The solution-phase synthetic approach used the following metal precursors (all purchased from Sigma-Aldrich): platinum acetylacetonate (Pt(acac)2, 97%), nickel (II) acetate tetrahydrate (Ni(Ac)2, 98%), cobalt (II) acetate tetrahydrate (Co(Ac)2, ≥99%), nickel (II) acetylacetonate (Ni(acac)2, 95%), cobalt (II) acetylacetonate (Co(acac)2, 97%), and molybdenum hexacarbonyl (Mo(CO)6, 98%). Oleylamine (OAm, 70%) and hexadecylamine (HDA, 90%) were employed as surfactants and benzyl ether (BE, 98%) as a high-boiling point solvent. Solvents (Sigma-Aldrich), such as absolute ethanol, acetone, and chloroform, used for precipitating, cleaning, and re-dispersing the particles, were all of analytical grade. All the chemicals were used as received without any further purification.
Molybdenumhexacarbonyl
Manufactured by Merck Group
Sourced in Germany, France
Molybdenumhexacarbonyl is an organometallic compound with the chemical formula Mo(CO)6. It is a colorless, volatile solid used as a precursor in chemical vapor deposition processes for the deposition of molybdenum thin films.
Automatically generated - may contain errors
Lab products found in correlation
Nickel 2 acetylacetonate, by Merck Group (2 mentions)
Tungsten hexacarbonyl, by Merck Group (2 mentions)
Oleic acid, by Merck Group (2 mentions)
Platinum acetylacetonate, by Merck Group (1 mentions)
Absolute ethanol, by Merck Group (1 mentions)
Cobalt 2 acetate tetrahydrate, by Merck Group (1 mentions)
Cobalt 2 acetylacetonate, by Merck Group (1 mentions)
Chloroform, by Merck Group (1 mentions)
Acetone, by Merck Group (1 mentions)
Nickel 2 acetate tetrahydrate, by Merck Group (1 mentions)
Nafion solution, by Thermo Fisher Scientific (1 mentions)
Iron 3 2 4 pentanedionate, by Thermo Fisher Scientific (1 mentions)
Platinum 2 acetylacetonate, by Merck Group (1 mentions)
Oleylamine, by Merck Group (1 mentions)
Glucose, by Merck Group (1 mentions)
Acetone, by Avantor (1 mentions)
Sulphuric acid, by Avantor (1 mentions)
Selenium, by Merck Group (1 mentions)
Ethanol, by Avantor (1 mentions)
Trioctylphosphine, by Merck Group (1 mentions)
8 protocols using molybdenumhexacarbonyl
1
Synthesis of Transition Metal Nanoparticles
2
Synthesis of Diverse Nanomaterials
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Platinum (II) acetylacetonate (Pt(acac)2, 97%), nickel (II) acetylacetonate (Ni(acac)2, 95%), Molybdenumhexacarbonyl (Mo(CO)6, 98%), oleylamine (OAm, >70%) and glucose were bought from Sigma-Aldrich. Cupric acetylacetonate (Cu(acac)2, 98%) was purchased from Energy Chemical. (1-Hexadecyl) trimethylammonium chloride (CTAC, 96%), Tris(2,4-pentanediaonato) Cobalt (III) (Co(acac)3, 98%), Iron (III) 2,4-pentanedionate (Fe(acac)3), Nafion solution (5 wt.%) were supplied by Alfa Aesar. Methanol, cyclohexane, ethanol, and isopropanol were bought from Beijing Tongguang Fine Chemicals Company. Potassium hydroxide (KOH, 90%) was purchased from Aladdin.
3
Synthesis and Characterization of Transition Metal Precursors
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Molybdenum hexacarbonyl (Mo(CO)6, ≥99.9% trace metals basis), tungsten hexacarbonyl (W(CO)6, 99.99% trace metals basis, excluding Mo), selenium (99.99% trace metals basis, 100 mesh), trioctylphosphine (TOP; 90%, technical grade), oleic acid (90%, technical grade), nitric acid (90%, ACS Reagent), and graphitic carbon foil (CF, 99.8%) were purchased from Sigma-Aldrich. Acetone (≥99%, technical grade), ethanol (96%, AnalaR NORMAPUR), and sulphuric acid (95%, AnalaR NORMAPUR) were purchased from VWR. Toray carbon paper (CP) was purchased from Alfa Aesar. Tungsten (Pure standard, 1000 μg mL−1 in H2O), molybdenum (Pure standard, 1000 μg mL−1 in H2O), and selenium (Pure standard, 1000 μg mL−1 in H2O, 2% HNO3) reference standards for ICP were purchased from PerkinElmer. All reagents were used without purification. trioctylphosphine was stored in an Ar filled glovebox to prevent oxidation.
1 M trioctylphosphine selenide (TOP:Se) stock solution was prepared by dissolving 5 mmol (395 mg) of Se powder in 5 mL of trioctylphosphine at room temperature under dry N2 atmosphere. 0.0125 M tungsten and molybdenum stock solutions were prepared by dissolving 0.125 mmol of the respective hexacarbonyl (either 33 mg of Mo(CO)6 or 44 mg of W(CO)6) in 10 mL of degassed oleic acid for 1 hour at 200 °C under vacuum. The ready stock solutions were stored in sealed glass vials in a drying desiccator.
