0.5 g of molybdenum hexacarbonyl (Mo(CO)6, >99.9%, Sigma Aldrich) powder was dissolved in 50 mL of dimethyl disulfide (CH3SSCH3, >99%, Sigma Aldrich). The mixture was kept in a quartz bubbler. To prevent the agglomeration, the solution was stirred with a magnetic bar on a home-made stirring system.
Mo co 6
Manufactured by Merck Group
Mo(CO)6 is a chemical compound consisting of one molybdenum (Mo) atom and six carbonyl (CO) groups. It is a solid, crystalline substance at room temperature.
Automatically generated - may contain errors
Lab products found in correlation
C2h5 2s, by Merck Group (3 mentions)
Cr co 6, by Merck Group (2 mentions)
Benzoic acid, by Thermo Fisher Scientific (1 mentions)
N n dimethylformamide (dmf), by Thermo Fisher Scientific (1 mentions)
Hclo4, by Merck Group (1 mentions)
Bmim ntf2, by Merck Group (1 mentions)
Ni acac 2, by Merck Group (1 mentions)
Pt acac 2, by Merck Group (1 mentions)
Cr acac 3, by Merck Group (1 mentions)
System 2000 ftir spectrometer, by PerkinElmer (1 mentions)
Ftir 8400s spectrometer, by Shimadzu (1 mentions)
Avance drx 400 mhz nmr spectrometer, by Bruker (1 mentions)
W co 6, by Merck Group (1 mentions)
N n dimethylformamide (dmf), by Merck Group (1 mentions)
10 protocols using mo co 6
1
Molybdenum Hexacarbonyl Solution Preparation
2
Large-Scale MoS2 Monolayer CVD Growth
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The growth of 4-inch wafer-scale MoS2 MLs was achieved using high-purity gas precursors, Mo(CO)6 (99.9%; Sigma-Aldrich) and (C2H5)2S (98%; Sigma-Aldrich). Four-inch quartz and SiO2/p+-Si wafers were placed in the center of a 6-inch hot-walled quartz tube furnace. Before the MOCVD process, the furnace was purged for 1 hour to eliminate residual contaminants, and the temperature was ramped up to 535°C for 30 min. The growth proceeded for 26 hours with partial pressure of precursors of 4.2 × 10−5 torr for Mo(CO)6 and 10−2 torr for (C2H5)2S. The base pressure of the reactor was ~7 torr under the carrier gas flow of 150 standard cubic centimeters per minute (sccm) for Ar (99.9999%) and 1 sccm for H2 (99.9999%).
3
Synthesis and Characterization of SAPO-5 Catalyst
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The SAPO-5 was prepared by hydrothermal
synthesis as reported elsewhere.23 (link),28 (link) To remove
the template, the sample was calcined at 550 °C in air overnight.
The AFI structure of the final product was verified by powder X-ray
diffraction (Figure S1 ) obtained on a PANalytical
Emryrean diffractometer employing Cu Kα radiation and is fully
consistent with data from previous studies.23 (link),28 (link) After calcination, the sample was dehydrated by thermal treatment
at 350 °C under dynamic vacuum (residual pressure <10–4 mbar) overnight in an EPR quartz cell.
Vanadium
incorporation was obtained by an anhydrous vapor exchange process
exposing the sample to the VCl4 vapors in a quartz cell
equipped with an EPR tube. The cell was evacuated after the reaction
to remove excess VCl4 and the reaction products (HCl),
following established protocols.29 (link)The bimetallic system was prepared by treating the calcined SAPO-5
powder with Mo(CO)6 (commercial Sigma-Aldrich) vapors at
room temperature. The metal grafting was obtained by treating the
sample under dynamic vacuum at 200 °C for 1 h. After this, molybdenum
was fully oxidized (Mo6+) by increasing the temperatures
from 100 to 300 °C in the presence of 100 mbar of molecular oxygen.
Lastly, the system was contacted with VCl4 vapors as described
above.
synthesis as reported elsewhere.23 (link),28 (link) To remove
the template, the sample was calcined at 550 °C in air overnight.
The AFI structure of the final product was verified by powder X-ray
diffraction (
Emryrean diffractometer employing Cu Kα radiation and is fully
consistent with data from previous studies.23 (link),28 (link) After calcination, the sample was dehydrated by thermal treatment
at 350 °C under dynamic vacuum (residual pressure <10–4 mbar) overnight in an EPR quartz cell.
Vanadium
incorporation was obtained by an anhydrous vapor exchange process
exposing the sample to the VCl4 vapors in a quartz cell
equipped with an EPR tube. The cell was evacuated after the reaction
to remove excess VCl4 and the reaction products (HCl),
following established protocols.29 (link)The bimetallic system was prepared by treating the calcined SAPO-5
powder with Mo(CO)6 (commercial Sigma-Aldrich) vapors at
room temperature. The metal grafting was obtained by treating the
sample under dynamic vacuum at 200 °C for 1 h. After this, molybdenum
was fully oxidized (Mo6+) by increasing the temperatures
from 100 to 300 °C in the presence of 100 mbar of molecular oxygen.
