Synthesis and Character of Amphiphobic Calcium Carbonate Nanoparticles In Situ

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.

2021 ◽  
Author(s):  
Fatma Unal

Abstract Terbium oxide (Tb2O3) particles (NPs) were synthesized by precipitation method using ammonium carbonate as precipitation agent. Effects of precursor molarity (0.1, 0.15 and 0.2 M) on photoluminescence (PL) behaviour of the NPs were investigated. The presence of the Tb2O3 phase was confirmed by X-Ray Diffraction (XRD) and Fourier-transform infrared spectroscopy (FT-IR) analyses. Morphological investigations of the produced powders were made by Field Emission Gun-Scanning Electron Microscopy (FEG-SEM). It showed that the morphology of Tb2O3 particles transformed from the nanograin chain to bundles morphology of rod-like as the amount of precursor molarity increased. Emission spectrum were investigated by Photoluminescence (PL) Spectroscopy. All the Tb2O3 particles exhibited the strongest peak at 493 nm ascribed to 5D4-7F6 (magnetic dipole (MD), C2) transition. The increase in the number of C2 sites released from the MD transition with the increase of the precursor molarity caused a negative increase in the b* (yellowness/blueness of the emission) value in the CIE diagram, indicating that the colour shifted to the blue region. The Tb2O3 particles produced by the precipitation method exhibited novel strong cyan colour and the PL emission intensity increased with increasing molarity.


Author(s):  
Aniek Setiya Budiatin ◽  
Samirah ◽  
Maria Apriliani Gani ◽  
Wenny Putri Nilamsari ◽  
Chrismawan Ardianto ◽  
...  

Bovine bone is a considerable source for the production of hydroxyapatite. The recent study reported a novel method to extract hydroxyapatite from bovine bone without producing hazardous residue. The bovine bones were cut and boiled in the opened chamber followed by boiling in pressurized tank. The bones were then soaked into 95% ethanol. Calcination was then conducted in 800°C, 900°C and 1,000°C, for 2 hours. The result was then grinded and sieved. The powder then was characterized using Fourier transform infrared (FT-IR), Scanning electron microscopy (SEM) and X-ray diffraction analysis (XRD) to measure the purity of hydroxyapatite. It is concluded that the hydroxyapatite derived from this process showed 100% purity, resulting 35.34 ± 0.39% w/w from the wet bone weight and 72.3% w/w from the dried weight. The present extraction method has been proven to yield high amount of pure hydroxyapatite as well as reducing the use of hazardous reagent.


2013 ◽  
Vol 457-458 ◽  
pp. 244-247
Author(s):  
Min Li ◽  
Li Guang Xiao ◽  
Hong Kai Zhao

Polyethylene/montmorillonite (PE/MMT) nanocomposites were prepared by in situ polymerization. The morphology of MMT/MgCl2/TiCl4 catalyst and PE/MMT nanocomposites was investigated by scanning electron microscopy (SEM). It can be seen that MMT/MgCl2/TiCl4 catalyst remained the original MMT sheet structures and many holes were found in MMT and the morphology of PE/MMT nanocomposites is part of the sheet in the form of existence, as most of the petal structure. X-ray diffraction (XRD) and transmission electron microscopy (TEM) were carried out to characterize all the samples. XRD results reveal that the original basal reflection peak of PEI1 and PEI2 disappears completely and that of PEI3 become very weak. MMT/MgCl2/TiCl4 catalyst was finely dispersed in the PE matrix. Instead of being individually dispersed, most layers were found in thin stacks comprising several swollen layers.


2015 ◽  
Vol 1120-1121 ◽  
pp. 572-575
Author(s):  
Hong Wei Liu ◽  
Feng Wang ◽  
Qiang Zhang ◽  
Xi Wu Li ◽  
Zhi Hui Li ◽  
...  

An innovative spray deposition technique has been applied to produce in situ TiB2/Zn-30Al-1Cu composites. The microstructures of the spray-deposited composite were studied using optical microscopy, scanning electron microscopy, and X-ray diffraction. Both theoretical and experimental results have shown that the TiB2particulates are formed in the microstructure. It was found that the TiB2particles were distributed in Zn-30Al-1Cu matrix uniformly, and the TiB2particles are about 2 μm in size. Moreover, the presence of the TiB2particles was led to increasing of α’ phase with less 2 μm size in the composites which have a tendency to decompose to α+η structure.


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.


