Materials 1.0 M (mol/L) LiPF6 in a 3:7 wt:wt ethylene carbonate (EC): ethyl methyl carbonate (EMC) (LP57, battery-grade, BASF), LiPF6 (>99.99%, battery-grade, Aldrich), LiBF4 (>99.99%, ultra-dry-grade, Aldrich), EC (battery-grade, BASF), EMC (battery-grade, BASF) were used as received. The electrolytes (except for LP57) were prepared by simple mixing of LiPF6 or LiBF4 and EC or EMC in an Argon-filled glove box (MBraun, < 0.5 ppm of H2O and O2). The residual water contents in the electrolytes were measured by Karl Fischer titration and were less than 20 ppm.
Lipf6
Manufactured by Merck Group
Sourced in United States, Germany
LiPF6 is a lithium-based compound used as a component in the electrolyte solution of lithium-ion batteries. It provides ionic conductivity and stability within the battery system.
Automatically generated - may contain errors
Lab products found in correlation
Li foil, by Thermo Fisher Scientific (3 mentions)
Lithium metal, by Merck Group (3 mentions)
Polyvinylidene fluoride (pvdf), by Merck Group (3 mentions)
Litfsi, by Merck Group (3 mentions)
Nh4pf6, by Strem Chemicals (2 mentions)
Polyvinylpyrrolidone, by Merck Group (2 mentions)
Chlorotrimethylsilane, by Merck Group (2 mentions)
Nonafluorobutanesulfonic acid, by Merck Group (2 mentions)
Tetrabutylammonium tba chloride, by Merck Group (2 mentions)
1 2 dichloroethane dce, by Merck Group (2 mentions)
Automatic battery cycler, by Wonatech (2 mentions)
N methyl 2 pyrrolidone nmp, by Merck Group (2 mentions)
Toluene, by Merck Group (2 mentions)
Diethyl carbonate, by Merck Group (2 mentions)
Dsc 8500, by PerkinElmer (2 mentions)
N methyl 2 pyrrolidone, by Merck Group (2 mentions)
Litfsi, by BASF (1 mentions)
Liclo4, by Merck Group (1 mentions)
Synthetic graphite, by Merck Group (1 mentions)
Stainless steel mesh, by Thermo Fisher Scientific (1 mentions)
44 protocols using lipf6
1
Preparation of Lithium-Based Electrolytes
2
Lithium-Ion Battery Evaluation Protocol
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The battery performances of all samples were evaluated using a Wonatech automatic battery cycler in a CR2016 type coin cell. The electrodes were fabricated by preparing a slurry of 80 wt% active material and 20 wt% polyvinylidene fluoride binder in N-methyl-2-pyrrolidone. The specific capacity was measured based on the mass of active material. The coin cells were assembled by employing a composite electrode with metallic lithium foil and 1M LiPF6 (Aldrich 99.99%) dissolved in a solution of ethylene carbonate/dimethyl carbonate/diethyl carbonate (1:2:1 v/v) as an electrolyte in a glove box filled with argon. The cell was galvanostatically cycled between 0.01 and 3.0 V vs. Li/Li+ at various specific currents.
3
Ionic Liquid Electrolyte with Redox-Active Additive
4
Preparation of Concentrated Electrolytes
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Three types
of salts, namely, LiPF6 (Aldrich, >99.99%), LiTFSI (BASF),
and LiFSI (Suzhou Fluolyte, >99.9%) were dissolved in a 1:1 (v/v) EC (Gotion)/DEC (Gotion) solvent mixture
to prepare electrolytes with concentrations of 1, 2, and 4 M. The
salts dried in a vacuum oven at 120 °C over 12 h for LiPF6, 120 °C over 48 h for LiTFSI, and 80 °C over 72
h for LiFSI. The electrolyte solvent was dried over molecular sieves
for at least 48 h (resulting in H2O content < 1 ppm)
and filtered through 200 nm PTFE membranes prior to mixing with the
salt. To prepare the concentrated electrolytes, the solutions were
heated to 60 °C for LiTFSI and LiFSI and to 45 °C in the
case of LiPF6. An electrolyte based on ionic liquid with
the formulation 1 M LiFSI in Pyr14FSI (Solvionic) was also
considered in this study. The H2O content in the LiFSI-
and LiTFSI-based electrolytes was determined using a 756 Karl Fischer
coulometer (Metrohm) and varied between 15 and 60 ppm depending on
the electrolyte concentration. The LiPF6 based electrolytes
and the 1 M LiFSI in Pyr14FSI showed a water content below
2 ppm. All electrolyte preparation took place in the glovebox.
