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Cobalt Ferrite Nanoparticles: Preparation, characterization and salinized with 3-aminopropyl triethoxysilane
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Energy Procedia 157 Energy Procedia 00(2019) (2017)1353–1365 000–000
Procedia 00 (2018) 000–000 www.elsevier.com/locate/procedia Technologies and Materials forEnergy Renewable Energy, Environment and Sustainability, TMREES18, www.elsevier.com/locate/procedia 19–21 September 2018, Athens, Greece Technologies and Materials for Renewable Energy, Environment and Sustainability, TMREES18, 19–21 September 2018, Athens, Greece
Cobalt Ferrite Nanoparticles: Preparation, characterization and salinized with 3-aminopropyl triethoxysilane The 15thNanoparticles: International Symposium on District Heating and Cooling Cobalt Ferrite Preparation, characterization and Technologies and Materials for Renewable Energy, Environment and Sustainability, TMREES18, salinized 3-aminopropyl triethoxysilane a19–21 b September Athens, Greece Wajeeh Kachi , with Ahmed Majeed Al-Shammari , Israa G.Zainala,b,* Assessing the feasibility of 2018, using the heat demand-outdoor a b a,b,* Kachi ,Technical Ahmed Al-Shammari ,characterization Israa G.Zainal temperature function forUniversity-Iraq, aMajeed long-term district heat demand forecast CobaltWajeeh Ferrite Nanoparticles: Preparation, and Middle Medical Technical Institute - Mansour, a,b,c a a b triethoxysilane c c with 3-aminopropyl Middle Technical Technical - Mansour, , O. Le Corre I.(Experimental Andrićsalinized *, A. Pina ,Iraqi P. University-Iraq, Ferrão , J.Medical Fournier ., Institute B. Lacarrière Therapy department, Centre for Cancer and Medical Genetic Research, Mustansiriyah University) a
b
a
a
a,b (Kirkuk university, faculty of science, chemistry department) IN+ Center for Innovation, Technology a and Policy Research - Instituto Superior Técnico, b Av. Rovisco Pais 1, 1049-001 a,b,* Lisbon, Portugal b (Experimental Therapy department, Iraqi Centre for291 Cancer andDreyfous Medical Daniel, Genetic 78520 Research, Mustansiriyah University) b Veolia Recherche & Innovation, Avenue Limay, France a,b (Kirkuk university, faculty of science, chemistry department) c Département Systèmes Énergétiques et Environnement - IMT Atlantique, 4 rue Alfred Kastler, 44300 Nantes, France
Abstract
Wajeeh Kachi , Ahmed Majeed Al-Shammari , Israa G.Zainal a
Middle Technical University-Iraq, Medical Technical Institute - Mansour,
Abstract Coprecipitation method was used to prepare pure and doped CoFe2O4 nanoparticles. Ferric and cobalt salts were used as precursors Sodium Dodecylbenzene Sulfonate was usedandasMedical surfactant. of cobalt ferrite (Experimental Therapy department, Iraqi Centre for Cancer GeneticSurface Research,functionalization Mustansiriyah University) Abstract bwhile nanoparticles is a was kindused of functional which been widely used in Ferric the biotechnology and catalysis. Coprecipitation(NPs) method toa,b(Kirkuk preparematerials, pure andfaculty doped CoFe2O4 nanoparticles. and cobalt salts were usedThe as university, ofhave science, chemistry department) precursors while Sodium Dodecylbenzene Sulfonate was used as surfactant. Surface functionalization of cobalt ferrite fabricated cobalt ferrite nanoparticles were functionalized with amino propyl triethoxy silane (APTES) by silanization reaction District heating networks are commonly addressed in the literature as one of the most effective solutions for decreasing the nanoparticles (NPs) isand a kind ofthe functional which have require been used in the X-ray biotechnology andthrough catalysis. The and both non-coated organosilane-coated magnetite characterized bywidely energy-dispersive spectroscopy (EDX), X-ray greenhouse gas emissions from buildingmaterials, sector. These systems high investments which are returned the heat Abstract cobaltFourier diffractometry, transformed spectroscopy (FTIR), atomic force microscopy (AFM) emission fabricated ferrite nanoparticles were functionalized with renovation amino propyl triethoxy (APTES) byfuture silanization reaction sales. Due to the changed climateinfrared conditions and building policies, heatsilane demand inand thefiled could scanning decrease, and bothmicroscope non-coated and organosilane-coated characterized energy-dispersive spectroscopy (EDX), X-ray electron (FESEM). Basic groups ofmagnetite amino anchored on the by external surface of theX-ray coated magnetite were observed. prolonging the investment return period. Coprecipitation method was used to prepare pure and doped CoFe2O4 nanoparticles. Ferric and cobalt salts were scanning used as diffractometry, Fourier transformed infrared spectroscopy (FTIR), atomic force microscopy (AFM) and filed emission The nanoparticles above have surface with free