2015 ◽  
Vol 817 ◽  
pp. 593-598
Author(s):  
Yan Feng Liang ◽  
Sheng Quan Dong ◽  
Gao Hong Li

In situ TiCp/Al-4.5wt.%Cu composites have been coated using an electro-less Ni-P plating technique. The morphology and composition of the plating coating have been examined by scanning electron microscopy, optical microscopy, and X-ray diffraction. The results indicated that the coating had a high-phosphorus amorphous microstructure. The coatings microstructures showed significantly changes when the citric acid concentration in the chemical bath was varied in the range 16-20g/L.


2016 ◽  
Author(s):  
Στυλιανός Κυριαζής

Οι παθήσεις των οστών και η θεραπεία τους σχετίζονται άμεσα με την γνώση των βλαβών που προκαλούν οι ασθένειες σε μοριακό επίπεδο των βιολογικών μορίων, ιστών και υγρών του σώματος. Μέχρι σήμερα, πολλές από τις ασθένειες δεν μπορούν να αντιμετωπιστούν μη επεμβατικά, επειδή δεν έχουν παρασκευασθεί φάρμακα τα οποία θα μπορούσαν να επιδιορθώσουν τις βλάβες. Δυστυχώς, μέχρι σήμερα, η συνήθης αντιμετώπιση των περισσότερων ασθενειών είναι η χειρουργική αφαίρεση του τμήματος του οστού που έχει φθαρεί. Η γνώση επομένως των βλαβών οι οποίες προκαλούνται από τις ασθένειες θα μπορούσε ενδεχομένως να οδηγήσει στην ανάπτυξη φαρμάκων και την εξέλιξη της μη επεμβατικής αντιμετώπισης αυτών των ασθενειών .Στην παρούσα μελέτη χρησιμοποιήθηκαν μη καταστρεπτικές μέθοδοι, όπως η υπέρυθρη φασματοσκοπία με μετασχηματισμό Fourier (Fourier Transform Infrared, FT-IR) και ηλεκτρονιακό μικροσκόπιο σάρωσης (Scanning Electron Microscopy, SEM) και περίθλαση ακτίνων Χ (XRD, X-Ray Diffraction).Για την μελέτη λήφθηκαν δείγματα φλοιώδους και σπογγώδους οστού, καθώς και χόνδρου οστού από 42 ασθενείς ηλικίας 31 έως 87 ετών, οι οποίοι υποβλήθηκαν σε χειρουργική αντιμετώπιση. Από αυτά 15 προήλθαν από ασθενείς με αναπτυξιακή δυσπλασία του ισχίου, 1 από αγκυλοποιητική αρθρίτιδα του ισχίου, 4 από έκτοπη οστεοποίηση του ισχίου, 3 λόγω οστεονέκρωσης της μηριαίας κεφαλής, 1 από ρευματοειδή αρθρίτιδα του γόνατος, 2 έπειτα από χαλάρωση ολικής αρθροπλαστικής γόνατος, 4 έπειτα από χαλάρωση ολικής αρθροπλαστικής ισχίου και 2 από ψωριασική αρθρίτιδα (ισχίου και γόνατος) και 10 καρκινικά. Τα δείγματα δεν υπέστησαν καμία επεξεργασία πέραν της αφαίρεσης των προσμίξεων αίματος και λιπαρών συστατικών του εξωτερικού περιβάλλοντος του οστού. Τα υπέρυθρα φάσματα έδειξαν σημαντικές διαφορές μεταξύ των υγιών οστών και των οστών τα οποία προήλθαν από τα δείγματα των ασθενών. Οι μεταβολές ήταν συνάρτηση της ασθένειας αλλά και των συστατικών του εκάστοτε οστού. Γενικά διαπιστώθηκε ότι σε κάθε περίπτωση το οξειδωτικό στρες συμμετέχει σε κάποιο από τα στάδια της ανάπτυξης της ασθένειας. Κατά το οξειδωτικό στρες παράγονται ελεύθερες ρίζες (ROS, reactive oxygen species) οι οποίες οδηγούν σε υπεροξείδωση των λιπιδίων και φωσφολιπιδίων των μεμβρανών των κυττάρων και κατά συνέπεια στην καταστροφή των κυττάρων. Από τις μειώσεις των εντάσεων και τις μετατοπίσεις των απορροφήσεων τάσης των ομάδων νΟΗ και νΝΗ στην περιοχή του φάσματος από 4000-3000 cm-1 φαίνεται ότι ο υδροξυαπατίτης χάνει τις ομάδες -ΟΗ, ενώ οι δεσμοί υδρογόνου οι οποίοι συγκρατούν την α-έλικα των κολλαγονούχων πρωτεϊνών μεταβάλλουν την έντασή τους. Αυτό επιβεβαιώνεται από τις μετατοπίσεις των ταινιών των Amide I και Amide II των πρωτεϊνών προς μικρότερες συχνότητες στην περιοχή 1700-1500 cm-1, ως αποτέλεσμα της καταστροφής της α-έλικας. Το φαινόμενο αυτό είναι περισσότερο έντονο στην περίπτωση των χόνδρων. Η ταινία περίπου στα 3080 cm-1, η οποία συνδέεται με την ολεφινική ομάδα (v=CH) επιβεβαιώνει την επίδραση των ελευθέρων ριζών στα στάδια της ασθένειας. Η αύξηση των εντάσεων των ταινιών των μεθυλ (vCH3) και μεθυλενομάδων (vCH2) στην περιοχή 3000-2850 cm-1 συνδέεται με την αύξηση του λιπόφιλου περιβάλλοντος, ως αποτέλεσμα της επίδρασης του οξειδωτικού στρες και τον σχηματισμό αμυλοειδών πρωτεϊνών. Η ταινία στα 1743 cm-1 η οποία αποδίδεται σε σχηματισμό αλδεϋδικών ομάδων συνδέεται με το οξειδωτικό στρες και επομένως με την φλεγμονή. Σε ασθενείς οι οποίοι εμφάνιζαν χρόνια φλεγμονή η ένταση της ταινίας είναι αρκετά υψηλή. Τα υπέρυθρα φάσματα έδειξαν την καταστροφή του υδροξυαπατίτη των οστών και την μετατροπή του σε άλατα του φωσφορικού ασβεστίου, προσδίδοντας επομένως μεγαλύτερη σκληρότητα και ευθραυστότητα στο οστό. Η καταστροφή του βιολογικού υδροξυαπατίτη επιβεβαιώθηκε με XRD ανάλυση.Οι SEM αναλύσεις έδειξαν την καταστροφή των πρωτεϊνών του οστού. Από την ανάλυση της εικόνας φάνηκαν οι θέσεις διασταυρούμενων (cross-link) και διακλαδούμενων (branch-link) πολυμερισμών. Οι θέσεις αυτές αποτελούν δραστικά σημεία σχηματισμού φωσφορικών αλάτων, τα οποία μειώνουν την αντοχή των οστών. Επίσης επιβεβαιώνουν την επίδραση των ελευθέρων ριζών.Η έκτοπη οστεοποίηση φαίνεται να μην είναι αποτέλεσμα της δράσης των οστεοβλαστών, αλλά της αδυναμίας λειτουργίας του ATP στον φυσιολογικό κύκλο λόγω ισχαιμικών επεισοδίων που επικρατούν στην περιοχή ανάπτυξης του οστού. Αυτό επιβεβαιώθηκε από την σύγκριση των φασμάτων έκτοπου οστού και επασβεστωμένης αορτικής βαλβίδας. Τέλος, στον σχηματισμό των αμυλοειδών πρωτεϊνών αποδίδουμε την αντίσταση στην θεραπευτική αγωγή και ακτινοθεραπεία των οστών.


