Ministry of Higher Education, Science and Technology of the Republic of Slovenia within the National Research Program

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Ministry of Higher Education, Science and Technology of the Republic of Slovenia within the National Research Program

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Publications

Hydrothermal synthesis of hematite (α-Fe2O3) nanoparticle forms: Synthesis conditions, structure, particle shape analysis, cytotoxicity and magnetic properties

Tadić, Marin; Trpkov, Đorđe; Kopanja, Lazar; Vojnović, Sandra; Panjan, Matjaž

(2019)

TY  - JOUR
AU  - Tadić, Marin
AU  - Trpkov, Đorđe
AU  - Kopanja, Lazar
AU  - Vojnović, Sandra
AU  - Panjan, Matjaž
PY  - 2019
UR  - https://linkinghub.elsevier.com/retrieve/pii/S0925838819312587
UR  - https://vinar.vin.bg.ac.rs/handle/123456789/8133
AB  - In this work, we present the magnetic and structural properties of α-Fe 2 O 3 nanoparticles synthesized by the hydrothermal synthesis method. XRD, FTIR and Raman spectroscopy indicate that the samples consist of single-phase α-Fe 2 O 3 nanoparticles. A microstructural analysis by TEM and SEM shows: (i) irregular nanoparticles (∼50 nm), (ii) plate-like nanoparticles (with thickness t∼10 nm and diameter d∼50–80 nm) and (iii) microsized ellipsoid 3D superstructures (with length l∼3.5 and diameter d∼1.5 μm) composed of nanosized building blocks (∼50 nm). We used circularity, elongation and convexity measures to quantitatively analyze the shape of the particles. Irregular hematite nanoparticles were synthesized using a water solution of ferric precursor and sodium acetate during the hydrothermal reaction (reaction conditions: T = 180 °C, t = 12 h). The same hydrothermal reaction temperature, reaction duration and ferric precursor (without sodium acetate) were used for synthesizing hematite ellipsoid 3D superstructures. Addition of urea and glycine surfactants in hydrothermal reaction resulted in the formation of nanoplate hematite particles. The role of these surfactants on the structure and morphology of the particles was also investigated. Magnetic measurements at the room temperature displayed a wide range of coercivities, from H C = 73 Oe for irregular nanoparticles, H C = 689 Oe for nanoplates to H C = 2688 Oe for hematite ellipsoid 3D superstructures. The measured coercivity for the ellipsoid superstructure was about 35 times higher than in the case of irregular hematite nanoparticles and about 4 times than the coercivity of hematite nanoplates. Magnetic properties of synthesized samples were related to their structure and morphology. We conclude that shape anisotropy influenced enhancement of the coercivity in hematite nanoplates whereas hematite ellipsoid 3D superstructure (nanoparticle clusters) induced the formation of multidomain magnetic structure and highest coercivity revealing its superior structure for enhanced magnetic properties. The synthesized hematite nanoparticle structures exhibit low cytotoxicity levels on the human lung fibroblasts (MRC5) cell line demonstrating a safe use of these nanoparticles for practical applications. © 2019 Elsevier B.V.
T2  - Journal of Alloys and Compounds
T1  - Hydrothermal synthesis of hematite (α-Fe2O3) nanoparticle forms: Synthesis conditions, structure, particle shape analysis, cytotoxicity and magnetic properties
VL  - 792
SP  - 599
EP  - 609
DO  - 10.1016/j.jallcom.2019.03.414
ER  - 
@article{
author = "Tadić, Marin and Trpkov, Đorđe and Kopanja, Lazar and Vojnović, Sandra and Panjan, Matjaž",
year = "2019",
