Effect of Grinding and the Mill Type on Magnetic Properties of Carboxylated Multiwall Carbon Nanotubes
Abstract
:1. Introduction
2. Materials and Methods
2.1. Sample Preparation
2.2. Methods
- (i)
- Mössbauer spectroscopy (spectra were recorded at a home-made cryostat (Kraków, Poland) at 85 K, 220 K and 295 K; ΔT = 0.1 K; a source of γ—radiation with an energy of 14.4 keV: 57Co(Rh); an absorption spectrum of α-Fe at room temperature was used for the calibration).
- (ii)
- the Vibrating Sample Magnetometer (VSM) option of a 9 T Quantum Design Physical Property Measurement System (PPMS), (Quantum Design North America, San Diego, California); (temperature measurements within a wide range from 3 K to 350 K; the external field (μ0H) used: up to ± 8 T).
- (iii)
- a high-resolution transmission electron microscope (TEM), G2 F20X-Twin 200 kV, (FEI, Brno, Czech Republic) equipped with a Si(Li) detector SUTW, 136 eV (EDAX, Mahwah, USA) for recording of energy dispersive X-ray spectra (EDX).
- (iv)
- Inductively Coupled Plasma—Optical Emission Spectrometer (ICP-OES), Optima 7000 DV ICP-EOS (PerkinElmer, Waltham, MA, USA).
3. Results
3.1. Mössbauer Experiments
3.1.1. The Control Group of MWCNTs
3.1.2. MWCNTs Ground in the Agate Mill
3.1.3. MWCNTs Ground in the Steel Mill
3.2. VSM Experiments
3.3. TEM Images
4. Discussion
4.1. Characterization of Magnetic Properties of Fe-NPs Embedded Inside the Carbon Matrix of MWCNTs
4.2. Unique Effects of Milling on the Magnetic Properties of MWCNTs-COOH
5. Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
Nomenclature
CNTs | carbon nanotubes |
MWCNTs | multiwall carbon nanotubes |
SWCNTs | singlewall carbon nanotubes |
Fe-NPs | iron nanoparticles |
MAMs | microwave absorption materials |
VSM | vibrating sample magnetometer |
VSM | vibrating sample magnetometer |
PPMS | physical property measurement system |
TEM | transmission electron microscope |
EDX | energy dispersive X-ray spectroscopy |
ICP-OES | inductively coupled plasma—optical emission spectrometer |
MD method | microwave digestion method |
LAS | law of approach to saturation |
EMI | electromagnetic interface |
IS | isomer shift related to the metallic Fe [mm/s] |
QS | quadrupole splitting [mm/s] |
Hhf | hyperfine magnetic field [T] |
∆Q | quadrupole splitting distribution [mm/s] |
∆H | magnetic field distribution [T] |
C | relative contribution [%] |
Γ | line width [mm/s] |
Γ | line width [mm/s] |
IS | isomer shift related to the metallic Fe [mm/s] |
dSM | diameter of NPs estimated from Mössbauer data |
VkB | volume of a particle [m3]Boltzmann constant, 1.380649x10-23 J/K |
M | mass magnetization [Am2/kg] |
MS | saturation magnetization [Am2/kg] |
Mr | remanence, remanent field [Am2/kg] |
μ0Hc | coercivity, coercive field [T] |
ΔHc | differences between the coercive fields [T] |
μ0H | external field [T] |
μ0 | vacuum magnetic permeability, 4π × 10−7 H/m |
μ | magnetic moment [Am2] |
(BH)max | maximum energy product [J/m3] |
K | magnetocrystalline anisotropy energy [J/m3] |
Keff | effective magnetic anisotropy constant [J/m3] |
χp | paramagnetic susceptibility [m3/kg] |
Kd | shape anisotropy constant [J/m3] |
Nc, Na | demagnetization factors |
dc | critical diameter [m] |
dt | threshold diameter [m] |
lK | crystalline anisotropy length [m] |
lex | magnetostatic exchange length [m] |
lKeff | effective anisotropy length [m] |
A | exchange-stiffness constant [J/m] |
T | temperature [K] |
TB | blocking temperature [K] |
TC | Curie temperature [K] |
TC | Curie temperature [K] |
T0s, T0r | characteristic temperatures above which magnetic ordering disappears [K] |
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Grinding Jar Material | Agate | Stainless Steel |