of salts, namely, LiPF6 (Aldrich, >99.99%), LiTFSI (BASF),
and LiFSI (Suzhou Fluolyte, >99.9%) were dissolved in a 1:1 (v/v) EC (Gotion)/DEC (Gotion) solvent mixture
to prepare electrolytes with concentrations of 1, 2, and 4 M. The
salts dried in a vacuum oven at 120 °C over 12 h for LiPF6, 120 °C over 48 h for LiTFSI, and 80 °C over 72
h for LiFSI. The electrolyte solvent was dried over molecular sieves
for at least 48 h (resulting in H2O content < 1 ppm)
and filtered through 200 nm PTFE membranes prior to mixing with the
salt. To prepare the concentrated electrolytes, the solutions were
heated to 60 °C for LiTFSI and LiFSI and to 45 °C in the
case of LiPF6. An electrolyte based on ionic liquid with
the formulation 1 M LiFSI in Pyr14FSI (Solvionic) was also
considered in this study. The H2O content in the LiFSI-
and LiTFSI-based electrolytes was determined using a 756 Karl Fischer
coulometer (Metrohm) and varied between 15 and 60 ppm depending on
the electrolyte concentration. The LiPF6 based electrolytes
and the 1 M LiFSI in Pyr14FSI showed a water content below
2 ppm. All electrolyte preparation took place in the glovebox.
5
Dual-Salt Electrolyte Composition and Properties
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Battery-grade EC and DMC solvents were purchased from Sigma-Aldrich (purity > 99%). Lithium salt LiPF6 was purchased from Aldrich (purity ≥ 99.99% trace metals basis). Battery-grade LiTFSI (purity > 98%) and LiODFB (purity > 99%) were purchased from Adamas. All untreated chemicals were stored in a glove box filled with purified argon during the preparation of electrolytes. The dual-salt electrolyte was composed of 0.6 M LiTFSI and 0.4 M LiODFB (or LiTFSI0.6-LiODFB0.4) in EC+DMC (2:3, v/v). For comparison, the control electrolyte composed of 1 M LiPF6 in the same EC+DMC (2:3, v/v) mixture was investigated as well. The physico-chemical properties of the above electrolyte lithium salts and solvents are listed in Table 1 .
6
Electrochemical Characterization of Ionic Solutions
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Poly(vinyl
pyrrolidone) (PVP; average molecular
weight, 40 kDa), nonafluorobutanesulfonic acid, LiPF6,
tetraphenylarsonium chloride (TPhAsCl), LiClO4, tetrabutylammonium
(TBA+) chloride, 1,2-dichloroethane (DCE), and chlorotrimethylsilane
(≥99%) were purchased from Aldrich (Milwaukee, WI). The PF6 salt of (ferrocenylmethyl)trimethyl ammonium (FcTMA+) was prepared by metathesis of its iodide salt (Strem Chemicals,
Newburyport, MA) and NH4PF6 (Strem Chemicals).
The tetrakis(pentafluorophenyl)borate salt of tetradodecylammonium
was obtained by metathesis and used as organic supporting electrolytes.
Deionized water (18.2 MΩ·cm; Nanopure, Barnstead, Dubuque,
IA) was used to prepare the mock intracellular buffer solution at
pH 7.4 containing 90 mM KCl, 10 mM NaCl, 2 mM MgCl2, 1.1
mM EGTA, 0.15 mM CaCl2, and 10 mM HEPES. Furthermore, 15
or 5.5 g/L PVP was added to the buffer solution to prepare an isotonic
or a hypotonic solution, respectively.
pyrrolidone) (PVP; average molecular
weight, 40 kDa), nonafluorobutanesulfonic acid, LiPF6,
tetraphenylarsonium chloride (TPhAsCl), LiClO4, tetrabutylammonium
(TBA+) chloride, 1,2-dichloroethane (DCE), and chlorotrimethylsilane
(≥99%) were purchased from Aldrich (Milwaukee, WI). The PF6 salt of (ferrocenylmethyl)trimethyl ammonium (FcTMA+) was prepared by metathesis of its iodide salt (Strem Chemicals,
Newburyport, MA) and NH4PF6 (Strem Chemicals).
The tetrakis(pentafluorophenyl)borate salt of tetradodecylammonium
was obtained by metathesis and used as organic supporting electrolytes.
Deionized water (18.2 MΩ·cm; Nanopure, Barnstead, Dubuque,
IA) was used to prepare the mock intracellular buffer solution at
pH 7.4 containing 90 mM KCl, 10 mM NaCl, 2 mM MgCl2, 1.1
mM EGTA, 0.15 mM CaCl2, and 10 mM HEPES. Furthermore, 15
or 5.5 g/L PVP was added to the buffer solution to prepare an isotonic
or a hypotonic solution, respectively.
7
Solid Solution Electrodes for High-Voltage Li-Ion Batteries
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Solid solution electrodes of composition Li1.25Cr0.25Mn1.5O4:LiNi0.5Mn1.5O4 of 3:7 mole ratio (Li1.075Cr0.075Ni0.35Mn1.5O4) were mixed with carbon and PVDF in an NMP slurry to produce an 80:15:5 composite coating of the active: carbon black: PVDF on an Al foil current collector. The active loading was ~6 mg/cm3. The C rate was based on a capacity of 147 mAh g−1 for LiNi0.5Mn1.5O4. Coin cells (Hohsen, Al clad, Pred Materials, New York, NY, USA) were fabricated using an electrolyte 1 M LiPF6 dissolved in EC:EMC 1:1 (weight ratio, Sigma-Aldrich, Saint Louis, MO, USA) and 2% tris (trimethylsilyl) phosphate (TCI Americas, Portland, OR, USA) an electrolyte stabilizing additive for use at high voltage [61 (link)] and Li foil (Johnson Matthey, Alpharetta, GA, USA) as anode. The electrochemical data was collected on a Maccor 4000 Battery cycler (Maccor Inc., Tulsa, OK, USA) The charge and discharge rates were equal for each charge/discharge cycle and charge and discharge rates were varied each five cycles (cycles 1–30) in order from 0.2C, 0.33C, 1C, 2C, 5C to 10C and then fixed at 1C for cycles 31–60.
