Glass microfiber (Grade GF/D, Whatman) was used as the separator between the electrodes. The assembled cells were then inserted into a laminated aluminum film pouch (from inside to out: polypropylene/aluminum foil/polyamide). Each separator was soaked with approximately 0.9 mL of microemulsion. The pouch was then sealed under vacuum. Supercapacitor cell assembly was performed on a lab bench under ambient conditions.
Glass microfiber
Manufactured by Cytiva
Glass microfiber is a type of filtration media used in laboratory applications. It is composed of fine glass fibers that are woven or bonded together to form a porous matrix. The primary function of glass microfiber is to act as a high-efficiency filter, capturing small particulates and contaminants from liquids or gases passing through it.
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9 protocols using glass microfiber
1
Supercapacitor Cell Assembly Protocol
2
Electrochemical Characterization of NMNO_B
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Electrochemical tests were carried out by using a BioLogic VSP-300
potentiostat/galvanostat. Hohsen CR2032 coin cells were assembled
by testing the active material formulation as the working electrode,
metallic Na as the counter electrode, glass microfiber (Whatman) as
the separator and 1 M NaClO4 in propylene carbonate (PC)
with 2% fluoroethylene carbonate (FEC) as the electrolyte. Measurements
were carried out testing the half-cells with a gravimetric current
of 10 mA g–1 in the potential interval 2.0–4.3
V vs Na+/Na.
Water content in the electrolyte before
and after contact with NMNO_B has been measured through Karl Fischer
titration. Specifically, an electrode (area = 2 cm2) has
been soaked in 100 μL of the electrolyte for 24 h. The solution
was then taken and titrated using a Metrohm 899 Coulometer, and the
obtained value was compared with that measured in the pristine electrolyte.
potentiostat/galvanostat. Hohsen CR2032 coin cells were assembled
by testing the active material formulation as the working electrode,
metallic Na as the counter electrode, glass microfiber (Whatman) as
the separator and 1 M NaClO4 in propylene carbonate (PC)
with 2% fluoroethylene carbonate (FEC) as the electrolyte. Measurements
were carried out testing the half-cells with a gravimetric current
of 10 mA g–1 in the potential interval 2.0–4.3
V vs Na+/Na.
Water content in the electrolyte before
and after contact with NMNO_B has been measured through Karl Fischer
titration. Specifically, an electrode (area = 2 cm2) has
been soaked in 100 μL of the electrolyte for 24 h. The solution
was then taken and titrated using a Metrohm 899 Coulometer, and the
obtained value was compared with that measured in the pristine electrolyte.
3
Fabrication and Evaluation of KVPF-Al Electrode
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The KVPF-Al electrode was fabricated by mixing KVPO4F powder, conductive carbon (CNT, provided by XFnano), and PVDF (provided by Energy Chemical) in a weight ratio of 70:20:10 using NMP (provided by Energy Chemical) as the solvent. The resulting slurry was pasted on aluminum foil and vacuum dried overnight at 120 °C. The KVPF-film with mass loadings of 2 mg cm–2 was used as a cathode directly, without any conductive agent, binder, or current collector. CNT-K was high-temperature mixing of CNF with metallic K that can form prepotassiated carbon. In the CR2032-type coin cell, half-cells containing potassium metal foil as counter and reference electrodes and glass microfiber (Whatman) as the separator were assembled for electrochemical measurements. The electrolyte solution was 0.8 M KPF6 in a mixture of ethylene carbonate (EC) and diethylene carbonate (DEC) by a 1:1 volume ratio with 1.5 wt% tris(trimethylsilyl)phosphine (TMSP, provided by Adamas-beta). The cathode properties were galvanostatically charged–discharged between 2.0 and 5.0 V vs. K/K+ at various current densities on an automatic battery testing system (Neware CT-4008T). Based on the theoretical capacity of KVPO4F (131 mAh g–1), 131 mA g–1 is equivalent to 1 C in this work. CV and in situ EIS measurements were carried out on a Solartron 1470E (Solartron Public Co., Ltd.) multichannel electrochemical workstation.