NH2 groups which can transport ionic interface with carboxylic groups and act The main scope of this paper is to assess the feasibility of using the heat demand – outdoor temperature function for heat demand precursors while Sodium Dodecylbenzene Sulfonate was used as surfactant. Surface functionalization ofwere cobalt ferrite asforecast. a transporter of biological molecules, drugs, and metals. electron microscope (FESEM). Basic groups of amino anchored on the external surface of the coated magnetite observed. The district of Alvalade, located in Lisbon (Portugal), was used as a case study. The district is consisted of 665 nanoparticles (NPs) is a have kind surface of functional materials, which which have been widely used the biotechnology and groups catalysis. The The nanoparticles above with period free - NH2 groups can transport ionic in interface with carboxylic act Keywords: Coprecipitation; Silanization reaction . weather buildings thatNanoparticles; vary in bothAPTES; construction and typology. Three scenarios (low, medium, high) and threeand district fabricated cobaltofferrite nanoparticles were functionalized with amino propyl triethoxy silane (APTES) by silanization reaction asrenovation a transporter biological molecules, drugs, and metals. scenarios were developed (shallow, intermediate, deep). To estimate the error, obtained heat demand values were and both non-coated and organosilane-coated magnetite characterized by energy-dispersive X-ray spectroscopy (EDX), X-ray Keywords: Nanoparticles; Coprecipitation; reaction. developed compared with results from APTES; a dynamic heat demandSilanization model, previously and validated by the authors. © 2019 The Authors. Published by Elsevier diffractometry, Fourier transformed infraredLtd. spectroscopy (FTIR), atomic force microscopy (AFM) and filed emission scanning ©The 2018 The Authors. Published by Elsevier Ltd. results showed that when onlythe weather change is license considered, the margin of error could be acceptable for some applications This is an open access article under CC BY-NC-ND (https://creativecommons.org/licenses/by-nc-nd/4.0/) electron Basic of amino anchored on the external surface of the coated magnetite were observed. This anmicroscope open access(FESEM). article under thegroups CCthan BY-NC-ND license (https://creativecommons.org/licenses/by-nc-nd/4.0/) (theiserror in peer-review annual demand wasresponsibility lower 20% all weather scenarios considered). However, afterfor introducing Selection and under of theforscientific committee of Technologies and Materials Renewablerenovation Energy, The nanoparticles above have surface with free - NH2 groups which can transport ionic interface with carboxylic groups Energy, and act © 2018 The Authors. Published by Elsevier Ltd. Selection and peer-review under responsibility of the scientific committee of Technologies andscenarios Materials for Renewable scenarios, the error value increased up to 59.5% (depending on the weather and renovation combination considered). Environment and Sustainability, TMREES18. as a transporter ofSustainability, biological molecules, drugs, and metals. This is an open access article under the CC BY-NC-ND license (https://creativecommons.org/licenses/by-nc-nd/4.0/) Environment and TMREES18. The value of slope coefficient increased on average within the range of 3.8% up to 8% per decade, that corresponds to the Keywords: Nanoparticles; APTES; Coprecipitation; Silanization reaction . of Selection and peer-review responsibility of the scientific committee Technologies andonMaterials for Renewable Energy, decrease in the number ofunder heating hours of 22-139h during the heating season (depending the combination of weather and Keywords: Type your keywords here, separated by semicolons ; Environment and Sustainability, TMREES18. renovation scenarios considered). On the other hand, function intercept increased for 7.8-12.7% per decade (depending on the coupled scenarios). The values suggested could be used to modify the function parameters for the scenarios considered, and
© 2018 The Published byseparated Elsevier Keywords: Type your keywords byLtd. semicolons ; improve theAuthors. accuracy of heathere, demand estimations. Corresponding ; [email protected] This is an openauthor access article under the CC BY-NC-ND license (https://creativecommons.org/licenses/by-nc-nd/4.0/)
Selection and Authors. peer-review under responsibility of the scientific committee of Technologies and Materials for Renewable Energy, © 2017 The Published by Elsevier Ltd. Peer-review under responsibility of the Scientific Committee of The 15th International Symposium on District Heating and Cooling. 1876-6102 © 2018 The Authors. Published by Elsevier Ltd.
Corresponding author ; [email protected] Environment and Sustainability, TMREES18.