abstract = "In this work, we present the magnetic and structural properties of α-Fe 2 O 3 nanoparticles synthesized by the hydrothermal synthesis method. XRD, FTIR and Raman spectroscopy indicate that the samples consist of single-phase α-Fe 2 O 3 nanoparticles. A microstructural analysis by TEM and SEM shows: (i) irregular nanoparticles (∼50 nm), (ii) plate-like nanoparticles (with thickness t∼10 nm and diameter d∼50–80 nm) and (iii) microsized ellipsoid 3D superstructures (with length l∼3.5 and diameter d∼1.5 μm) composed of nanosized building blocks (∼50 nm). We used circularity, elongation and convexity measures to quantitatively analyze the shape of the particles. Irregular hematite nanoparticles were synthesized using a water solution of ferric precursor and sodium acetate during the hydrothermal reaction (reaction conditions: T = 180 °C, t = 12 h). The same hydrothermal reaction temperature, reaction duration and ferric precursor (without sodium acetate) were used for synthesizing hematite ellipsoid 3D superstructures. Addition of urea and glycine surfactants in hydrothermal reaction resulted in the formation of nanoplate hematite particles. The role of these surfactants on the structure and morphology of the particles was also investigated. Magnetic measurements at the room temperature displayed a wide range of coercivities, from H C = 73 Oe for irregular nanoparticles, H C = 689 Oe for nanoplates to H C = 2688 Oe for hematite ellipsoid 3D superstructures. The measured coercivity for the ellipsoid superstructure was about 35 times higher than in the case of irregular hematite nanoparticles and about 4 times than the coercivity of hematite nanoplates. Magnetic properties of synthesized samples were related to their structure and morphology. We conclude that shape anisotropy influenced enhancement of the coercivity in hematite nanoplates whereas hematite ellipsoid 3D superstructure (nanoparticle clusters) induced the formation of multidomain magnetic structure and highest coercivity revealing its superior structure for enhanced magnetic properties. The synthesized hematite nanoparticle structures exhibit low cytotoxicity levels on the human lung fibroblasts (MRC5) cell line demonstrating a safe use of these nanoparticles for practical applications. © 2019 Elsevier B.V.",
journal = "Journal of Alloys and Compounds",
title = "Hydrothermal synthesis of hematite (α-Fe2O3) nanoparticle forms: Synthesis conditions, structure, particle shape analysis, cytotoxicity and magnetic properties",
volume = "792",
pages = "599-609",
doi = "10.1016/j.jallcom.2019.03.414"
}
Tadić, M., Trpkov, Đ., Kopanja, L., Vojnović, S.,& Panjan, M.. (2019). Hydrothermal synthesis of hematite (α-Fe2O3) nanoparticle forms: Synthesis conditions, structure, particle shape analysis, cytotoxicity and magnetic properties. in Journal of Alloys and Compounds, 792, 599-609.
https://doi.org/10.1016/j.jallcom.2019.03.414
Tadić M, Trpkov Đ, Kopanja L, Vojnović S, Panjan M. Hydrothermal synthesis of hematite (α-Fe2O3) nanoparticle forms: Synthesis conditions, structure, particle shape analysis, cytotoxicity and magnetic properties. in Journal of Alloys and Compounds. 2019;792:599-609.
doi:10.1016/j.jallcom.2019.03.414 .
Tadić, Marin, Trpkov, Đorđe, Kopanja, Lazar, Vojnović, Sandra, Panjan, Matjaž, "Hydrothermal synthesis of hematite (α-Fe2O3) nanoparticle forms: Synthesis conditions, structure, particle shape analysis, cytotoxicity and magnetic properties" in Journal of Alloys and Compounds, 792 (2019):599-609,
https://doi.org/10.1016/j.jallcom.2019.03.414 . .
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Magnetic properties of novel superparamagnetic iron oxide nanoclusters and their peculiarity under annealing treatment