4
Operando Synchrotron-Based XRD for Li-Air Batteries
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A LAB cell was specially designed for operando synchrotron-based XRD measurements. The cell was assembled in an Ar-filled glove box by sandwiching an as-prepared cathode (diameter: 16 mm), porous separator (glass microfiber, thickness: 0.26 mm, Whatman) and Li foil. The window of the LAB cell was Al-coated Kapton. The details and schematic drawing of the Li–air battery cell assembly is described in Section 1 of the ESI.† The area where electrochemical reaction proceeds was 1 cm2. The electrolyte was 1 M LiCF3SO3/tetraethylene glycol dimethyl ether (TEGDME).
5
Asymmetric Supercapacitor using BiPO4 and ZIF-8
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To obtain the working electrodes the electroactive materials (BiPO4, ZIF-8, and BiPO4@ZIF-8): 85 wt %, acetylene black:
10 wt % and PDVF: 5 wt % were intermingled with the inclusion of a
few drops of the NMP solvent. The chosen current collector was a nickel
foam in the dimensions of 1 cm × 1 cm. The oxide layer on the
nickel foam was removed by cleaning 1 M HCl. The electrode was obtained
by dropping the slurry on the nickel foam and drying at 85 °C
for 12 h under vacuum. Roughly 1.1 mg mass of the active material
was acquired.
A Gamry Reference 3000 electrochemical workstation
was used to test the electrochemical measurements of the patterns
in a typical three-electrode configuration by cyclic voltammetry (CV),
galvanostatic charge–discharge (GCD), and electrochemical impedance
spectroscopy (EIS). The electroactive materials were operated as working
electrodes, Pt foil (1 × 1 cm2) as the counter electrode
in which the reference electrode was silver/silver chloride (Ag/AgCl).
All electrochemical analysis and measurements were conducted in 2
M KOH aqueous electrolyte.
The ASC device was formed by using
BiPO4 as the anode
and ZIF-8@BiPO4 as the cathode with a glass microfiber
(Whatman) fiber as a separator. The CV, GCD, EIS, and the long-term
test measurements of the asymmetric device were performed in the voltage
range of 0–1.4 V.
10 wt % and PDVF: 5 wt % were intermingled with the inclusion of a
few drops of the NMP solvent. The chosen current collector was a nickel
foam in the dimensions of 1 cm × 1 cm. The oxide layer on the
nickel foam was removed by cleaning 1 M HCl. The electrode was obtained
by dropping the slurry on the nickel foam and drying at 85 °C
for 12 h under vacuum. Roughly 1.1 mg mass of the active material
was acquired.
A Gamry Reference 3000 electrochemical workstation
was used to test the electrochemical measurements of the patterns
in a typical three-electrode configuration by cyclic voltammetry (CV),
galvanostatic charge–discharge (GCD), and electrochemical impedance
spectroscopy (EIS). The electroactive materials were operated as working
electrodes, Pt foil (1 × 1 cm2) as the counter electrode
in which the reference electrode was silver/silver chloride (Ag/AgCl).
All electrochemical analysis and measurements were conducted in 2
M KOH aqueous electrolyte.
The ASC device was formed by using
BiPO4 as the anode
and ZIF-8@BiPO4 as the cathode with a glass microfiber
(Whatman) fiber as a separator. The CV, GCD, EIS, and the long-term
test measurements of the asymmetric device were performed in the voltage
range of 0–1.4 V.
6
Sodium-ion Battery Electrochemical Characterization
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The weight ratio of active materials in the positive and negative electrodes was adjusted to 3.0 : 1.0, which corresponds to the capacity ratio of 1.2 : 1.0 = QPositive electrode: QNegative electrode (Q denotes practical capacity) considering the practical capacities of NaCrO2 (100 mAh g -1 ) and HC (250 mAh g -1 ). The loading masses of the positive and negative electrodes were 4.5-5 and 1.3-1.5 mg cm -2 , respectively. Galvanostatic charge-discharge tests were conducted using a three-electrode cell configuration (EC Frontier co., LTD) by separately monitoring the positive and negative electrode potentials. Sodium metal (Sigma-Aldrich Chemistry, 99.95% purity) was cut into a disk (13 mm diameter) and fixed on an Al plate current collector as the negative electrode for half-cell measurement. Glass microfiber (Whatman GF/D) was used as a separator, and Na metal ring was used for a reference electrode. Cyclic voltammetry (CV) was carried out using a coin-cell configuration with an Al working electrode (10 mm diameter) and a Na metal counter electrode. Linear sweep voltammetry (LSV) was performed to 5.5 V with a Pt working electrode (10 mm diameter) and a Na metal counter electrode. Chargedischarge and CV tests were controlled by a VSP potentiostat (Bio-Logic) at 298 K.