2011 ◽  
Vol 696 ◽  
pp. 290-295 ◽  
Author(s):  
Vladislav Kolarik ◽  
Maria del Mar Juez-Lorenzo ◽  
Harald Fietzek

Micro-sized spherical Al particles have recently attracted interest for the development of a new concept for coatings based on their capability to form hollow alumina spheres and aluminized diffusion zones in the substrate. For understanding better their oxidation behaviour, spherical µm-Al particles with different sizes were oxidized in air on heating up to 1300°C and under isothermal conditions at 800°C and 850°C. The oxide formation was studiedin situby high temperature X-ray diffraction and the oxidised particles were analysed by scanning electron microscopy. On heating the µm-Al particles begin to form a g-Al2O3scale before reaching the melting point and the molten Al is kept within the g-Al2O3shell. On further heating q-Al2O3is detected, which forms simultaneously with the g-Al2O3. The g-Al2O3/ q-Al2O3scale is stable and protective under isothermal conditions up to 800°C within the investigated times. On further heating the g-Al2O3and q-Al2O3transform simultaneously to a-Al2O3in a temperature range of 850°C to 1100°C. Under isothermal conditions the g à a-Al2O3transformation is observed after 160 min at 850°C. During the g à a-Al2O3transformation shrinkage occurs that leads to formation of pores. A model is proposed describing the mechanism that leads to the formation of the observed whiskers morphologies during the g à a-Al2O3transformation.


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.


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