Tadić, Marin; Kralj, Slavko; Jagodič, Marko; Hanžel, Darko; Makovec, Darko

(2014)

TY  - JOUR
AU  - Tadić, Marin
AU  - Kralj, Slavko
AU  - Jagodič, Marko
AU  - Hanžel, Darko
AU  - Makovec, Darko
PY  - 2014
UR  - https://vinar.vin.bg.ac.rs/handle/123456789/59
AB  - The aim of this work is to present the magnetic properties of novel superparamagnetic-iNANOvative (TM)vertical bar silica nanoparticle clusters. A TEM analysis showed that these nanoparticle clusters, approximately 80 nm in size, contained an assembly of maghemite nanoparticles in the core and an amorphous silica shell. The maghemite nanoparticles in the core were approximately 10 nm in size, whereas the uniform silica shell was approximately 15-nm thick. The number of magnetic nanoparticles that were densely packed in the core of the single nanocluster was estimated to be approximately 67, resulting in a high magnetic moment for the single nanocluster of m(nc) similar to 1.2 x 10(6) mu(B). This magnetic property of the nanoparticle cluster is advantageous for its easy manipulation using an external magnetic field, for example, in biomedical applications, such as drug delivery, or for magnetic separation in biotechnology. The magnetic properties of the iNANOvative (TM)vertical bar silica nanoparticle clusters were systematically studied, with a special focus on the influence of the magnetic interactions between the nanoparticles in the core. For comparison, the nanoparticle clusters were annealed for 3 h at 300 degrees C in air. The annealing had no influence on the nanoparticles size and phase; however, it had a unique effect on the magnetic properties, i.e., a decrease of the blocking temperature and a weakening of the inter-particle interactions. We believe that this surprising observation is related to the thermal decomposition of the organic surfactant on the surfaces of the nanoparticles at the high annealing temperatures, which resulted in the formation of amorphous carbon inside the nanocluster. (C) 2014 Elsevier B.V. All rights reserved.
T2  - Applied Surface Science
T1  - Magnetic properties of novel superparamagnetic iron oxide nanoclusters and their peculiarity under annealing treatment
VL  - 322
SP  - 255
EP  - 264
DO  - 10.1016/j.apsusc.2014.09.181
ER  - 
@article{
author = "Tadić, Marin and Kralj, Slavko and Jagodič, Marko and Hanžel, Darko and Makovec, Darko",
year = "2014",
abstract = "The aim of this work is to present the magnetic properties of novel superparamagnetic-iNANOvative (TM)vertical bar silica nanoparticle clusters. A TEM analysis showed that these nanoparticle clusters, approximately 80 nm in size, contained an assembly of maghemite nanoparticles in the core and an amorphous silica shell. The maghemite nanoparticles in the core were approximately 10 nm in size, whereas the uniform silica shell was approximately 15-nm thick. The number of magnetic nanoparticles that were densely packed in the core of the single nanocluster was estimated to be approximately 67, resulting in a high magnetic moment for the single nanocluster of m(nc) similar to 1.2 x 10(6) mu(B). This magnetic property of the nanoparticle cluster is advantageous for its easy manipulation using an external magnetic field, for example, in biomedical applications, such as drug delivery, or for magnetic separation in biotechnology. The magnetic properties of the iNANOvative (TM)vertical bar silica nanoparticle clusters were systematically studied, with a special focus on the influence of the magnetic interactions between the nanoparticles in the core. For comparison, the nanoparticle clusters were annealed for 3 h at 300 degrees C in air. The annealing had no influence on the nanoparticles size and phase; however, it had a unique effect on the magnetic properties, i.e., a decrease of the blocking temperature and a weakening of the inter-particle interactions. We believe that this surprising observation is related to the thermal decomposition of the organic surfactant on the surfaces of the nanoparticles at the high annealing temperatures, which resulted in the formation of amorphous carbon inside the nanocluster. (C) 2014 Elsevier B.V. All rights reserved.",
journal = "Applied Surface Science",
title = "Magnetic properties of novel superparamagnetic iron oxide nanoclusters and their peculiarity under annealing treatment",
volume = "322",
pages = "255-264",
doi = "10.1016/j.apsusc.2014.09.181"
}
Tadić, M., Kralj, S., Jagodič, M., Hanžel, D.,& Makovec, D.. (2014). Magnetic properties of novel superparamagnetic iron oxide nanoclusters and their peculiarity under annealing treatment. in Applied Surface Science, 322, 255-264.
https://doi.org/10.1016/j.apsusc.2014.09.181
Tadić M, Kralj S, Jagodič M, Hanžel D, Makovec D. Magnetic properties of novel superparamagnetic iron oxide nanoclusters and their peculiarity under annealing treatment. in Applied Surface Science. 2014;322:255-264.
doi:10.1016/j.apsusc.2014.09.181 .
Tadić, Marin, Kralj, Slavko, Jagodič, Marko, Hanžel, Darko, Makovec, Darko, "Magnetic properties of novel superparamagnetic iron oxide nanoclusters and their peculiarity under annealing treatment" in Applied Surface Science, 322 (2014):255-264,
https://doi.org/10.1016/j.apsusc.2014.09.181 . .
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Magnetic properties of NiMn2O4-delta (nickel manganite): Multiple magnetic phase transitions and exchange bias effect

