylamine solution in alcohol (48 mL, 0 °C cooling)
was added into hydroiodic acid (20 mL) and stirred for 3 h. To guarantee
the complete reaction of hydroiodic acid, the amount of methylamine
was excessive. During the reaction process, N2 was continuously
piped to the solution. The blended solution appeared pale yellow in
color when the reaction was completed. By evaporating the solvents
at 60 °C for 1 h with a rotary evaporator, the precipitated yellow-white
crystal was collected. The products were purified with anhydrous diethyl
ether and collected with a suction filter. Finally, the product, MAI,
was dried in a vacuum oven at room temperature for 24 h. CH3NH3PbI3 solution (40 wt %) was prepared by
adding the MAI powder, PbI2, and DMSO at a mole ratio of
1:1:1 in DMF and stirred for 1 h.
Methylamine, hydroiodic acid,
DMSO, and DMF were all purchased from Alfa Aesar and used as received.
in our lab. Methylamine solution in alcohol (48 mL, 0 °C cooling)
was added into hydroiodic acid (20 mL) and stirred for 3 h. To guarantee
the complete reaction of hydroiodic acid, the amount of methylamine
was excessive. During the reaction process, N2 was continuously
piped to the solution. The blended solution appeared pale yellow in
color when the reaction was completed. By evaporating the solvents
at 60 °C for 1 h with a rotary evaporator, the precipitated yellow-white
crystal was collected. The products were purified with anhydrous diethyl
ether and collected with a suction filter. Finally, the product, MAI,
was dried in a vacuum oven at room temperature for 24 h. CH3NH3PbI3 solution (40 wt %) was prepared by
adding the MAI powder, PbI2, and DMSO at a mole ratio of
1:1:1 in DMF and stirred for 1 h.
Methylamine, hydroiodic acid,
DMSO, and DMF were all purchased from Alfa Aesar and used as received.
8
Synthesis of Lead-Based Perovskite Materials
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Lead(II) oxide (PbO > 99%), lead(II) iodide (PbI2 > 99%), 3-(aminomethyl)piperidine (3AMP), 4-(aminomethyl)piperidine (4AMP), benzylamine, hypophosphorous acid (H3PO2), N,N’-dimethylformamide (DMF), dimethyl sulfoxide (DMSO) and diethyl ether (DEE) were purchased from Sigma Aldrich and used without further purification. Phenylethylammonium iodide (PEAI) was purchased from GreatCell Solar, and hydroiodic acid (HI, 55–58%) was obtained from Alfa Aesar.
9
Synthesis and Deposition of Methylammonium Lead Iodide Perovskite
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Synthesis of methylammonium iodide (CH3NH3I) was carried out by dropwise addition of hydroiodic acid (57 wt%, aqueous, Alfa Aesar) into aqueous methylamine (40 wt%, Sigma Aldrich) under stirring at 0 °C for 2 h. The solvent was then removed by rotary evaporation and the crystals were washed in triplicate with diethyl ether and dried overnight under vacuum.
Equimolar quantities of PbI2 (99%, Acros Organics) and CH3NH3I were dissolved in N,N-dimethylformamide at 200 mg ml−1 to form the CH3NH3PbI3 precursor solution. The solution was heated to 70 °C and stirred for 1 h to ensure full solvation of the precursor components. Glass cover slips were cleaned by first sonicating in detergent solution followed by rinsing with deionized water and a second round of sonication in ethanol. The perovskite precursor solution was deposited on the clean glass substrates by spin coating at 2,000 r.p.m. for 30 s. The films were then treated at 100 °C for 20 min to form CH3NH3PbI3. All preparation steps were carried out in a dry nitrogen atmosphere.
Equimolar quantities of PbI2 (99%, Acros Organics) and CH3NH3I were dissolved in N,N-dimethylformamide at 200 mg ml−1 to form the CH3NH3PbI3 precursor solution. The solution was heated to 70 °C and stirred for 1 h to ensure full solvation of the precursor components. Glass cover slips were cleaned by first sonicating in detergent solution followed by rinsing with deionized water and a second round of sonication in ethanol. The perovskite precursor solution was deposited on the clean glass substrates by spin coating at 2,000 r.p.m. for 30 s. The films were then treated at 100 °C for 20 min to form CH3NH3PbI3. All preparation steps were carried out in a dry nitrogen atmosphere.
10
Perovskite Solar Cell Fabrication
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
PbI2 (99.99%) and chiral (S, R)1-(2-naphthyl)ethylamine (NEA) were
purchased from TCI. Methylammonium iodide (MAI) (>99%) was purchased
from Greatcell Solar. DMF, DMSO and chlorobenzene were purchased from
Sigma-Aldrich. Hydroiodic acid, methanol, ethanol and other solvents
were purchased from Fisher Scientific. All chemicals were directly
used without further purification. Quartz substrates were obtained
from Ossila.
purchased from TCI. Methylammonium iodide (MAI) (>99%) was purchased
from Greatcell Solar. DMF, DMSO and chlorobenzene were purchased from
Sigma-Aldrich. Hydroiodic acid, methanol, ethanol and other solvents
were purchased from Fisher Scientific. All chemicals were directly
used without further purification. Quartz substrates were obtained
from Ossila.
About PubCompare
Our mission is to provide scientists with the largest repository of trustworthy protocols and intelligent analytical tools, thereby offering them extensive information to design robust protocols aimed at minimizing the risk of failures.
We believe that the most crucial aspect is to grant scientists access to a wide range of reliable sources and new useful tools that surpass human capabilities.
However, we trust in allowing scientists to determine how to construct their own protocols based on this information, as they are the experts in their field.
Ready to get started?
Sign up for free.
Registration takes 20 seconds.
Available from any computer
No download required
Revolutionizing how scientists
search and build protocols!