Keywords: Type your keywords here, separated by semicolons ; This is an open access article under the CC BY-NC-ND license (https://creativecommons.org/licenses/by-nc-nd/4.0/) Keywords: Heat demand;under Forecast; Climate change Selection peer-review of the scientific 1876-6102and © 2018 The Authors. responsibility Published by Elsevier Ltd. committee of Technologies and Materials for Renewable Energy, Environment and Sustainability, TMREES18. This is an open author access article under the CC BY-NC-ND license (https://creativecommons.org/licenses/by-nc-nd/4.0/) Corresponding ; [email protected] Selection and peer-review under responsibility of the scientific committee of Technologies and Materials for Renewable Energy, Environment and Sustainability, TMREES18.
1876-6102 © 2017 The Authors. Published by Elsevier Ltd. 1876-6102 © 2019 The Authors. Published by Elsevier Ltd. 1876-6102 © 2018 Authors. Published by Elsevier Ltd. of The 15th International Symposium on District Heating and Cooling. Peer-review underThe responsibility of the Scientific Committee This is an open access article under the CC BY-NC-ND license (https://creativecommons.org/licenses/by-nc-nd/4.0/) This is an open article under CC BY-NC-ND (https://creativecommons.org/licenses/by-nc-nd/4.0/) Selection and access peer-review underthe responsibility of license the scientific committee of Technologies and Materials for Renewable Energy, Selection and peer-review under responsibility of the scientific committee of Technologies and Materials for Renewable Energy, Environment Environment and Sustainability, TMREES18. and Sustainability, TMREES18. 10.1016/j.egypro.2018.11.300
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Wajeeh Kachi et al. / Energy Procedia 157 (2019) 1353–1365 Author name / Energy Procedia 00 (2018) 000–000
1. Introduction Amongst magnetic ferrites with the general formula AFe2O4 (A – transition metal), cobalt ferrites have a myriad of applications in the fields of electronics [1], medical therapeutics diagnostics, magnetic devices and magnetic drug carriers[2,3]. Also, Magnetic iron oxide nanoparticles have been extensively investigated for their various biomedical applications [4]. The number of biomedical applications using magnetic iron oxide nanoparticles has been increasing exponentially over the past few years[5]. A few examples are: magnetic biosensor systems[6], local heat sources for cancer treatment by hyperthermia[7], separation immunoassays[8], drug carriers[9],contrast agents for magnetic resonance imaging (MRI)[10] and magnetic particle imaging (MPI)[11], parasite diagnostic assays[11], and nanobridge substances for surgery and wound healing[12].A number of different synthesis methods have been proposed for preparing CoFe2O4, including: ceramic [13], co-precipitation [14], hydrothermal[15], thermal decomposition [16], sol-gel[17] and combustion methods [18].Generally, in most types of nanoparticles prepared by these methods, control of size and size distribution is not possible[19]. The prepared nanoparticles were functionalized for various applications, including drug delivery [22], magnetic resonance imaging (MRI) [23]&[24], bioseparation of proteins, DNA and cells [25],[26]&[27], catalysis[28]&[29], Ferrofluids [30], data storage [31], and adsorption [32]. The modified magnetic materials are composed of a cobalt- iron oxide core coated with organic or inorganic molecules, which form a chemical bond with the core surface. The cobalt iron oxide core is obtained as a fine powder containing nanometer-sized particles. Functional groups tailored for specific tasks are anchored as an organic molecule shell around of the core.[33] The surface of nanoparticles was modified with 3aminopropyltriethoxysilane (APTES) to introduce reactive amine groups on the surface of nanoparticles.[34]. Functionalization of magnetic nanoparticles is a key factor for efficient capture of the target.[35]. The integration of biomolecules with metallic nanoparticles produces new hybrid nanostructures of exceptional structures that combine the properties of the biomolecules and the nano-elements. These exceptional structures of the hybrid biomolecule/nanoparticle systems offer the basis for the rapid development of the area of nanobiotechnology [36]. Moreover, the silane agent is often considered as a candidate for modifying on the surface of iron oxide NPs directly, for the advantages of the biocompatibility as well as high density of surface functional end groups and allowing for connecting to other metal, polymer or biomolecules.