Nanostructured La Ba F was mechanosynthesized with the help of a high-energy planetary mill (Fritsch Pulverisette 7 Premium line, Fritsch GmbH, Idar-Oberstein, DE). For this purpose, stoichiometric amounts of the educts viz. LaF (99.99%, Alfa Aesar, Kandel, DE) and BaF (99.99%, Sigma Aldrich, Darmstadt, DE) were loaded into a ZrO milling beaker with a volume of 45 mL. We added 180 balls made of the same material; the diameter of each milling ball was 5 mm. The milling procedure was carried out at a rotation speed of 600 rpm; the mixture was milled for 10 h whereby 15 min milling was followed by a break of 15 min to allow cooling of the mixture and the beaker. Loading as well as unloading of the beakers was strictly carried out under inert atmosphere; we used an Ar-filled glovebox (O , H O < 0.5 ppm) to avoid any contamination by water vapor or moisture.
Pulverisette 7 premium line
Manufactured by Fritsch
Sourced in Germany
The Pulverisette 7 premium line is a high-performance planetary ball mill designed for the fine grinding and homogenization of solid samples. It features a compact, robust design and can accommodate up to four grinding bowls simultaneously.
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Lab products found in correlation
Baf 2, by Merck Group (1 mentions)
Hsqcedetgpsisp2, by Bruker (1 mentions)
Avance 3 hd 600 mhz, by Bruker (1 mentions)
Fe no3 3 9h2o, by Merck Group (1 mentions)
Ethylene glycol, by Merck Group (1 mentions)
Pulverisette 6 classic line, by Fritsch (1 mentions)
Dimethyl sulfoxide (dmso), by Thermo Fisher Scientific (1 mentions)
Sonoplus hd 2200, by Bandelin (1 mentions)
Lithium chloride (licl), by Merck Group (1 mentions)
Dv 3 ultra, by Ametek (1 mentions)
Nova nanosem 230, by Thermo Fisher Scientific (1 mentions)
Zetasizer nano, by Malvern Panalytical (1 mentions)
Sdt 650, by TA Instruments (1 mentions)
Smartlab se, by Rigaku (1 mentions)
28 protocols using pulverisette 7 premium line
1
Mechanosynthesis of Nanostructured Lanthanide Fluoride
2
Waelz Slag Magnetic Separation Protocol
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The Waelz slag samples were ground using the micromill Fritsch Pulverisette 7 premium line (Fritsch, Germany) or an agate mortar with a pestle, depending on the required fineness degree. Wet magnetic separation was realized by the XCGS-50 (Shaoxing Weibang Mining Machinery Manufacturing Co., Ltd., Shaoxing, China) device (Davis tube) with a magnetic field strength in the range of 0.5–4.5 kOe. The device consists of a glass tube with a diameter of 50 mm and a length of 770 mm, which is placed between the poles of the electromagnetic system. The Waelz slag sample of 10 g in weight of a required grinding fineness was placed into the device, which was filled with tap water with preset required magnetic field strength. The translational and rotational motion of the tube with a tap water flow led to the separation of the magnetic fraction, whereas the non-magnetic particles were poured out through a hose at the end of the tube into a container. After the tap water flow became clear, the electromagnetic system was turned off, and the magnetic fraction was poured out through the hose in another container. The obtained products were filtered using a suction flask and a porous porcelain filter, dried at 105 °C for 120 min and then weighted.
3
Synthesis of Porous Silicon Nanoparticles
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Porous silicon (pSi) layers were prepared by anodizing p-type heavily boron-doped (100)-oriented silicon (SiMat, Germany) wafers with resistivity of 0.001–0.002 Ω cm in a hydrogen fluoride (HF, CAS 7664-39-3, 48%, Merck)/ethanol (CAS 64-17-5, ≥99.8%, VWR Chemicals) mixture 1:1 v/v and current density of 50 mA/cm2 for 1 h. The obtained porous layers were separated from the wafer by applying 3 pulses of current density of 600 mA/cm2 for 3 s. After drying at room temperature (RT) overnight, the layers were ground in agar mortar into millimeter-sized particles. The obtained particles were then ball milled in deionized water in the planetary mill (Fritsch Pulverisette 7 premium line, FRITSCH GmbH) for 30 min with zirconium oxide balls of diameter 2.5 μm and then for 30 min with balls of diameter 0.1 μm. Nanoparticles (NPs) were collected from the sample by centrifugation at 12,500 rpm for 20 min, leaving the supernatant for further work. The obtained pSiNPs were stored in deionized water.
