Tetrachloroauric acid trihydrate (HAuCl4.3H2O, ≥99.9% trace metal basis), sodium borohydride (NaBH4, ≥98.0%), benzyl alcohol and dodecane (≥99%) were purchased from Sigma-Aldrich. L-glutathione (HSG, +98%) and cesium carbonate (99%, metal basis) were obtained from Alfa Aesar, Methanol (HPLC grade) from VWR International, and toluene from Emsure. Zirconium oxide (ZrO2) was prepared from Zr(OH)4 calcined at 550 °C for 12 hours under air flow at a rate of 2 °C/min. All chemicals were used without further purification. All glassware were washed with aqua regia and rinsed with ethanol. Ultrapure water (18 MΩ) was used in all experiments.
Cesium carbonate
Manufactured by Thermo Fisher Scientific
Cesium carbonate is an inorganic compound with the chemical formula Cs2CO3. It is a white, crystalline solid that is soluble in water and acts as a source of the cesium cation (Cs+). Cesium carbonate is commonly used in various laboratory applications, including as a reagent, catalyst, and additive.
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Lab products found in correlation
Oleic acid, by Thermo Fisher Scientific (2 mentions)
1 octadecene ode, by Merck Group (2 mentions)
Benzyl alcohol, by Merck Group (1 mentions)
L glutathione, by Thermo Fisher Scientific (1 mentions)
Hplc grade methanol, by Avantor (1 mentions)
Dodecane, by Merck Group (1 mentions)
Sodium borohydride, by Merck Group (1 mentions)
Tetrachloroauric acid trihydrate, by Merck Group (1 mentions)
Spiro ometad, by Lumtec (1 mentions)
Toluene, by Thermo Fisher Scientific (1 mentions)
Triphenylphosphine oxide, by Merck Group (1 mentions)
1 octadecene, by Thermo Fisher Scientific (1 mentions)
N hexane, by Thermo Fisher Scientific (1 mentions)
N octane, by Thermo Fisher Scientific (1 mentions)
Oleylamine, by Merck Group (1 mentions)
Acetonitrile, by Merck Group (1 mentions)
Sodium acetate, by Merck Group (1 mentions)
Chlorobenzene, by Merck Group (1 mentions)
Ethyl acetate, by Duksan Pure Chemicals (1 mentions)
Empyrean x ray diffractometer, by Malvern Panalytical (1 mentions)
6 protocols using cesium carbonate
1
Synthesis of Gold Nanoparticles with Glutathione
2
Perovskite Solar Cell Fabrication
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All chemicals were purchased from Sigma-Aldrich and used as received unless otherwise specified. Cesium carbonate (Cs2CO3; 99.9%), PbI2 (99.9985%; Alfa Aesar), oleic acid (OA; technical grade, 90%), oleylamine (OAm; technical grade, 70%), 1-octadecene (ODE; technical grade, 90%), hexane (reagent grade, ≥95%), octane (anhydrous, ≥99%), MeOAc (anhydrous, 99.5%), Pb(NO3)2 (99.999%), EtOAc (anhydrous, 99.8%), CsI (99.999%), FAI (Dyesol), FABr (Dyesol), MAI (Dyesol), MABr (Dyesol), ethanol (EtOH; 200 proof, ≥99.5%), titanium ethoxide (≥97%), hydrochloric acid (HCl; 37% in water), 2,2′,7,7′-tetrakis(N,N-di-p-methoxyphenylamine)-9,9′-spirobifluorene (spiro-OMeTAD; ≥99.5%; Lumtec), chlorobenzene (anhydrous, 99.8%), 4-tert-butylpyridine (4-TBP; 96%), bis(trifluoromethane)sulfonimide lithium salt (Li-TFSI), and acetonitrile (anhydrous, 99.8%).
3
Synthesis of Perovskite Solar Cell Materials
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Lead iodide (II) (PbI2, 99.999%), 1‐octadecene (technical grade 90%), oleic acid (technical grade 90%), cesium carbonate (Cs2CO3, 99.99%), n‐hexane (anhydrous), n‐octane (99%), toluene (anhydrous), 2‐pentanol (2‐PeOH, 99%), lithium bis(trifluoromethylsulfonyl)imide (Li‐TFSI, 98%), and 2‐n‐pentylpyridine were purchased from Alfa Aesar. Oleylamine (technical grade 70%), sodium acetate (NaOAc, 99.995%), chlorobenzene (anhydrous 99.8%), and acetonitrile (99.8%), triphenylphosphine oxide (TPPO, 98%), were purchased from Sigma–Aldrich. Phenethylammonium iodide (PEAI) was purchased from GreatcellSolar. 2,20,7,70‐Tetrakis(N,N‐di‐p‐methoxyphenylamine)‐9,90‐spirobifluorene (Spiro‐OMeTAD, ≥ 99.5%) was purchased from Lumtec. Methyl acetate (MeOAc, ≥ 99.5%) and ethyl acetate (EtOAc, ≥ 99.5%) were purchased from Duksan. TiO2 precursor solution (0.15 M), and TiCl4 aqueous solution (2 M) were purchased from Sharechem. Phenyl‐C61‐butyric acid methyl ester (PCBM, ≥99.95%) was purchased from 1‐Materials.
