Saccharide-capped Superparamagnetic Copper Cations-doped Magnetite Nanoparticles for Biomedical Applications: A Novel and Simple Synthesis Procedure, In-situ Surface Engineering and Characterization

2020 ◽  
Vol 16 (5) ◽  
pp. 770-778
Author(s):  
Mustafa Aghazadeh ◽  
Mohammad Reza Ganjali ◽  
Mina Mohebi Morad ◽  
Davoud Gharailou

Background: Recently, superparamagnetic and electromagnetic nano-materials have been extensively studied and their potential applications have also been investigated in various fields. In this regard, currently, Fe3O4 NPs are valuable candidates as diagnostic agents such as magnetic resonance imaging, enzyme immobilization, biosensing and cell labeling, and therapeutic probes, including drug delivery, bacteria detection, magnetic separation, and hyperthermia agents. Objective: In this study, electrochemical synthesis of Cu2+ cations-doped superparamagnetic magnetite nanoparticles (Cu-SMNPs) and their in situ surface coating with saccharides (i.e., glucose, sucrose and starch) are reported. The prepared glucose/Cu-SMNPs, sucrose/Cu-SMNPs and starch/Cu-SMNPs samples are characterized by structural, magnetic and morphological analyses by XRD, FT-IR, FE-SEM, EDAX and VSM. The suitability of the prepared samples for biomedical use is also proved. Methods: A simple cathodic electrochemical set-up was used to fabricate the iron oxide samples. The bath electrolyte was one litre deionized water containing 1.5g iron chloride, 3g iron nitrate, 0.5g copper chloride and 0.5g saccharide (i.e., glucose or sucrose or starch). The cathode and anode electrodes were connected to a DC power supply (PROVA 8000) as the power source. The deposition experiments were conducted at 10 mA cm-2 for 30 min. For the preparation of glucose/Cu-SMNPs, sucrose/Cu-SMNPs and starch/Cu-SMNPs samples, three electrodeposition experiments were carried out in three similar baths with only a change in the dissolved saccharide type. The prepared SMNPs samples were characterized by structural, morphological and magnetic analyses including X-ray powder diffraction (XRD, a Phillips PW-1800 diffractometer Smart Lab), field-emission scanning electron microscopy (FE-SEM, Mira 3-XMU with accelerating voltage of 100 kV), transmission electron microscopy (TEM, model Zeiss EM900 with an accelerating voltage of 80 kV), fourier transform infrared (FT-IR, a Bruker Vector 22 Fourier transformed infrared spectrometer) and vibrating sample magnetometers (VSM, model Lakeshore 7410). Results: Three types of metal-cations doped superparamagnetic magnetite nanoparticles (SMNPs), glucosegrafted Cu2+-doped MNPs (glucose/Cu-SMNPs), sucrose-grafted Cu2+-doped SMNPs (sucrose/Cu-SMNPs) and starch-grafted Cu2+-doped SMNPs (starch/Cu-SMNPs), were prepared for the first time. Fourier-transform infrared spectroscopy, field-emission scanning electron microscopy and energy dispersive X-ray techniques proved the presence of saccharide capped layer on the surface of deposited SMNPs and also copper cations doping on their crystal structures. Superparamagnetic behaviors, including low coercivity and remanence values, were observed for all the prepared samples. Conclusion: SMNPs capped with saccharides (i.e., glucose, sucrose and starch) were successfully synthesized via one-pot simple deposition procedures. These particles showed suitable superparamagnetic properties with negligible remanence values and proper saturation magnetization, thus proving that they all have required physicochemical and magnetic characteristics for biomedical purposes.

2013 ◽  
Vol 774-776 ◽  
pp. 629-633
Author(s):  
Ji Feng Jiang ◽  
Kang Kang Guo ◽  
Ya Ping Zhu ◽  
Fan Wang ◽  
Hui Min Qi

Triethynylborazine-polyhydromethylsiloxane copolymers (TEB-PHMSs) were prepared through hydrosilylation reaction between -C≡CH attached to boron and ≡Si-H. The structures of TEB-PHMSs were characterized by Fourier transform Infrared (FT-IR) and Nuclear Magnetic Resonance (NMR) spectroscopy. Their cure behavior were examined by Differential Scanning Calorimeter (DSC) and FT-IR, and then thermostability and ceramization of cured TEB-PHMS were investigated by Thermogravimetric analysis (TGA), pyrolysis-GC-MS, X-ray diffraction (XRD) and Scanning Electron Microscopy (SEM). The results indicated that TEB-PHMSs could be cured and converted into an outstanding thermostable SiBCN ceramics.