[37]&[38]. In general, silane-coated iron oxide NPs still maintains the physical characteristics of naked NPs, the 3-aminopropyltriethyloxysilane (APTES) agent were mostly employed for providing the amino group. The physicochemical mechanism of the silane agent modifying on the surface of iron oxide NPs according to Arkles method [39]. The chemical group (hydroxyl groups) on the iron oxide NPs surface reacted with the methoxy groups of the silane molecules resulting in the formation of Si–O bonds and feat the terminal functional groups accessible for immobilization the other substance. This study aimed at preparation of CoFe2O4 nanoparticles then modified with APTES. The morphology/size and magnetization were determined for these nanoparticles using energy-dispersive X-ray spectroscopy (EDX), X-ray diffractometry, Fourier transformed infrared spectroscopy (FTIR), atomic force microscopy (AFM) and field emission scanning electron microscope (FESEM). 2. Materials & Methods FeCl3.6H2O, CoCl2.4H2O, NaOH, APTES (3-aminopropyl-triethoxysilane), and Sodium dodecyl benzene sulfonate (SDBS) were purchased from (Sigma-Aldrich) Company. The chemicals were used as is without additional purifications. All the glassware (glass bottle and small pieces of glass substrate) was cleaned and sonicated in ethanol for 5 minutes, rinsed with double distilled water, soaked in H2O/HNO3 (65%)/H2O2 (1:1:1, v/v/v) solution, rinsed again with doubly distilled water(DDW), and finally dried in air[40]. 2.1. Preparations of CoFe2O4 nanoparticles Magnetite particles were prepared by the coprecipitation method. By adding a (0.5) ml of (0.1M) SDBS solution (as surfactant,) into a mixed solution of (25) ml of (0.4M) FeCl3.6H2O and (25)ml of (0.2M) CoCl2.6H2O in deionized water. Slowly add 1M of NaOH solution to the salt solution dropwise, and the reactants were constantly stirred using a mechanical stirrer until obtaining pH between (11-12), the reactants were sonicated for 15min and
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then the liquid precipitate was brought to a reaction temperature of 80°C and stirred for one hour. The above steps can be regarded as ferritisation step. The product was cooled to R.T and the precipitate was washed twice with D.W and then with ethanol. The precipitate was then derided overnight at 100°C. The acquired substance was then grinded into a fine powder. At this stage, the product (CoFe2O4) contains some associated water which was then removed by heating to 600oC for 3 hours. 2.2. Cobalt Ferrite (CoFe2O4) Nanoparticles Purification Depending on magnetic properties of CoFe2O4 NPs, these NPs can purify by adding 3 volumes from deionized water to one weight of CoFe2O4 NPs. The mixture was dispersed by bath sonication for 15 min at RT. The suspended NPs were separated magnetically, and the settled product was re-dispersed by deionized water and sonication, then isolated with magnetic decantation for 3 times as cleared in figure (1):
Fig.1.: attracting magnetite nanoparticles by a Magnet.
The precipitated product CoFe2O4 NPs was dried at RT. 2.3. Salinization of CoFe2O4 nanoparticles with 3-aminopropyl triethoxysilane. The CoFe2O4 nanoparticles powder (1 g) was dispersed by 150 mL ethanol/water (volume ratio, 1:1) solution using probe sonication for 30 min, then 6 mL of (99%) (3-aminopropyl) triethoxysilane (APTES) H2N(CH2)3Si(OCH3)3] ) were added to the mixture. The resulting mixture was stirred under mechanical stirring at 40 ºC for 8 hours. The final product was separated from the solution and washed for 5 times by water, acetone and ethanol. The precipitated product (APTES– CoFe2O4) was isolated and purified with magnetic decantation and dried to RT under vacuum. 2.4. Characterization The crystalline phases, chemical composition and morphology of the nanoparticle's before and after the silanization were identified by means by using: energy dispersive X-ray spectroscopy SEM-EDX(Quanta 200 FEG) in order to investigate the morphology and elemental composition of CoFe2O4 nanoparticles, AFM Veeco-dilnnova (Veeco Inc., USA) and field emission scanning electron microscopy (FESEM), Powder X-ray diffraction (XRD) patterns of CoFe2O4 nanoparticles were recorded with a Shimadzu XRD-6000 instrument (Shimadzu Corporation, Kyoto, Japan) in the range of 20°–80° using CuKα as a radiation source (λ = 1.5418 Å) generated at 40 kV and 30 mA. Fourier transform infrared (FTIR) spectra of CoFe2O4 nanoparticle powder were recorded over the range of 400–4000 cm−1 on a Thermo Nicolet Nexus, Smart Orbit spectrometer using a sample of approximately 1% in 200 mg of spectroscopic-grade potassium bromide (KBr) with 10 tons of pressure. 3. Results
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Preparing of CoFe2O4 nanoparticles was carried out by the co-precipitation method in an aqueous medium, through reaction in section (2.2).So the reaction was carried out as in the equations below: 2Fe3+ + Co2+
Fe2Co (OH) 8
…….
(1)
Fe2Co (OH) 8
CoFe2O4 + 4H2O
…….