4
Isotopic Enrichment of Cesium Dihydrogen Phosphate
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Isotopic 17O enrichment of CsH2PO4 was performed
by using a methanol induced precipitation method as
described previously6 (link) with the starting
materials, 20% 17O-enriched phosphoric acid (Sigma-Aldrich,
80 wt % in 20% 17O-enriched H2O) and cesium
carbonate (Alpha-Aesar, 99.9%). The synthetic route is identical to
that employed for the nonenriched materials except for the use of
20% 17O-enriched phosphoric acid. The as-prepared 17O-enriched CsH2PO4 was packed and stored
in a rotor for the NMR experiments in a dry argon atmosphere to prevent
any moisture contamination and exchange with nonenriched oxygen ions
(in water). While the enrichment level was not measured post synthesis,
it is likely not much lower than the 20% level of the reagents employed
due to the rapid precipitation method, which limited exposure to ambient
air. The phases present in both pristine and 17O-enriched
CsH2PO4 samples were identified by Powder X-ray
diffraction (PXRD) measurements obtained on a Panalytical Empyrean
X-ray diffractometer using Cu Kα radiation (Figure S1 ) and by 1H NMR (δiso = 10.9 and 14.3 ppm for H1 and H2 at room temperature, respectively5 ,20 ). The PXRD patterns are consistent with the reported monoclinic
phase (space group P21/m).15
by using a methanol induced precipitation method as
described previously6 (link) with the starting
materials, 20% 17O-enriched phosphoric acid (Sigma-Aldrich,
80 wt % in 20% 17O-enriched H2O) and cesium
carbonate (Alpha-Aesar, 99.9%). The synthetic route is identical to
that employed for the nonenriched materials except for the use of
20% 17O-enriched phosphoric acid. The as-prepared 17O-enriched CsH2PO4 was packed and stored
in a rotor for the NMR experiments in a dry argon atmosphere to prevent
any moisture contamination and exchange with nonenriched oxygen ions
(in water). While the enrichment level was not measured post synthesis,
it is likely not much lower than the 20% level of the reagents employed
due to the rapid precipitation method, which limited exposure to ambient
air. The phases present in both pristine and 17O-enriched
CsH2PO4 samples were identified by Powder X-ray
diffraction (PXRD) measurements obtained on a Panalytical Empyrean
X-ray diffractometer using Cu Kα radiation (
phase (space group P21/m).15
5
Synthesis of Colloidal Nanocrystals
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Commercial chemicals, including lead oxide (99.0%, Chengdu Kelong Chemical Reagent Factory), cesium carbonate (99.9%, Alfa Aesar), dimethyldioctadecylammonium bromide (DDOABr, ≥98%, Aldrich), oleic acid (OA, 90%, Aldrich), 1-octadecene (ODE, Aldrich) and hexanoic acid (99.5%, Aldrich), toluene (99.5%), cyclohexane (99.5%) and CDCl3 (99.8%, Adamas) were used as received without further purification.
6
Colloidal Synthesis of Perovskite Nanocrystals
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Acetone (HPLC grade, Fischer Scientific), ethanol (200 proof, anhydrous, Koptec), n-heptane (99%, spectrophotometric grade, Sigma-Aldrich), n-hexane (95%, anhydrous, Sigma-Aldrich), cesium carbonate (Cs 2 CO 3 , 99.9%, metals basis, Alfa Aesar), lead(II) bromide (PbBr 2 , 98%, Sigma-Aldrich), lead(II) iodide (PbI 2 , 99.999%, trace metals basis, Sigma-Aldrich), 1-octadecene (ODE) (95%, Sigma-Aldrich), oleic acid (OAc) (technical grade, 90%, Sigma-Aldrich), oleylamine (OAm) (technical grade, 70%, Sigma-Aldrich), and titanium dioxide paste (Ti-Nanoxide T/SP, solaronix) were used without further purification. VWR Microscope Slides (1 mm thickness)
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