2014 ◽  
Vol 17 (3) ◽  
pp. 80-85
Author(s):  
Nur Dwi Lestari ◽  
Pardoyo Pardoyo ◽  
Agus Subagio

Telah dilakukan penelitian sintesis dan karakterisasi CNT (Carbon Nanotube) dengan doping logam kobalt. Penelitian ini bertujuan untuk menentukan karakter CNT sebelum dan setelah didoping dengan variasi konsentrasi logam 10%, 20%, 30%, 40% dan 50%. Metode yang digunakan pada penelitian ini adalah impregnasi basah yang meliputi perendaman pada larutan logam dan kalsinasi. Hasil impregnasi dianalisis menggunakan Fourier Transform-Infra Red (FT-IR), GSA (Gas Sorption Analysis), Scanning Electron Microscopy (SEM) dan Energy Dispersive X-Ray Spectroscopy (EDS). Analisis FT-IR menunjukkan adanya vibrasi ulur dari ikatan Co-C dan Co-O.  Hasil GSA menunjukkan bahwa CNT loading 30% mempunyai luas permukaan tertinggi yaitu 69,192 m2/g. Hasil SEM-EDS menunjukkan bahwa morfologi permukaan dinding CNT ditutupi aggregat-aggregat kobalt. Pada hasil EDS fraksi kobalt dihasilkan adalah 1,96 % yang nilainya tidak jauh berbeda dari fraksi Fe yaitu 1,49%. Hal ini menunjukkan bahwa CNT doping logam Co menggunakan metode impregnasi basah tidak efektif.


2014 ◽  
Vol 789 ◽  
pp. 259-261
Author(s):  
Zhi Jie Wang ◽  
Jing Hua Gong ◽  
Shu Guang Yang ◽  
Jing Hong Ma ◽  
Jian Xu

Polyvinylpyrrolidone (PVP)/boehmite nanocomposites fibers were successfully prepared by electrospinning using boehmite sol containing PVP as the spinning solution. Several techniques, including Fourier transform infrared (FT-IR), thermal gravimetric analyzer (TGA) and field emission scanning electron microscopy (FE-SEM) were used to characterize their ingredients, thermal properties and morphology. The results showed that PVP concentration exhibited significant effect on the PVP/boehmite nanofibers morphology. With increasing PVP concentration, the morphology changed from beaded, beaded fiber to uniform fiber. These PVP/boehmite nanofibers can be used as good candidates for continuously preparing uniform and compact alumina nanofibers.


RSC Advances ◽  
2016 ◽  
Vol 6 (54) ◽  
pp. 48329-48335 ◽  
Author(s):  
Heng-Zhi Duan ◽  
Hong-Yan Zeng ◽  
Hua-Miao Xiao ◽  
Chao-Rong Chen ◽  
Gao-Fei Xiao ◽  
...  

SO42− intercalated Mg–Al hydrotalcite (S-LDH) was prepared under microwave irradiation and characterized by powder X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM).


2011 ◽  
Vol 295-297 ◽  
pp. 1675-1679
Author(s):  
Chang Yu Liu ◽  
Shu Liang Wang ◽  
Jian Li ◽  
Cheng Yu Wang

Amphiphobic vaterite with a size of about 50 nm, was prepared via crystallization of CaCO3with perfluorooctane surfapropyl betaine(DF-921)in methanol by mimicking the process of biomineralization. The products were analyzed by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) and contact angle analysis. The results indicate that the CaCO3powder samples had both hydrophobic and oleophobic properties. The DF-921 used in this research not only controlled the crystal type of the CaCO3particles but also changed the surface properties of the final products.


2017 ◽  
Vol 888 ◽  
pp. 136-140 ◽  
Author(s):  
Suzi Salwah Jikan ◽  
Nur Azam Badarulzaman ◽  
Shehu Yahaya ◽  
Ajiya Dahiru Adamu

The effect of milling on structure of kaolinite-urea intercalates were studied. Untreated and treated kaolinite samples were examined by Field scanning electron microscopy (FESEM), X-ray powder diffraction (XRPD) and Fourier transform infrared (FT-IR) spectroscopy. The basal spacing of kaolinite measured by X-ray powder diffraction (XRPD) increased from 1.02 to 3.62 nm after intercalation by urea. Significantly, nature of intercalation was reached through formation of hydrogen bonds between urea and both Si-O and AlOH groups of the interlayer surface of kaolinite.