(2)
Cobalt iron oxide nanoparticles surface modified by the process Silanization. This reaction involves the covering of a surface cobalt iron oxide nanoparticles through self-assembly with (3-aminopropyl)- tri ethoxy silane molecules. During this reaction ,hydroxyl groups on the surface of iron oxide nanoparticles attack and replace ethoxy groups of APTES ,thus is formed a covalent -Si-O-Si- bond and amino propyl-terminated surface. The surface coating of nanoparticles by APTES depends on experimental parameters like silane concentration, temperature and reaction time. 3.1. Characterization of the samples 3.1.1. E – DX analysis The elemental composition of the CoFe2O4 and APTES– CoFe2O4 nanoparticles were estimated by using an EDX detector and the results were shown in Fig.2 (a&b).
Fig,2.: Elemental analysis of NPs by energy dispersive X-ray (EDX) analysis. CoFe2O4 nanoparticles(a), APTES – CoFe2O4 nanoparticles(b).
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This figure indicates that the CoFe2O4 nanoparticles contained 14.30 % of Co, 51.70 % of Fe and 34.01 % of O2, while the APTES– CoFe2O4 nanoparticles contained 8.41 % of Co, 29.62 % of Fe, 5.78 % of O2, 0.02 % of Si, 15.58 % of N2 and 40.59 % of C, the presence Silicon, nitrogen and carbon indicated the successful conjugation of APTES with CoFe2O4 nanoparticles. 3.1.2.X-RD analysis Phase investigation of the crystallized product was performed by XRD analysis for the CoFe2O4 NPs and APTES coated nanoparticles as presented in Figure 3(a&b):
Fig.3.: X-ray powder diffraction patterns.(a) CoFe2O4 nanoparticles, (b) APTES – CoFe2O4 nanoparticles.
All of the observed diffraction peaks were indexed by the cubic structure of CoFe2O4 according to crystallographic standard (JCPDS 22-1086).The peaks appear with high intensity and a high basal width of all reflections observed which indicating that the samples were crystalline and formed nanoparticles. Figure 3 also cleared that after silanization of nanoparticles with silane agent (3-minopropyltrimethoxysilane) there were reduction in crystallinity and increase in crystallite size. The particle size was calculated by using Debye–Scherrer’s equation: � � � ����⁄������
(3)
Where D is the crystalline size, λ is the incident X-ray wavelength, β is the full width at half-maximum, and θ is the diffraction angle. Since the value of the crystalline size was next, ranging from 21.86 to 26.70 nm, with a maximum difference in size of 4.48nm. This indicated good uniformity of sample. It can be observed that the reduction in the amount of crystallinity for the silanized cobalt ferrite nanoparticles was attributed to the presence of silane incorporated with the cobalt ferrite, thus indicating that the silane was effective and that the ferrite structure is preserved. The average crystalline size showed that the values were different for both ferrites and the observation of increase after Silanization. 3.1.3.FESEM analysis The surface morphology of naked CoFe2O4 and APTES-CoFe2O4 nanoparticles was observed by scanning electron microscopy, Figure 4(A & B).
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(A)
(B)
Fig,4. Field emission scanning electron microscopy images of (A) CoFe2O4 NPs., (B) APTES –CoFe2O4 NPs.
The FESEM images of the prepared nanoparticles respectively were showed the formation of nanoparticles is nearly uniform and spherical shape. In the other words, during the silanization reaction, morphological properties of nanoparticles do not noticeably change. 3.1.4.AFM images Figure 5 represented the AFM images and the size distribution histogram which presented the films of naked cobalt ferrite NPs and APTES- cobalt ferrite nanoparticles which obtained by depositing a micro volume of the colloidal solution onto high-grade mica and allowing too dry at RT in a clean laminar flow chamber, Particles with an approximate spherical shape and an average diameter of 22.42 nm in the absence of APTES (left) & 28.06 nm in the presence of APTES (right) were observed. This may be considered as indirect evidence that difference of 5.64 nm corresponds to the APTES-coating.
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Fig,5.: AFM images of cobalt Ferrite NPs without (left) and with (right) APTES & size distribution histogram obtained from the AFM images.
3.1.5.FTIR analysis
The surface nature of samples was qualitatively assessed before and after silanization step
by using FTIR spectroscopy. Figure 6 (A&B). (A)
8
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(B)
3.