Tadić, Marin; Savić, S. M.; Jagličić, Zvonko; Vojisavljevic, K.; Radojkovic, A.; Prsic, S.; Nikolic, Dobrica

(2014)

TY  - JOUR
AU  - Tadić, Marin
AU  - Savić, S. M.
AU  - Jagličić, Zvonko
AU  - Vojisavljevic, K.
AU  - Radojkovic, A.
AU  - Prsic, S.
AU  - Nikolic, Dobrica
PY  - 2014
UR  - https://vinar.vin.bg.ac.rs/handle/123456789/5850
AB  - We present magnetic properties of NiMn2O4-delta (nickel manganite) which was synthesized by complex polymerization synthesis method followed by successive heat treatment and final calcinations in air at 1200 degrees C. The sample was characterized by using X-ray powder diffractometer (XRPD), scanning electron microscopy (SEM), field-emission scanning electron microscopy (FE-SEM) and superconducting quantum interference device (SQUID) magnetometer. The XRPD and FE-SEM studies revealed NiMn2O4-delta phase and good crystallinity of particles. No other impurities have been observed by XRPD. The magnetic properties of the sample have been studied by measuring the temperature and field dependence of magnetization. Magnetic measurements of M(T) reveal rather complex magnetic properties and multiple magnetic phase transitions. We show three magnetic phase transitions with transition temperatures at T-M1 = 35 K (long-range antiferromagnetic transition), T-M2 = 101 K (antiferromagnetic-type transition) and T-M3 = 120 K (ferromagnetic-like transition). We found that the T-M1 transition is strongly dependent on the strength of the applied magnetic field (T-M1 decreases with increasing applied field) whereas the T-M3 is field independent. Otherwise, the T-M2 maximum almost disappears in higher applied magnetic fields (H = 1 kOe and 10 kOe). Magnetic measurements of M(H) show hysteretic behavior below T-M3. Moreover, hysteresis properties measured after cooling of the sample in magnetic field of 10 kOe show exchange bias effect with an exchange bias field vertical bar H-EB vertical bar= 196 Oe. In summary, the properties that distinguish the investigated NiMn2O4-delta sample from other bulk, thin film, ceramic and nanoparticle NiMn2O4-delta systems are the triple magnetic transitions with sharp increase of the ZFC and FC magnetizations at 120 K and the exchange bias effect. The analysis of the results and comparison with literature data allowed us to conjecture that the mixed oxidation states of Mn ions, ferromagnetic and antiferromagnetic sublattice orders and surface effects in the sample tailor these interesting magnetic properties. (C) 2013 Elsevier B. V. All rights reserved.
T2  - Journal of Alloys and Compounds
T1  - Magnetic properties of NiMn2O4-delta (nickel manganite): Multiple magnetic phase transitions and exchange bias effect
VL  - 588
SP  - 465
EP  - 469
DO  - 10.1016/j.jallcom.2013.11.025
ER  - 
@article{
author = "Tadić, Marin and Savić, S. M. and Jagličić, Zvonko and Vojisavljevic, K. and Radojkovic, A. and Prsic, S. and Nikolic, Dobrica",
year = "2014",