2018 ◽  
Vol 54 (4B) ◽  
pp. 80
Author(s):  
Luu Cam Loc

In this work, photocatalysts TiO2-HT prepared by hydrothermal method and TiO2-P25 Degussa were characterized by Energy Dispersive X-Ray analysis (EDX), X-ray powder diffraction analysis (XRD), Raman Spectroscopy, BET surface area measurements, scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) and UV-Vis absorption spectroscopy and tested in degradation of recalcitrant organic pollutants in bio-treated seafood wastewater (COD > 80 mg/L). After 9 hours of photodegradation under UV-A irradiation, COD removal efficiency reached 85.6 % and 48.9 % on TiO2-P25 and TiO2 catalysts, respectively. COD values of seafood wastewater treated by photocatalysis met the standard discharge requirement - QCVN 11:2008 – level A (COD £ 50 mg/L). 


2016 ◽  
Vol 5 (1) ◽  
pp. 6
Author(s):  
Budi Setiawan ◽  
Erizal Zaini ◽  
Salman Umar

Sebuah penelitian tentang sistem dispersi padat dari asiklovir dengan poloxamer 188 telah dilakukan formulasi dengan pencampuran secara fisika dengan rasio 1 : 1, 1 : 3, 1 : 5 dan dispersi padat 1 : 1, 1 : 3, 1 : 5 dan penggilingan 1:1 sebagai pembanding. Dispersi padat dibuat menggunakan metode pencairan (fusi), yang digabung dengan poloxamer 188 pada hotplate kemudian asiklovir dimasukkan ke dalam hasil poloxamer 188 lalu di kocok hingga membentuk masa homogen. Semua formula yang terbentuk termasuk asiklovir poloxamer 188 murni dianalisis karakterisasinya dengan Differential Thermal Analysis (DTA), X-ray Diffraction, Scanning Electron Microscopy (SEM), dan Fourier Transform Infrared (FTIR), kemudian pengambilan dilakukan  (penentuan kadar) mengunakan spektrofotometer UV pada panjang gelombang 257,08 nm dan uji laju disolusi dengan aquadest bebas CO2 menggunakan metode dayung. Hasil pengambilan  (penentuan kadar) menunjukkan bahwa semua formula memenuhi persyaratan farmakope Amerika edisi 30 dan farmakope Indonesia edisi 4 yaitu 95-110%. Sedangkan hasil uji laju disolusi untuk campuran fisik 1: 1, dan dispersi padat 1: 1, dan penggilingan 1: 1 menunjukkan peningkatan yang nyata dibandingkan asiklovir murni. Hal ini juga dapat dilihat dari hasil perhitungan statistik  menggunakan analisis varian satu arah  SPSS 17.


2012 ◽  
Vol 476-478 ◽  
pp. 2059-2062
Author(s):  
Chen Wang ◽  
Ya Dong Li ◽  
Gu Qiao Ding

Tributyl borate was first adopted for the introduction of boron in the preparation of bioactive borosilicate xerogel by sol-gel method. The xerogel reacted continuously in 0.25M K2HPO4 solution with a starting pH value of 7.0 at 37 °C for 1day. The structural, morphologies and compositional changes resulting from the conversion were characterized using X-ray diffraction, scanning electron microscopy and Fourier transform infrared spectroscopy. The results indicated that speed of formation of HA was cut way back on the time with the addition of boron and the induction period for the HA nucleation on the surface of the borosilicate xerogel was short than 1 days. The conversion mechanism of the borosilicate xerogels to hydroxyapaptite was also discussed.


2014 ◽  
Vol 20 (5) ◽  
pp. 1534-1543 ◽  
Author(s):  
Annalaura Restivo ◽  
Ilaria Degano ◽  
Erika Ribechini ◽  
Josefina Pérez-Arantegui ◽  
Maria Perla Colombini

Abstract:An innovative approach, combining field-emission scanning electron microscopy (FESEM) with energy dispersive X-ray spectroscopy (EDX) analysis, is presented to investigate the degradation mechanisms affecting tannin-dyed wool. In fact, tannin-dyed textiles are more sensitive to degradation then those dyed with other dyestuffs, even in the same conservation conditions.FESEM-EDX was first used to study a set of 48 wool specimens (artificially aged) dyed with several raw materials and mordants, and prepared according to historical dyeing recipes. EDX analysis was performed on the surface of wool threads and on their cross-sections. In addition, in order to validate the model formulated by the analysis of reference materials, several samples collected from historical and archaeological textiles were subjected to FESEM-EDX analysis.FESEM-EDX investigations enabled us to reveal the correlation between elemental composition and morphological changes. In addition, aging processes were clarified by studying changes in the elemental composition of wool from the protective cuticle to the fiber core in cross-sections. Morphological and elemental analysis of wool specimens and of archaeological and historical textiles showed that the presence of tannins increases wool damage, primarily by causing a sulfur decrease and fiber oxidation.


Sign in / Sign up

Export Citation Format

Share Document