7
Spectrophotometric Determination of Algal Biomass
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The biomass parameter of the isolates was determined spectrophotometrically [28 ]. The 50 ml volume of the culture suspension was filtered through 1.2 μm filter (glass microfiber, Whatman, 1822-047) and incubated at 105 °C for 24 h. The biomass dry weight (DW) was recorded and an equation (Eq.1) was developed based on its relationship with OD730 to express the biochemical composition of the isolates as portion of DW.
The dry biomass was further ashed in a furnace at 550 °C for 30 min. The relationship between OD730 and ash-free dry weight (AFDW) of algal biomass (mg L−1) was established. The obtained regression equation (Eq.2) was used to calculate biomass concentration:
The specific growth rate of the isolates was also calculated using Eq.3 :
Where μ (day−1) is the specific growth rate, and X1 and X2 are the biomass concentrations at respectively 1st (t1) and 21st (t2) day of cultivation, during the exponential growth phase.
The dry biomass was further ashed in a furnace at 550 °C for 30 min. The relationship between OD730 and ash-free dry weight (AFDW) of algal biomass (mg L−1) was established. The obtained regression equation (Eq.2) was used to calculate biomass concentration:
The specific growth rate of the isolates was also calculated using Eq.
Where μ (day−1) is the specific growth rate, and X1 and X2 are the biomass concentrations at respectively 1st (t1) and 21st (t2) day of cultivation, during the exponential growth phase.
8
Sodium-ion Battery Protocol Development
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The electrodes were prepared by dispersing the as-prepared material (80 wt%) and poly (Vinylidene fluoride) binder (PVDF, 20 wt%) in N-methyl-2-pyrrolidone (NMP) to form a slurry. The resultant slurry was pasted onto copper foil using a doctor blade and dried in a vacuum oven for 12 h, followed by pressing at 200 kg cm -2 . The loading weight of the electro-active material is around 1.1 mg cm -2 . Electrochemical measurements were carried out using two electrode coin cells with Na metal as counter and reference electrodes and the glass micro-fiber (Whatman) as the separator. The CR2032-type coin cells were assembled in an argon-filled glove box (UniLab, Mbraun, Germany). The electrolyte solution was 1 M NaClO 4 dissolved in a mixture of ethylene carbonate (EC) and propylene carbonate (PC) with a volume ratio of 1 : 1 with a 5 vol% addition of fluoroethylene carbonate (FEC). All the capacities were calculated based on the mass of the composites. Cyclic voltammetry (CV) was conducted on a CHI 660C instrument between 0.01 and 3 V vs. Na/Na + at room temperature. For the electrochemical impedance spectroscopy (EIS) measurement, the excitation amplitude applied to the cells was 5 mV. The charge-discharge measurements were performed at ambient temperature at different current densities in the voltage range from 0.01 and 3 V vs. Na/Na + .
9
Electrochemical Characterization of Lithium-Ion Batteries
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The electrochemical characteristics were measured in vacuum-sealed cells ("pouch cells"). Two electrode cells were assembled: the tested working electrode (WE) and a metallic Li counter electrode (CE) (∼3 cm 2 ) were placed oppositely over a separator ("Whatman" glass microfiber). The electrolyte used was 1 M LiPF 6 in EC:DEC (1:1 by volume), all received from Aldrich. The galvanostatic measurements were performed using a "VMP3" (Bio-Logic) potentiostat/galvanostat running with EC-Lab ® software. All the comparative measurements of LiCoO 2 , LiFePO 4 -C, LiMnPO 4 -C materials were conducted at 25 °C.
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