8
Synthesis of Electrode Materials for Li-ion Batteries
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Synthetic graphite (<45 µm, 99.99%), LiPF6 (battery grade, ≥99.99%), DMC (anhydrous, ≥99%), and alginic acid sodium salt (Alg, medium viscosity) were purchased from Sigma Aldrich. Super P, Li foil (~250 μm in thickness), and stainless steel mesh were bought from Alfa Aesar. Li(CF3SO2NSO2CF3)2 (LiTFSI, 99.5%) and Li(FSO2NSO2F)2 (LiFSI, 99.5%) were purchased from Solvionic. 5,10,15,20-(tetra-4-aminophenyl) porphyrin, 1,4-phenylene-4,4’-bis (2,6-diphenyl-4-pyrylium tetrafluoroborate), sodium oleyl sulfate (SOS) and solvents (e.g., chloroform) were purchased from PorphyChem and Sigma-Aldrich, and used directly without further purification. Water was purified using a Milli-Q purification system (Merck KGaA). All the reactions were carried out under an ambient atmosphere. Substrates (e.g., 300 nm SiO2/Si wafer, quartz glass and copper grids) were obtained from Microchemicals and Plano GmbH.
9
Coin Cell Fabrication and Electrochemical Characterization
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The anodes were assembled into CR2016-type coin cells with Celgard 2400 as the separator, LiPF6 in ethylene carbonate/dimethyl carbonate (v/v = 1 : 1, from Sigma-Aldrich) as the electrolyte and Li foil as the counter electrode. The electrochemical impedance spectrum (EIS) was measured over the frequency range from 105 Hz to 10−2 Hz by applying an ac voltage with 5 mV amplitude (CHI 660E). Galvanostatic cycling was carried out between 0.01 V and 3 V versus Li/Li+ (Land CT2001A). After electrochemical cycling, the anodes were took out from the cells and washed in acetonitrile to remove residual electrolyte and then dried in an Ar-filled glove box for 12 hours for physical characterization.
10
Comprehensive Electrochemical Characterization
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Spherical CNs including EC300J
(Lion, Japan), Super P (Timcal), Denka (Japan), and ENSACO (Timcal),
lithium manganese oxide, lithium cobalt oxide, lithium nickel manganese
cobalt oxide, lithium iron phosphate (Gelon, Hong Kong), sulfuric
acid (H2SO4, 98%, QRec), nitric acid (HNO3, 65%, QRec), PVDF (Sigma-Aldrich), ferrocenemethanol (97%,
Sigma-Aldrich), hydrazine hydrate (99%, Loba Chemie), N-methylpyrrolidone (NMP, 99.5%, QRec), and 1 M lithium hexafluorophosphate
(LiPF6, Sigma-Aldrich) in the mixture of ethylene carbonate
(EC), ethyl methyl carbonate (EMC, Sigma-Aldrich), and dimethyl carbonate
(DMC, Sigma-Aldrich) (1:1:1 v/v/v) (Gelon) were of analytical grade
and used without further purification. Carbon fiber paper (CFP) (SGL
Carbon SE, Germany) was used as a current collector. Deionized water
was purified by using the Milli-Q system (>18 MΩ·cm,
Millipore).
Teflon-mounted GC electrode with 3.0 mm in diameter was from Metrohm
Siam Co., Ltd.
(Lion, Japan), Super P (Timcal), Denka (Japan), and ENSACO (Timcal),
lithium manganese oxide, lithium cobalt oxide, lithium nickel manganese
cobalt oxide, lithium iron phosphate (Gelon, Hong Kong), sulfuric
acid (H2SO4, 98%, QRec), nitric acid (HNO3, 65%, QRec), PVDF (Sigma-Aldrich), ferrocenemethanol (97%,
Sigma-Aldrich), hydrazine hydrate (99%, Loba Chemie), N-methylpyrrolidone (NMP, 99.5%, QRec), and 1 M lithium hexafluorophosphate
(LiPF6, Sigma-Aldrich) in the mixture of ethylene carbonate
(EC), ethyl methyl carbonate (EMC, Sigma-Aldrich), and dimethyl carbonate
(DMC, Sigma-Aldrich) (1:1:1 v/v/v) (Gelon) were of analytical grade
and used without further purification. Carbon fiber paper (CFP) (SGL
Carbon SE, Germany) was used as a current collector. Deionized water
was purified by using the Milli-Q system (>18 MΩ·cm,
Millipore).
Teflon-mounted GC electrode with 3.0 mm in diameter was from Metrohm
Siam Co., Ltd.
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