abstract = "We present magnetic properties of NiMn2O4-delta (nickel manganite) which was synthesized by complex polymerization synthesis method followed by successive heat treatment and final calcinations in air at 1200 degrees C. The sample was characterized by using X-ray powder diffractometer (XRPD), scanning electron microscopy (SEM), field-emission scanning electron microscopy (FE-SEM) and superconducting quantum interference device (SQUID) magnetometer. The XRPD and FE-SEM studies revealed NiMn2O4-delta phase and good crystallinity of particles. No other impurities have been observed by XRPD. The magnetic properties of the sample have been studied by measuring the temperature and field dependence of magnetization. Magnetic measurements of M(T) reveal rather complex magnetic properties and multiple magnetic phase transitions. We show three magnetic phase transitions with transition temperatures at T-M1 = 35 K (long-range antiferromagnetic transition), T-M2 = 101 K (antiferromagnetic-type transition) and T-M3 = 120 K (ferromagnetic-like transition). We found that the T-M1 transition is strongly dependent on the strength of the applied magnetic field (T-M1 decreases with increasing applied field) whereas the T-M3 is field independent. Otherwise, the T-M2 maximum almost disappears in higher applied magnetic fields (H = 1 kOe and 10 kOe). Magnetic measurements of M(H) show hysteretic behavior below T-M3. Moreover, hysteresis properties measured after cooling of the sample in magnetic field of 10 kOe show exchange bias effect with an exchange bias field vertical bar H-EB vertical bar= 196 Oe. In summary, the properties that distinguish the investigated NiMn2O4-delta sample from other bulk, thin film, ceramic and nanoparticle NiMn2O4-delta systems are the triple magnetic transitions with sharp increase of the ZFC and FC magnetizations at 120 K and the exchange bias effect. The analysis of the results and comparison with literature data allowed us to conjecture that the mixed oxidation states of Mn ions, ferromagnetic and antiferromagnetic sublattice orders and surface effects in the sample tailor these interesting magnetic properties. (C) 2013 Elsevier B. V. All rights reserved.",
journal = "Journal of Alloys and Compounds",
title = "Magnetic properties of NiMn2O4-delta (nickel manganite): Multiple magnetic phase transitions and exchange bias effect",
volume = "588",
pages = "465-469",
doi = "10.1016/j.jallcom.2013.11.025"
}
Tadić, M., Savić, S. M., Jagličić, Z., Vojisavljevic, K., Radojkovic, A., Prsic, S.,& Nikolic, D.. (2014). Magnetic properties of NiMn2O4-delta (nickel manganite): Multiple magnetic phase transitions and exchange bias effect. in Journal of Alloys and Compounds, 588, 465-469.
https://doi.org/10.1016/j.jallcom.2013.11.025
Tadić M, Savić SM, Jagličić Z, Vojisavljevic K, Radojkovic A, Prsic S, Nikolic D. Magnetic properties of NiMn2O4-delta (nickel manganite): Multiple magnetic phase transitions and exchange bias effect. in Journal of Alloys and Compounds. 2014;588:465-469.
doi:10.1016/j.jallcom.2013.11.025 .
Tadić, Marin, Savić, S. M., Jagličić, Zvonko, Vojisavljevic, K., Radojkovic, A., Prsic, S., Nikolic, Dobrica, "Magnetic properties of NiMn2O4-delta (nickel manganite): Multiple magnetic phase transitions and exchange bias effect" in Journal of Alloys and Compounds, 588 (2014):465-469,
https://doi.org/10.1016/j.jallcom.2013.11.025 . .
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Magnetic properties of hematite (alpha-Fe2O3) nanoparticles prepared by hydrothermal synthesis method