4
Biochar Synthesis from Wood Apple Shell
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A total of 10 g of weighed, chopped wood apple shell in a ceramic crucible boat was inserted into a horizontal tube furnace of stainless steel having length of 720 mm, 50 mm diameter (Carbolite, UK,) at 700 °C for 4 h, and argon gas was flowed at 80 mL/min. The furnace temperature was gradually increased for 70 min at the rate of 10 °C/min; then, the sample was allowed to cool under argon atmosphere. The collected biochar was ground in a ball milling apparatus (Fritsch, Pulverisette 7 Premium line, Germany) with zirconia ceramic and steel balls at 400 rpm for 8 h. The final ball milling biochar product was named WAS-BC (wood apple fruit shell biochar). WAS-BC was stored in an airtight desiccator and used without any further treatment for the removal of phenolic contaminants.
5
Isolation and Purification of Milled Wood Lignin from Eucalyptus
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MWL was isolated from eucalyptus according to a previously reported method16 (link) (Extended Data Fig. 4 ). Specifically, 5 g of air-dried eucalyptus wood particles (>20 mesh) was first extracted with 150 ml of benzene–ethanol (2:1, v/v) for 24 h in a Soxhlet extractor to remove extractives. The extractive-free eucalyptus wood particles were subjected to milling with ZrO2 balls at 600 r.p.m. for 10 h in a planetary ball mill (Pulverisette 7 Premium Line, Fritsch). A 20 g quantity of the ball-milled wood was extracted three times with 200 ml 96% dioxane–water (96:4, v/v) at 50 °C and 150 r.p.m. for 24 h. All extracts were combined and concentrated at 50 °C with a vacuum evaporator. The concentrated lignin solution (around 20 ml) was dried by freeze-drying to obtain crude MWL, which was further purified by dissolution in 20 ml 90% acetic acid/water (v/v) followed by precipitation in 200 ml deionized water. The purified MWL was collected by centrifugation, followed by washing with water until the pH of the filtrate reached neutral and freeze-drying under vacuum. The obtained dry MWL was directly used for preparing lignin adhesives by simply mixing it with deionized water at room temperature.
6
Lignin Characterization by NMR Spectroscopy
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NMR spectra were recorded on a Bruker AVANCE III HD 600 MHz spectrometer24 (link). Lignin samples (80 mg) were dissolved in 0.5 ml dimethylsulfoxide (DMSO)-d6 in an NMR tube. Owing to poor solubility in DMSO-d6, all hot-pressed lignins were ball milled in advance at 500 r.p.m. for 1 h in a planetary ball mill (Pulverisette 7 Premium Line, Fritsch) to facilitate dissolution. The Bruker program hsqcedetgpsisp 2.3 was selected for heteronuclear single quantum coherence characterization. Heteronuclear single quantum coherence characterization of the lignin samples was carried out with the following parameters: acquired from 10 to 0 ppm in F2 (1H) with 2,048 data points and a 1-s recycle delay, 160 to 0 ppm in F1 (13C) with 256 increments of 64 scans. The total acquisition time for a sample was 5 h. The central DMSO solvent peak δ ppm (39.5, 2.49) was used for calibration of correlation peaks. The heteronuclear single quantum coherence spectra were analysed with MestReNova 6.1.0.
7
Glimepiride Nanocrystal Suspensions Preparation
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Glimepiride nanocrystal suspensions were prepared employing the wet media milling technique on a planetary ball mill (Pulverisette 7 Premium line, Fritsch GmbH, Idar-Oberstein, Germany). Glimepiride (0.5 g) and one of the tested stabilizers (25% w/w relative to glimepiride amount) were placed in 45 mL milling bowl loaded with 70 g of zirconium oxide milling beads (0.1 mm diameter). After addition 6 mL of water, milling was performed at 450 rpm mill rotation speed in 20 cycles of 3 min with 5 min breaks after each milling cycle to prevent instrumentation and sample overheating.