Fig.6.: FT-IR spectra of: (A) the naked CoFe2O4, (B) APTES- CoFe2O4
Figure 6(A&B)shown that the vibration spectrum of the infrared region, in the range 4000-400cm-1 using KBr pellet method for the prepared CoFe2O4 and silanized CoFe2O4 .The modification of basic functional group such as amino groups is important because these groups can be used to bind various biomolecules, drugs and metals by covalent bond or chemical interaction. FTIR spectra indicated the existence of these functional groups on MNP, respectively. For the amino groups on the MNP, the presence of N–H (1,533.45 cm-1), C–H (2,930.43 cm-1) and O– H (3,433.43 cm-1) bonding as chemical bonds on the surface of the MNPs was confirmed, as cleared in figure 6(B). The spectra shown two absorption bands below 1000 cm-1,the sharp which revealed peak around (572-435) cm1can be observed in (A) and (B) spectra which is relates to the absorption peak of (Fe- O) bond of nanoparticles. Figure 6(A) showed that there was band also observed in the range of about (3550) cm-1 which characteristic of the (O-H-O) bonds, from the presence of water in the sample, which may be derived from surface adsorption of atmospheric air and due to the use of KBr in the prepared samples. The presence of APTES on the surface of cobalt ferrite nanoparticles is proven by the bands at 1100 and 905 cm1 that dedicated to the Si –O stretching vibrations of APTES on the surface of magnetic NPs, and the broad band at 3433cm-1 and absorption peak at 1533.45cm-1 are attributed to stretching of the N-H (group NH2) and C=O amide groups, respectively Figure 7(B). The presence of the propyl group of APTES was confirmed by C–H stretching vibrations that appeared at 2922 cm-1. 4. Discussion. Cobalt-ferrite nanoparticles were synthesized by coprecipitating Co (II) and metal (Fe III) in alkaline medium. The pure and doped cobalt ferrite nanoparticles were synthesized by coprecipitation method. Due to low cost the coprecipitation method is widely used for the preparation of the nanoparticles for the industry use. The aqueous solution of divalent metal cations (Co2+ and Fe3+) results in precipitation of ferrite nanoparticles. Initially in coprecipitation method, the formation of metal hydroxides occurs in form of colloidal particles in alkaline medium (NaOH), through reaction [1].The next step can be regarded as ferritization. In this step the colloidal solution is heated up to 80oC and the solid solution of metal hydroxides converts into the required ferrite, through reaction [2]. The third step of coprecipitation method is called annealing, in which water from the product is removed through heating. The product contains a small amount of water (10%). This water in product cannot be removed during reaction. To remove this water from the product, it is then annealed at 600 °C Some parameters can affect the size and size distribution of nanoparticles prepared by coprecipitation method.
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In coprecipitation method two processes are important, namely nucleation and growth of the nuclei (center of crystallization). The rate of mixing of reactants is extremely important. Uniform and small particles are formed when the nucleation rate is faster than growth rate. The condition for the synthesis of uniform and small particles can be obtained by quick addition and fast stirring of reagents [41]. Increase in temperature in the range from (20 to 100) °C, is directly related to the rate of formation of ferrite. Different ferrites are formed at different activation energies. The yield of ferrite tends to grow when pH of the reaction becomes within the range from (7 to 10). The yield grows drastically when pH of the reaction reaches 12.5. Variation of pH of the reaction also affects the particle size [42]. Thus, the size variation and control has been achieved by both the rate of reaction and the annealing conditions. This work also includes coated the prepared cobalt ferrite NPs with APTES by development of a physical mixing procedure using a temperature without any initiator. This approach was more convenient, cheaper and less time consuming. Apart from this, using APTES as ligand and it was introduced to cobalt ferrite nanoparticles. The APTES has silane and amino terminals, the silane end covalently attached with nanoparticle surface and the amino ends are freely exposed [43].The process of surface modification by silanization reaction is very complex. Several parameters such as reaction time, temperature and silane concentration influence the reactivity of the silane molecule to the inorganic surface. The reaction between an alkoxy silane and a solid material does not involve a single mechanism, and many different intermediates are possible [44]. The silanization reaction occurs with two steps: First, the organo silane is placed into an aqueous solution of an acid that acts as a catalyst. It is hydrolyzed, and a condensation reaction occurs to form a silane polymer [45]. The following equation represents the simplified reaction of hydrolysis and condensation with production of silane polymer, as in the equation below:
The above equation cleared that alkoxide groups (-OC2H5) are replaced by hydroxyl groups (OH) to form reactive silanol groups, which condense with other silanol groups to produce siloxane bonds (Si–O–Si). Alcohol (C2H5OH) and water are produced as by-products of condensation [46]. In the second step, the polymer associates with the NPs forming a covalent bond with OH groups. Dehydration as well as adsorption of silane polymers to the metal oxide occurs [47], as in the equation below :
The cobalt ferrite nanoparticles core was using as template and it showed very high affinity towards the hybrid network. After that, the surface was modified with aminopropyl triethoxy silane (APTES). The ligands offered free amino functional group for binding. The below scheme clears the preparation steps for fabricating APTES-functionalized magnetic CoFe2O4 NPs:
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Schematic image of preparations of the APTES-CoFe3O4 nanoparticles The EDX analysis, figure (2) cleared the elemental composition which also revealed that the APTES molecules were successfully coated with nanoparticles, since the presence Silicon, nitrogen and carbon in the modification NPs and absent in necked NPs indicated the successful conjugation of APTES with CoFe2O4 nanoparticles, also, figure (3) cleared the variation between the values of the crystalline size, this difference may be attributed to the presence of the silane. The increase in crystalline size is due to the presence of silane agent which decreases the base width of reflections. However, since this reduction was slightly found that the presence of silane agent did not alter the structure of ferrite. Figures (4&5) showed the formation of nanoparticles is nearly uniform and spherical shape. In other words, during the silanization reaction morphological properties of nanoparticles do not noticeably change. Also, the figures showed the increase in the size between necked and modified NPs in AFM and FESEM images. In addition to the successful APTES coating onto nanoparticles, the surface nature of synthesized nanoparticles was qualitatively assessed by using FTIR spectroscopy. The FTIR spectra showed stretch the N-H (group NH2) and C=O amide groups, and the presence of the propyl group of APTES was confirmed by C–H stretching vibrations that appeared clearly indicated that the APTES was successfully coated to nanoparticles. Conclusions In conclusions this paper presented the preparation of CoFe2O4 nanoparticles with the range between (22-28) nm. The size of the nanoparticles was measured both by XRD and AFM and were in a good agreement with each other indicating that there was no agglomeration and the size distribution of the prepared nanoparticles was small. Also, the data indicated easy and effective method for the preparation of a modified cobalt ferrite nanoparticles with APTES to bind organo silane to a metal oxide nanoparticle by adsorption or covalent bonding, and the active amino group in its structure can combine with biomolecules, drugs and metals. The results showed that the heating of magnetite nanoparticles during the silanization reaction did not affect particle size; these were roughly spherical in shape and were around 28 nm in diameter. This value is very close to the size of magnetite crystalline, suggesting the formation of a continuous and very fine layer of silane on the surface of the magnetite core. So, finally the results in this study cleared the fact that the final product exhibited basic groups of amino and hydroxyl anchored on the external surface which can be used in many technological applications especially in various bio processes.
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Procedia 00 (2018) 000–000 www.elsevier.com/locate/procedia Technologies and Materials forEnergy Renewable Energy, Environment and Sustainability, TMREES18, www.elsevier.com/locate/procedia 19–21 September 2018, Athens, Greece Technologies and Materials for Renewable Energy, Environment and Sustainability, TMREES18, 19–21 September 2018, Athens, Greece
Cobalt Ferrite Nanoparticles: Preparation, characterization and salinized with 3-aminopropyl triethoxysilane The 15thNanoparticles: International Symposium on District Heating and Cooling Cobalt Ferrite Preparation, characterization and Technologies and Materials for Renewable Energy, Environment and Sustainability, TMREES18, salinized 3-aminopropyl triethoxysilane a19–21 b September Athens, Greece Wajeeh Kachi , with Ahmed Majeed Al-Shammari , Israa G.Zainala,b,* Assessing the feasibility of 2018, using the heat demand-outdoor a b a,b,* Kachi ,Technical Ahmed Al-Shammari ,characterization Israa G.Zainal temperature function forUniversity-Iraq, aMajeed long-term district heat demand forecast CobaltWajeeh Ferrite Nanoparticles: Preparation, and Middle Medical Technical Institute - Mansour, a,b,c a a b triethoxysilane c c with 3-aminopropyl Middle Technical Technical - Mansour, , O. Le Corre I.(Experimental Andrićsalinized *, A. Pina ,Iraqi P. University-Iraq, Ferrão , J.Medical Fournier ., Institute B. Lacarrière Therapy department, Centre for Cancer and Medical Genetic Research, Mustansiriyah University) a
b
a
a
a,b (Kirkuk university, faculty of science, chemistry department) IN+ Center for Innovation, Technology a and Policy Research - Instituto Superior Técnico, b Av. Rovisco Pais 1, 1049-001 a,b,* Lisbon, Portugal b (Experimental Therapy department, Iraqi Centre for291 Cancer andDreyfous Medical Daniel, Genetic 78520 Research, Mustansiriyah University) b Veolia Recherche & Innovation, Avenue Limay, France a,b (Kirkuk university, faculty of science, chemistry department) c Département Systèmes Énergétiques et Environnement - IMT Atlantique, 4 rue Alfred Kastler, 44300 Nantes, France