Tadić, Marin; Panjan, Matjaž; Damnjanović, Vesna; Milošević, Irena

(2014)

TY  - JOUR
AU  - Tadić, Marin
AU  - Panjan, Matjaž
AU  - Damnjanović, Vesna
AU  - Milošević, Irena
PY  - 2014
UR  - https://vinar.vin.bg.ac.rs/handle/123456789/225
AB  - Hematite (alpha-Fe2O3) nanoparticles are successfully synthesized by using the hydrothermal synthesis method. An X-ray powder diffraction (XRPD) of the sample shows formation of the nanocrystalline alpha-Fe2O3 phase. A transmission electron microscopy (TEM) measurements show spherical morphology of the hematite nanoparticles and narrow size distribution. An average hematite nanoparticle size is estimated to be about 8 nm by TEM and XRD. Magnetic properties were measured using a superconducting quantum interference device (SQUID) magnetometry. Investigation of the magnetic properties of hematite nanoparticles showed a divergence between field-cooled (FC) and zero-field-cooled (ZFC) magnetization curves below T-irr =103 K (irreversibility temperature). The ZFC magnetization curve showed maximum at T-B = 52 K (blocking temperature). The sample did not exhibit the Morin transition. The M(H) (magnetization versus magnetic field) dependence at 300 K showed properties of superparamagnetic iron oxide nanoparticles (SPION). The M(H) data were successfully fitted by the Langevin function and magnetic moment,up = 657 tu and diameter d= 8.1 nm were determined. Furthermore, magnetic measurements showed high magnetization at room temperature (M-S =3.98 emu/g), which is desirable for application in spintronics and biomedicine. Core-shell structure of the nanoparticles was used to describe high magnetization of the hematite nanoparticles. (C) 2014 Elsevier B.V. All rights reserved.
T2  - Applied Surface Science
T1  - Magnetic properties of hematite (alpha-Fe2O3) nanoparticles prepared by hydrothermal synthesis method
VL  - 320
SP  - 183
EP  - 187
DO  - 10.1016/j.apsusc.2014.08.103
ER  - 
@article{
author = "Tadić, Marin and Panjan, Matjaž and Damnjanović, Vesna and Milošević, Irena",
year = "2014",
abstract = "Hematite (alpha-Fe2O3) nanoparticles are successfully synthesized by using the hydrothermal synthesis method. An X-ray powder diffraction (XRPD) of the sample shows formation of the nanocrystalline alpha-Fe2O3 phase. A transmission electron microscopy (TEM) measurements show spherical morphology of the hematite nanoparticles and narrow size distribution. An average hematite nanoparticle size is estimated to be about 8 nm by TEM and XRD. Magnetic properties were measured using a superconducting quantum interference device (SQUID) magnetometry. Investigation of the magnetic properties of hematite nanoparticles showed a divergence between field-cooled (FC) and zero-field-cooled (ZFC) magnetization curves below T-irr =103 K (irreversibility temperature). The ZFC magnetization curve showed maximum at T-B = 52 K (blocking temperature). The sample did not exhibit the Morin transition. The M(H) (magnetization versus magnetic field) dependence at 300 K showed properties of superparamagnetic iron oxide nanoparticles (SPION). The M(H) data were successfully fitted by the Langevin function and magnetic moment,up = 657 tu and diameter d= 8.1 nm were determined. Furthermore, magnetic measurements showed high magnetization at room temperature (M-S =3.98 emu/g), which is desirable for application in spintronics and biomedicine. Core-shell structure of the nanoparticles was used to describe high magnetization of the hematite nanoparticles. (C) 2014 Elsevier B.V. All rights reserved.",
journal = "Applied Surface Science",
title = "Magnetic properties of hematite (alpha-Fe2O3) nanoparticles prepared by hydrothermal synthesis method",
volume = "320",
pages = "183-187",
doi = "10.1016/j.apsusc.2014.08.103"
}
Tadić, M., Panjan, M., Damnjanović, V.,& Milošević, I.. (2014). Magnetic properties of hematite (alpha-Fe2O3) nanoparticles prepared by hydrothermal synthesis method. in Applied Surface Science, 320, 183-187.
https://doi.org/10.1016/j.apsusc.2014.08.103
Tadić M, Panjan M, Damnjanović V, Milošević I. Magnetic properties of hematite (alpha-Fe2O3) nanoparticles prepared by hydrothermal synthesis method. in Applied Surface Science. 2014;320:183-187.
doi:10.1016/j.apsusc.2014.08.103 .
Tadić, Marin, Panjan, Matjaž, Damnjanović, Vesna, Milošević, Irena, "Magnetic properties of hematite (alpha-Fe2O3) nanoparticles prepared by hydrothermal synthesis method" in Applied Surface Science, 320 (2014):183-187,
https://doi.org/10.1016/j.apsusc.2014.08.103 . .
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