8
Synthesis of BiFeO3 Nanoparticles
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BiFeO3 was synthesized by a sol–gel
method based on the study of Ma et al.,32 (link) where 1.2 × 10–2 mol (5.822 g) Bi(NO3) ×5H2O (98%, Sigma-Aldrich) and 1.0 ×
10–2 mol (4.040 g) Fe(NO3)3 × 9H2O (≥98%, Sigma-Aldrich) were mixed with
8–10 mL of ethylene glycol (99.8%, Sigma-Aldrich) under magnetic
stirring at 100 rpm and 60 °C for 1 h. Subsequently, the temperature
was increased to 100 °C to allow for a slow evaporation of the
solvent via autocombustion. The resulting dry gel was then transferred
to an Al2O3 crucible and calcined in air at
350 °C for 3 h in a muffle oven (Carbolite Furnaces CWF 1200)
and cooled to room temperature. The product was then crushed to powder
in an agate mortar, pressed to a pellet, and treated at 650 °C
for 8 h. To decrease the particle size, 2 g of the obtained product
was ball-milled with 85 g of 3 mm stainless steel balls in a Pulverisette
7 Premium Line (Fritsch) for 20 min at 250 rpm in an argon atmosphere.
method based on the study of Ma et al.,32 (link) where 1.2 × 10–2 mol (5.822 g) Bi(NO3) ×5H2O (98%, Sigma-Aldrich) and 1.0 ×
10–2 mol (4.040 g) Fe(NO3)3 × 9H2O (≥98%, Sigma-Aldrich) were mixed with
8–10 mL of ethylene glycol (99.8%, Sigma-Aldrich) under magnetic
stirring at 100 rpm and 60 °C for 1 h. Subsequently, the temperature
was increased to 100 °C to allow for a slow evaporation of the
solvent via autocombustion. The resulting dry gel was then transferred
to an Al2O3 crucible and calcined in air at
350 °C for 3 h in a muffle oven (Carbolite Furnaces CWF 1200)
and cooled to room temperature. The product was then crushed to powder
in an agate mortar, pressed to a pellet, and treated at 650 °C
for 8 h. To decrease the particle size, 2 g of the obtained product
was ball-milled with 85 g of 3 mm stainless steel balls in a Pulverisette
7 Premium Line (Fritsch) for 20 min at 250 rpm in an argon atmosphere.
9
Synthesis of Carbonaceous Materials from CaC2 and C3Cl3N3
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Granular calcium carbide (CaC 2 ≤ 75%) was purchased from Sigma Aldrich and ground for 2 h at 500 rpm in a planetary mono mill Pulverisette 6 classic line from Fritsch GmbH. The main impurities of CaC 2 are CaO and Ca(OH) 2 , although traces of S can also be detected (ESI Fig. 1 and2 †). 99% pure cyanuric chloride (C 3 Cl 3 N 3 ) was purchased from Sigma Aldrich. The synthesis of the carbonaceous materials was performed by mixing both reactants in a 45 mL zirconium oxide grinding bowl with 22 zirconium oxide balls (d = 10 mm, ∼75.7 g) using a planetary micro mill Pulverisette 7 premium line from Fritsch GmbH at the rotational speed of 500 rpm. The system was prepared under argon atmosphere inside a glove box. We tested four different CaC 2 /C 3 Cl 3 N 3 mass ratios, namely 0.5, 0.7, 2.3, 4.6. The evolution of pressure and temperature inside the grinding bowl for all samples was monitored by gas pressure and temperature measurement (GTM) automatic system (45 mL zirconium oxide bowl and 22 zirconium oxide balls), see ESI Fig. 3. † After the ignition was detected with the GTM system, the product was milled for 5 min or 120 min, giving 8 samples in total (see ESI Table 1
10
Ball Milling of Amino Acid Mixtures
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For the reactions containing mixtures of amino acids, equimolar amounts of amino acids were homogenized by ball milling in a 20 mL stainless steel jar equipped with ten stainless steel balls (diameter = 10 mm) at 400 rpm for 10 min in the planetary ball mill Pulverisette 7 premium line (Fritsch GmbH, Idar-Oberstein, Germany). The detailed list of sample weights can be found in the Supplementary Information.
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