Three precursors [nickel (K2Ni(CN)4), cobalt (K3Co(CN)6), and iron (K4Fe(CN)6)] were purchased from Sigma Aldrich. When they were dissolved in DI water alone, pH values measured with a pH meter (PH-8100PLUS, NAVMRO) of 0.1 M K2Ni(CN)4, K3Co(CN)6 and K4Fe(CN)6 were 9.1, 9.0, and 8.4, respectively. Because the protonation of the N atom in P4VP is difficult in the basic solution, we controlled the pH of the precursor solution by using buffer solution (Samchun Chemicals) with various pH ranging from 4 to 7. The concentration of all precursors in the buffer solution was fixed at 0.1 M.
K3 co cn 6
Manufactured by Merck Group
K3[Co(CN)6] is a chemical compound used as a laboratory reagent. It consists of a cobalt(III) center coordinated to six cyanide ligands. This compound is commonly used in various chemical analyses and reactions.
Automatically generated - may contain errors
Lab products found in correlation
K4fe cn 6, by Merck Group (1 mentions)
K2ni cn 4, by Merck Group (1 mentions)
Triethylamine, by Thermo Fisher Scientific (1 mentions)
K3fe cn 6, by Merck Group (1 mentions)
Cu no3 2 3h2o, by Merck Group (1 mentions)
Ethanedithiol, by Thermo Fisher Scientific (1 mentions)
Sodium citrate na3c6h5o7 2h2o, by Merck Group (1 mentions)
Ga no3 3, by Merck Group (1 mentions)
Fecl2, by Merck Group (1 mentions)
Ni no3 2 6h2o, by Merck Group (1 mentions)
Co no3 2 6h2o, by Merck Group (1 mentions)
Acs reagent, by Merck Group (1 mentions)
Methylamine hydrochloride, by Merck Group (1 mentions)
8 protocols using k3 co cn 6
1
Synthesis of Metal-Organic Frameworks
2
Synthesis of Metal-Organic Coordination Complexes
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Triethylamine, activated carbon (AC), 4-vinylbenzyl chloride (pCMS), and ethanedithiol were purchased from Alfa Aesar (China). Cu(NO3)2·3H2O, benzene tricarboxylic acid (BTC), 2,2′-azobis(2-methylpropionitrile) (AIBN), K2Pt(CN)4, K3Co(CN)6, CuCN, and K3Fe(CN)6 were purchased from Sigma-Aldrich. All other reagents used in this study were commercially available analytical-grade reagents. Cu(CN)32− was prepared according to literature report [11 (link)]. The metal salts were mixed together in water as needed.
3
Cobalt Disulfide Nanoparticle Synthesis
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First, the cobalt Prussian blue analogue (Co-PBA), namely Co3[Co(CN)6]2 powder, was used as a starting material before sulfurization. The Co-PBA was synthesized through a facile precipitation method. Two types of solutions were used for precipitation. The recipe for the type 1 solution was 30 mM cobalt acetate (Co(CH3COO)2∙4H2O, Aldrich) and 17 mM sodium citrate (Na3C6H5O7∙2H2O, Sigma-Aldrich) in deionized water (DIW). The concentration of potassium hexacyanocobaltate (III) (K3[Co(CN)6], Sigma-Aldrich) was 20 mM in DIW41 (link). Then, the type 1 solution was dropwise added into the type 2 solution through a syringe pump at 400 ml/hr and vigorously stirred for 10 min. Subsequently, the mixed solution was aged for 18 hours at room temperature. The dispersed precipitate was filtered through a vacuum pump and washed with DIW several times to remove residues. Finally, the obtained powder was dried in an oven at 60 °C for 12 hours.
Second, the cobalt disulfide (CoS2) nanoparticles were synthesized through thermal treatment. The 30 mg of the synthesized Co-PBA and certain amounts of sulfur (S, Sigma-Aldrich) were loaded in a 5 ml ampoule. After that, the prepared ampoule was sealed through a vacuum pump under 0.1 Torr. Finally, the sealed ampoule was thermally treated in a furnace at 500 °C for 2 hours at a ramp rate of 5 °C/min7 (link).
Second, the cobalt disulfide (CoS2) nanoparticles were synthesized through thermal treatment. The 30 mg of the synthesized Co-PBA and certain amounts of sulfur (S, Sigma-Aldrich) were loaded in a 5 ml ampoule. After that, the prepared ampoule was sealed through a vacuum pump under 0.1 Torr. Finally, the sealed ampoule was thermally treated in a furnace at 500 °C for 2 hours at a ramp rate of 5 °C/min7 (link).
4
Synthesis of GaHCCo Nanoparticles
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GaHCCo nanoparticles (NPs) were synthesized by a co-precipitation method involving the simultaneous dropwise addition of 100 mL Ga(NO3)3 (0.01 M) (Sigma-Aldrich) and 100 mL K3[Co(CN)6] (0.01 M) (Sigma-Aldrich) to 200 mL deionized H2O. The entire synthesis process was carried out at 80 °C with vigorous stirring. The formation of a precipitate was observed after a period of heating. After a cooling of the mixture to room temperature, the precipitate was separated and rinsed with large amounts of deionized water several times to remove the impurity ions (such as K+) and subsequently dried in a vacuum oven at 60 °C; it was then ready for subsequent use.