Lastly, the system was contacted with VCl4 vapors as described
above.
4
Growth of Monolayer MoS2 for aBN/MoS2 Quantum Wells
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Monolayer MoS2 material for aBN/MoS2 quantum well structures is grown via MOCVD. A custom-built MOCVD system is utilized to grow monolayer MoS2 films on 1 cm2 c-plane sapphire substrates (Cryscore Optoelectronic Ltd, 99.996%). Mo(CO)6 (99.99%, Sigma-Aldrich) serves as the Mo precursor and H2S (99.5%, Sigma-Aldrich) provides sulfur during synthesis. Details of the growth process for achieving uniform monolayer MoS2 films have been previously described in our publication51 (link).
5
Monolayer MoS2 Growth via MOCVD
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Monolayer MoS2 films were grown under low pressure by metal-organic chemical vapor deposition (MOCVD)48 (link). Molybdenum hexacarbonyl (Mo(CO)6, Sigma Aldrich) and diethyl sulfide ((C2H5)2S, Sigma Aldrich) which were selected as precursors of Mo and S, respectively, were supplied in the gas phase into a one-inch quartz tube furnace using a bubbler system with Ar as the carrier gas. The MoS2 film was synthesized on a 300 nm-thick SiO2 layer on a Si wafer with a flow rate of 100 sccm for Ar, 0.1 sccm for Molybdenum hexacarbonyl, and 1.0 sccm for diethyl sulfide at a growth temperature of less than 350 °C. The growth time was about 20 h. After growth, the furnace temperature was ramped down to room temperature. The quality of the monolayer MoS2 films was characterized by Raman spectroscopy and photoluminescence (Supplementary Fig. 1c, d ).
6
Scalable MOCVD Synthesis of MoS2 Thin Films
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Large-area MoS2 was synthesized in an
MOCVD growth system
under low-pressure conditions [Figure 1 a]. The system consists of a quartz tube with an inner
diameter of 22 mm (outer diameter = 25 mm) inside a single zone Lindberg/Blue
M furnace. The precursors used for MoS2 growth are molybdenum
hexacarbonyl, Mo(CO)6 (Sigma-Aldrich, CAS number 13939-06-05,
99.9%), and diethyl sulfide, (C2H5)2S (Sigma-Aldrich, CAS number 352-93-2, 98%). The target substrate
used in this work was 285 nm SiO2 grown on highly doped
double-side-polished p-type Si. At the start of the growth process,
the target substrate (measuring 10 cm × 1.7 cm) was placed approximately
10 cm into the furnace and the system was pumped down to base pressure
(∼1.5 mTorr) following which three subsequent purge cycles
using ultrahigh purity Ar at 100 sccm were performed. Afterward, Ar
flow was cut off and H2 flow was introduced at 5 sccm as
the carrier gas for the rest of the growth. Background pressure of
the system was held at 5 mTorr. Mo(CO)6 and (C2H5)2S precursors were kept in bubblers in APs
at 45 °C and at room temperature, respectively, and the flow
rates were controlled via needle valves. The growth was conducted
at 850 °C for a duration of 1 min after which the precursor gas
flow was cut off and the furnace was allowed to cool down, with only
the carrier gas flowing.
MOCVD growth system
under low-pressure conditions [
diameter of 22 mm (outer diameter = 25 mm) inside a single zone Lindberg/Blue
M furnace. The precursors used for MoS2 growth are molybdenum
hexacarbonyl, Mo(CO)6 (Sigma-Aldrich, CAS number 13939-06-05,
99.9%), and diethyl sulfide, (C2H5)2S (Sigma-Aldrich, CAS number 352-93-2, 98%). The target substrate
used in this work was 285 nm SiO2 grown on highly doped
double-side-polished p-type Si. At the start of the growth process,
the target substrate (measuring 10 cm × 1.7 cm) was placed approximately
10 cm into the furnace and the system was pumped down to base pressure
(∼1.5 mTorr) following which three subsequent purge cycles
using ultrahigh purity Ar at 100 sccm were performed. Afterward, Ar
flow was cut off and H2 flow was introduced at 5 sccm as
the carrier gas for the rest of the growth. Background pressure of
the system was held at 5 mTorr. Mo(CO)6 and (C2H5)2S precursors were kept in bubblers in APs
at 45 °C and at room temperature, respectively, and the flow
rates were controlled via needle valves. The growth was conducted
at 850 °C for a duration of 1 min after which the precursor gas
flow was cut off and the furnace was allowed to cool down, with only
the carrier gas flowing.
7
Organometallic Compounds Synthesis Protocol
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Pt(acac)2 (98%),
Ni(acac)2 (95%), Mo(CO)6 (99%), HClO4 (70 wt %), [BMIM][NTF2] (98%), and 7-methyl-1,5,7-triazabicyclo[4.4.0]dec-5-ene
([MTBD], 98%) were purchased from Sigma-Aldrich. N,N-Dimethylformamide (99.8+%) and benzoic acid (99%)
were purchased from Alfa Aesar. Lithium bis(perfluoroethylsulfonyl)imide
(99%) was purchased from IoLiTec GmbH. All chemicals were used as
received without further purification. Deionized water (<1.1 μS
cm–1) was supplied by VWR chemicals and was used
for the prepartion of all aqueous solutions.