1 M trioctylphosphine selenide (TOP:Se) stock solution was prepared by dissolving 5 mmol (395 mg) of Se powder in 5 mL of trioctylphosphine at room temperature under dry N2 atmosphere. 0.0125 M tungsten and molybdenum stock solutions were prepared by dissolving 0.125 mmol of the respective hexacarbonyl (either 33 mg of Mo(CO)6 or 44 mg of W(CO)6) in 10 mL of degassed oleic acid for 1 hour at 200 °C under vacuum. The ready stock solutions were stored in sealed glass vials in a drying desiccator.
4
Synthesis of Metal Carbonyl Compounds
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Molybdenumhexacarbonyl (Mo(CO)6, 98%) was bought from Sigma–Aldrich. Hexacarbonylchromium (Cr(CO)6, 99%) and Octacarbonyldicobalt (Co2(CO)8) were supplied by Alfa Aesar. Triruthenium dodecacarbonyl (Ru3(CO)12, 98%) was purchased from Aladdin. Carbon nanotube was bought from Aladdin.
5
Synthesis of Nanoparticle Precursors
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Molybdenum hexacarbonyl (Mo(CO)6, 98%), tungsten hexacarbonyl (W(CO)6, 99.99 %), tetradecylphosphonic acid (TDPA, 97%), oleic acid (OA, technical, 90%), and diphenyl diselenide (Ph2Se2, 98%) were purchased from Sigma-Aldrich (Darmstadt, Germany). Solvents, including toluene (99.5%) and n-butanol (99%), were purchased from Duksan (Ansan, South Korea). All chemicals were used as received, without further purification.
6
Synthesis of MoS2/γ-Al2O3 and Carbonyl-Based Catalysts
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MoS2/γ-Al2O3 catalyst precursors
were prepared by incipient
wetness impregnation of γ-Al2O3 (provided
by the Chevron company) with an ammonium heptamolybdate (99.98% purity;
Sigma-Aldrich) solution of appropriate concentration. The impregnated
sample was dried at 383 K overnight followed by calcination in 100
mL·min–1 synthetic air (temperature ramp: 5
K·min–1 to 673 K, hold for 2 h).
Carbonyl-based
catalyst precursors were prepared by chemical vapor deposition (CVD).
Approximately 200 mg of NaY (Zeolyst CBV100; Si/Al ∼ 2.5; pelletized
and sieved to 250–355 μm) was treated under reduced pressure
(10–2 mbar) at elevated temperatures (temperature
ramp: 5 K·min–1 to 408 K, held for 2 h; 5 K·min–1 to 503 K, held for 2 h; 5 K·min–1 to 653 K, held for 1 h) to carefully remove adsorbed water. Molybdenum
hexacarbonyl (>99.9% purity; Sigma-Aldrich) was loaded on the dried
zeolite at room temperature under static conditions for a defined
amount of time. In the final step, the catalyst precursors were treated
under reduced pressure (10–2 mbar) for 10 min to
remove physisorbed Mo(CO)6. All carbonyl-based precursors
were stored in a glovebox to avoid exposure to air/moisture at any
time.
were prepared by incipient
wetness impregnation of γ-Al2O3 (provided
by the Chevron company) with an ammonium heptamolybdate (99.98% purity;
Sigma-Aldrich) solution of appropriate concentration. The impregnated
sample was dried at 383 K overnight followed by calcination in 100
mL·min–1 synthetic air (temperature ramp: 5
K·min–1 to 673 K, hold for 2 h).
Carbonyl-based
catalyst precursors were prepared by chemical vapor deposition (CVD).
Approximately 200 mg of NaY (Zeolyst CBV100; Si/Al ∼ 2.5; pelletized
and sieved to 250–355 μm) was treated under reduced pressure
(10–2 mbar) at elevated temperatures (temperature
ramp: 5 K·min–1 to 408 K, held for 2 h; 5 K·min–1 to 503 K, held for 2 h; 5 K·min–1 to 653 K, held for 1 h) to carefully remove adsorbed water. Molybdenum
hexacarbonyl (>99.9% purity; Sigma-Aldrich) was loaded on the dried
zeolite at room temperature under static conditions for a defined
amount of time. In the final step, the catalyst precursors were treated
under reduced pressure (10–2 mbar) for 10 min to
remove physisorbed Mo(CO)6. All carbonyl-based precursors
were stored in a glovebox to avoid exposure to air/moisture at any
time.
7
Synthesis of Molybdenum Complexes
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Molybdenum complexes were either commercially available (molybdenum hexacarbonyl, Sigma-Aldrich, St Quentin Fallavier, France) or synthetized from Mo(CO)6 and the corresponding tertiary phosphines upon treatment with trimethylamine oxide in acetonitrile. Characterization details of the complexes are given in the Supplementary Material.
8
Synthesis of Colloidal Nanocrystals
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Molybdenum hexacarbonyl, sulfur powder, tetrakis(acetonitrile)copper(i ) hexafluorophosphate (97%), and 1-octadecene (ODE, technical grade 90%) were all purchased from Sigma-Aldrich. Oleylamine (OLA, >50%) was purchased from TCI. The solvents such as hexanes (certified ACS grade) were acquired from Fisher Scientific. Ethanol (200 proof) was brought from Decon Laboratories, Inc. All chemicals were used as received without further purification.
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