5
Synthesis of FeHCCo and CeHCCo Nanoparticles
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FeHCCo NPs were synthesized by a coprecipitation method by simultaneous
dropwise addition of 100 mL of FeCl2 (0.03 M) (Sigma-Aldrich)
and 100 mL of K3[Co(CN)6] (0.03 M, Sigma-Aldrich)
to 100 mL of H2O under constant stirring; a milky white
precipitate ensued immediately. After sonicating for 30 min, the suspension
was allowed to sit for 1 h. The precipitate was separated and rinsed
several times with a large amount of deionized water and ethanol.
It was then dried in an oven at 60 °C for further use. The synthesis
of CeHCCo was carried out in a similar manner, except that cerium(III)
nitrate hexahydrate (Samchun, 0.03 M) was used as the initial reactant
and the codeposition process was performed at 80 °C. During the
synthesis of CeHCCo, a transparent solution, without any deposition,
was obtained at room temperature, which suggested the requirement
of heating treatment. In the deliberation for the appropriate heating
temperature, the maximum value attainable for aqueous solutions is
100 °C. However, a transparent solution obtained at 60 °C
indicates that a higher temperature is warranted. We thus synthesized
CeHCCo at 80 °C, and a white deposition was obtained.
dropwise addition of 100 mL of FeCl2 (0.03 M) (Sigma-Aldrich)
and 100 mL of K3[Co(CN)6] (0.03 M, Sigma-Aldrich)
to 100 mL of H2O under constant stirring; a milky white
precipitate ensued immediately. After sonicating for 30 min, the suspension
was allowed to sit for 1 h. The precipitate was separated and rinsed
several times with a large amount of deionized water and ethanol.
It was then dried in an oven at 60 °C for further use. The synthesis
of CeHCCo was carried out in a similar manner, except that cerium(III)
nitrate hexahydrate (Samchun, 0.03 M) was used as the initial reactant
and the codeposition process was performed at 80 °C. During the
synthesis of CeHCCo, a transparent solution, without any deposition,
was obtained at room temperature, which suggested the requirement
of heating treatment. In the deliberation for the appropriate heating
temperature, the maximum value attainable for aqueous solutions is
100 °C. However, a transparent solution obtained at 60 °C
indicates that a higher temperature is warranted. We thus synthesized
CeHCCo at 80 °C, and a white deposition was obtained.
6
Synthesis of High-Concentration K-Doped NiCo2O4
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All chemicals were used as received without further purification. The composition of the precursor solution was determined by the stoichiometry of the final compound, NiCo2O4. Ni(NO3)2·6H2O (Sigma Aldrich, 99.999%) and Co(NO3)2·6H2O (Sigma Aldrich, ≥99%) were dissolved in distilled water (40 mL) to concentrations of 0.333 M (3.877 g) and 0.267 M (3.104 g), respectively, and this solution was slowly (over 3 min) poured into a 0.400 M (5.317 g) solution of K3[Co(CN)6] (Sigma Aldrich, ≥97%) in distilled water (40 mL) at room temperature (∼25 °C). After 10 min stirring, the reaction mixture was transferred to an autoclave, heated at 100 °C for 1 h, cooled to room temperature, and filtered. The K–Ni–Co-PBA precipitate was washed with distilled water (5 × 100 mL), dried overnight at 60 °C, heated to 250 °C at 1 °C min−1, and maintained at this temperature for 3 h to induce the formation of high-concentration K-doped NCO (HK-NCO). For comparison, low-concentration K-doped NCO (LK-NCO) was prepared without the hydrothermal process. When synthesis was performed using 80 mL of distilled water, the catalyst was obtained in a high yield of 3.46 g (0.4325 g/10 mL distilled water), which demonstrated the upscalability of our method.
7
Synthesis of Methylammonium Hexacyanometallates
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Single crystals of the methylammonium derivatives (CH 3 NH 3 ) 2 [KCo(CN) 6 ] (1) and (CH 3 NH 3 ) 2 [KFe(CN) 6 ] (2) were prepared by a reaction of methylamine hydrochloride (Sigma, ≥98%) with K 3 Fe(CN) 6 (Sigma-Aldrich, ACS reagent, ≥99.0%) and K 3 Co(CN) 6 (Sigma-Aldrich, ≥97.0%) in a molar ratio of 3 : 1. In the case of (1), 0.012 mol of K 3 Co(CN) 6 and 0.036 mol of CH 3 NH 3 Cl were dissolved in distilled water (∼50 ml), and for crystal (2) 0.012 mol of K 3 Fe(CN) 6 was added to 0.032 mol of CH 3 NH 3 Cl in an aqua solution (∼50 ml). After a few days pale yellow crystals of (1) and deep red crystals of (2) were obtained, and the yield of the synthesis was ca. 70%. The crystalline product was then only once recrystallized from deionized water, because in the case of the crystal with Fe, multiple crystallization causes the formation of Prussian Blue. The dimensions of the single crystals chosen for either crystallographic or dielectric measurements were of course different and suitable for a particular method. The purity of the compounds was confirmed by an elemental analysis.
8
Aqueous Synthesis of Coordination Complexes
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FeCl2 and K3Co(CN)6 chemicals used in this work were reagent grade and were purchased from Sigma-Aldrich. Housedistilled water was further purified with Barnstead NANO Pure II system and was used throughout this work. All experiments were carried out at room temperature and in air, except the dehydration of the sample carried on in oven at 70°C.
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