Ni(acac)2 (95%), Mo(CO)6 (99%), HClO4 (70 wt %), [BMIM][NTF2] (98%), and 7-methyl-1,5,7-triazabicyclo[4.4.0]dec-5-ene
([MTBD], 98%) were purchased from Sigma-Aldrich. N,N-Dimethylformamide (99.8+%) and benzoic acid (99%)
were purchased from Alfa Aesar. Lithium bis(perfluoroethylsulfonyl)imide
(99%) was purchased from IoLiTec GmbH. All chemicals were used as
received without further purification. Deionized water (<1.1 μS
cm–1) was supplied by VWR chemicals and was used
for the prepartion of all aqueous solutions.
8
Synthesis of materials
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Unless otherwise specified, all syntheses and subsequent manipulations of purified materials were carried out under rigorous air- and water-free conditions, using Schlenk techniques or an Ar-atmosphere MBraun glovebox. The solvents N,N-dimethylformamide, acetonitrile, tetrahydrofuran, diethyl ether, and dichloromethane were dried using a commercial solvent purification system designed by JC Meyer Solvent Systems and were stored over 4 Å (DMF, CH3CN, THF, Et2O) or 3 Å (CH2Cl2) molecular sieves prior to use. Propylene carbonate was dried over melted sodium metal and distilled prior to use. The compound Mo(CO)6 (98%) was purchased from Sigma Aldrich and sublimed prior to use. The compounds NbCl3(DME),33 MoCl4(CH3CN)2,68 Ti(acac)3,69 (H2NMe2)2Ti2(Cl2dhbq)3, (H2NMe2)2V2(Cl2dhbq)3, and (H2NMe2)1.5Cr2(dhbq)3,25 (link) were synthesized according to previously reported procedures. All other reagents were purchased and used as received: triflic acid (99.5%, Oakwood Chemical), triflic anhydride (99.5%, Oakwood Chemical), chloranilic acid (98%, Alfa Aesar), and Cr(acac)3 (97%, Sigma Aldrich). Compositional C, H, N, and S analyses were obtained from the Microanalytical Laboratory at the University of California, Berkeley.
9
Synthesis and Characterization of Phosphino-Amine Complexes
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All experimental manipulations were performed under purified dry nitrogen using standard Schlenk and vacuum line techniques. Solvents were dried and freshly distilled under an atmosphere of nitrogen prior to use [26 ]. The chemicals Mo(CO)6, W(CO)6, Cr(CO)6, chlorodiphenylphosphine, and p-aminoacetophenone were purchased from Aldrich and used as received. N-(4-acetylphenyl)-N-(diphenylphosphino)amine ligand (1 ) was previously prepared [19 ]. Infra-red spectra were recorded with a PerkinElmer System 2000 FT-IR spectrometer between 4000 and 400 cm−1 using KBr disks. Microanalyses were performed on a Flash 2000 elemental analyzer. Infra-red spectra were recorded on a Shimadzu FTIR-8400S spectrometer between 4000-400 cm−1 using KBr disks. The NMR spectra were recorded at 25 °C on a Bruker-Avance-DRX-400 MHz NMR spectrometer operating at 400.17 (1H), 100.63 (13C), and 161.98 (31P) using tetramethylsilane for 1H and 85% H3PO4 for 31P NMR as external standards. Melting points were carried out on a Gallenkamp apparatus with open capillaries.
10
Synthesis of K8SnSb4 under Inert Conditions
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All manipulations and reactions were performed under a nitrogen atmosphere using standard Schlenk or glovebox techniques. En (Aldrich, 99%) and DMF (Aldrich, 99.8%) were freshly distilled by CaH2 prior to use, and stored in N2 prior to use. Tol (Aldrich, 99.8%) was distilled from sodium/benzophenone under nitrogen and stored under nitrogen. [2.2.2]-crypt (4,7,13,16,21,24-Hexaoxa-1,10-diazabicyclo (8.8.8) hexacosane, purchased from Sigma-Aldrich, 98%) was dried in a vacuum for one day prior to use. K8SnSb4 was prepared by heating a stoichiometric mixture of the elements (K: 625.6 mg, Sn: 237.4 mg, Sb: 974.4 mg; K: +99%, Sn: 99.999%, Sb: 99.9%, all from Strem) at a rate of 70 °C per hour to 700 °C and keeping it for 36 h in sealed niobium containers closed in evacuated quartz ampules according to the previous procedures26 (link). The K8SnSb4 solid was obtained with a high yield (~92%, 1.7 g) and stored under a dry nitrogen atmosphere in a glove box. Cr(CO)6 and Mo(CO)6 were purchased from Aldrich while Ag4Mes4 and Cu(PPh3) Cl were synthesized according to the literature with a yield of 55 and 60%, respectively58 (link),59 (link).
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