---|---|---|
Volume | 250 mL | 500 mL |
Inner diameter | 76 mm | 100 mm |
Designation | SiO2 | X90CrMoV18 |
Hardness | 6.5–7.0 Mohs | 265 HB |
Tensile strength | − | ≤925 N/mm2 |
Density | 2.65 g/mL | 7.7 g/mL |
Grinding Ball material | Agate | Stainless Steel |
Grinding Ball diameter | 10 mm | 10 mm |
MWCNTs | Hc [T] | Mr [Am2/kg Fe] | Ms1 [Am2/kg Fe] | Mr/Ms | Keff1 [kJ/m3] | Kd2 [kJ/m3] | |
---|---|---|---|---|---|---|---|
control | 3 K | ||||||
as prepared | 0.282 | 19.6 | 55 | 0.359 | 192 | 54 ÷ 108 | |
-COOH | 0.176 | 6.0 | 89 | 0.067 | 538 | 145 ÷ 290 | |
-COONH4 | 0.124 | 4.6 | 114 | 0.040 | 682 | 235 ÷ 471 (172 ÷ 344) | |
295 K | |||||||
as prepared | 0.032 | 9.1 | 39 | 0.233 | 114 | 27 ÷ 55 | |
-COOH | 0.029 | 3.1 | 42 | 0.074 | 290 | 32 ÷ 63 | |
-COONH4 | 0.027 | 2.3 | 51 | 0.044 | 380 | 48 ÷ 96 (35 ÷ 70) | |
agate mill | 3 K | ||||||
as prepared | 0.276 | 18.1 | 51 | 0.358 | 159 | 46 ÷ 93 | |
-COOH | 0.180 | 3.4 | 75 | 0.045 | 450 | 102 ÷ 203 | |
-COONH4 | 0.140 | 5.3 | 124 | 0.043 | 701 | 280 ÷ 560 (205 ÷ 410) | |
295 K | |||||||
as prepared | 0.034 | 8.5 | 36 | 0.236 | 104 | 24 ÷ 48 | |
-COOH | 0.027 | 1.7 | 41 | 0.041 | 289 | 30 ÷ 60 | |
-COONH4 | 0.028 | 2.6 | 55 | 0.048 | 277 | 55 ÷ 111 (40 ÷ 81) | |
steel mill | 3 K | ||||||
as prepared | 0.268 | 17.4 | 51 | 0.343 | 162 | 47 ÷ 94 | |
-COOH | 0.045 | 5.9 | 159 | 0.037 | 686 | 460 ÷ 920 (336 ÷ 673) | |
-COONH4 | 0.127 | 6.0 | 114 | 0.053 | 616 | 234 ÷ 468 (171 ÷ 342) | |
295 K | |||||||
as prepared | 0.032 | 9.0 | 36 | 0.249 | 98 | 24 ÷ 48 | |
-COOH | 0.019 | 3.1 | 53 | 0.059 | 313 | 51 ÷ 101 (37 ÷ 74) | |
-COONH4 | 0.026 | 2.8 | 51 | 0.056 | 317 | 47 ÷ 93 (34 ÷ 68) |
MWCNTs | dSM [nm] | lKeff [nm] | lex [nm] | lKeff [nm] | lex [nm] | |
---|---|---|---|---|---|---|
control | 3 K | 295 K | ||||
as prepared | 11.3 | 13.0 | 17.3 ÷ 24.4 | 9.6 12.0 * | 17.9 ÷ 25.3 22.5 ÷ 31.8 * | |
-COOH | 9.3 | 9.9 | 13.5 ÷ 19.1 | 5.0 7.4 * | 14.6 ÷ 20.6 21.7 ÷ 30.7 * | |
-COONH4 | 9.2 | 9.9 | 12.0 ÷ 16.9 | 4.9 7.3 * | 13.0 ÷ 18.3 19.6 ÷ 27.6 * | |
agate mill | 3 K | 295 K | ||||
as prepared | 9.1 | 13.7 | 18.0 ÷ 25.4 | 12.5 15.7 * | 18.6 ÷ 26.3 23.3 ÷ 33.0 * | |
-COOH | 8.2 | 9.9 | 14.8 ÷ 20.9 | 7.2 10.0 * | 15.7 ÷ 22.2 22.0 ÷ 31.1 * | |
-COONH4 | 8.1 | 10.2 | 11.4 ÷ 16.2 (13.4 ÷ 18.9) | 7.8 11.9 * | 12.4 ÷ 17.6 (14.5 ÷ 20.5) 18.9 ÷ 26.7 * (22.1 ÷ 31.2 *) | |
steel mill | 3 K | 295 K | ||||
as prepared | 9.8 | 13.6 | 17.9 ÷ 25.3 | 12.9 16.3 * | 18.5 ÷ 26.2 23.3 ÷ 33.0 * | |
-COOH | 8.0 | 11.7 | 10.1 ÷ 14.3 (11.8 ÷ 16.7) | 6.4 11.0 * | 11.3 ÷ 16.0 (13.2 ÷ 18.7) 19.3 ÷ 27.3 * (22.5 ÷ 31.9) * | |
-COONH4 | 8.9 | 10.5 | 12.1 ÷ 17.0 (14.1 ÷ 20.0) | 7.1 10.7 * | 13.1 ÷ 18.5 (15.3 ÷ 21.6) 19.7 ÷ 27.9 * (23.1 ÷ 32.6) * |
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Jamrozik, A.; Przewoznik, J.; Krysiak, S.; Korecki, J.; Trykowski, G.; Małolepszy, A.; Stobiński, L.; Burda, K. Effect of Grinding and the Mill Type on Magnetic Properties of Carboxylated Multiwall Carbon Nanotubes. Materials 2021, 14, 4057. https://doi.org/10.3390/ma14144057
Jamrozik A, Przewoznik J, Krysiak S, Korecki J, Trykowski G, Małolepszy A, Stobiński L, Burda K. Effect of Grinding and the Mill Type on Magnetic Properties of Carboxylated Multiwall Carbon Nanotubes. Materials. 2021; 14(14):4057. https://doi.org/10.3390/ma14144057
Chicago/Turabian StyleJamrozik, Agnieszka, Janusz Przewoznik, Sonia Krysiak, Jozef Korecki, Grzegorz Trykowski, Artur Małolepszy, Leszek Stobiński, and Kvetoslava Burda. 2021. "Effect of Grinding and the Mill Type on Magnetic Properties of Carboxylated Multiwall Carbon Nanotubes" Materials 14, no. 14: 4057. https://doi.org/10.3390/ma14144057