Abstract
Wajeeh Kachi , Ahmed Majeed Al-Shammari , Israa G.Zainal a
Middle Technical University-Iraq, Medical Technical Institute - Mansour,
Abstract Coprecipitation method was used to prepare pure and doped CoFe2O4 nanoparticles. Ferric and cobalt salts were used as precursors Sodium Dodecylbenzene Sulfonate was usedandasMedical surfactant. of cobalt ferrite (Experimental Therapy department, Iraqi Centre for Cancer GeneticSurface Research,functionalization Mustansiriyah University) Abstract bwhile nanoparticles is a was kindused of functional which been widely used in Ferric the biotechnology and catalysis. Coprecipitation(NPs) method toa,b(Kirkuk preparematerials, pure andfaculty doped CoFe2O4 nanoparticles. and cobalt salts were usedThe as university, ofhave science, chemistry department) precursors while Sodium Dodecylbenzene Sulfonate was used as surfactant. Surface functionalization of cobalt ferrite fabricated cobalt ferrite nanoparticles were functionalized with amino propyl triethoxy silane (APTES) by silanization reaction District heating networks are commonly addressed in the literature as one of the most effective solutions for decreasing the nanoparticles (NPs) isand a kind ofthe functional which have require been used in the X-ray biotechnology andthrough catalysis. The and both non-coated organosilane-coated magnetite characterized bywidely energy-dispersive spectroscopy (EDX), X-ray greenhouse gas emissions from buildingmaterials, sector. These systems high investments which are returned the heat Abstract cobaltFourier diffractometry, transformed spectroscopy (FTIR), atomic force microscopy (AFM) emission fabricated ferrite nanoparticles were functionalized with renovation amino propyl triethoxy (APTES) byfuture silanization reaction sales. Due to the changed climateinfrared conditions and building policies, heatsilane demand inand thefiled could scanning decrease, and bothmicroscope non-coated and organosilane-coated characterized energy-dispersive spectroscopy (EDX), X-ray electron (FESEM). Basic groups ofmagnetite amino anchored on the by external surface of theX-ray coated magnetite were observed. prolonging the investment return period. Coprecipitation method was used to prepare pure and doped CoFe2O4 nanoparticles. Ferric and cobalt salts were scanning used as diffractometry, Fourier transformed infrared spectroscopy (FTIR), atomic force microscopy (AFM) and filed emission The nanoparticles above have surface with free NH2 groups which can transport ionic interface with carboxylic groups and act The main scope of this paper is to assess the feasibility of using the heat demand – outdoor temperature function for heat demand precursors while Sodium Dodecylbenzene Sulfonate was used as surfactant. Surface functionalization ofwere cobalt ferrite asforecast. a transporter of biological molecules, drugs, and metals. electron microscope (FESEM). Basic groups of amino anchored on the external surface of the coated magnetite observed. The district of Alvalade, located in Lisbon (Portugal), was used as a case study. The district is consisted of 665 nanoparticles (NPs) is a have kind surface of functional materials, which which have been widely used the biotechnology and groups catalysis. The The nanoparticles above with period free - NH2 groups can transport ionic in interface with carboxylic act Keywords: Coprecipitation; Silanization reaction . weather buildings thatNanoparticles; vary in bothAPTES; construction and typology. Three scenarios (low, medium, high) and threeand district fabricated cobaltofferrite nanoparticles were functionalized with amino propyl triethoxy silane (APTES) by silanization reaction asrenovation a transporter biological molecules, drugs, and metals. scenarios were developed (shallow, intermediate, deep). To estimate the error, obtained heat demand values were and both non-coated and organosilane-coated magnetite characterized by energy-dispersive X-ray spectroscopy (EDX), X-ray Keywords: Nanoparticles; Coprecipitation; reaction. developed compared with results from APTES; a dynamic heat demandSilanization model, previously and validated by the authors. © 2019 The Authors. Published by Elsevier diffractometry, Fourier transformed infraredLtd. spectroscopy (FTIR), atomic force microscopy (AFM) and filed emission scanning ©The 2018 The Authors. Published by Elsevier Ltd. results showed that when onlythe weather change is license considered, the margin of error could be acceptable for some applications This is an open access article under CC BY-NC-ND (https://creativecommons.org/licenses/by-nc-nd/4.0/) electron Basic of amino anchored on the external surface of the coated magnetite were observed. This anmicroscope open access(FESEM). article under thegroups CCthan BY-NC-ND license (https://creativecommons.org/licenses/by-nc-nd/4.0/) (theiserror in peer-review annual demand wasresponsibility lower 20% all weather scenarios considered). However, afterfor introducing Selection and under of theforscientific committee of Technologies and Materials Renewablerenovation Energy, The nanoparticles above have surface with free - NH2 groups which can transport ionic interface with carboxylic groups Energy, and act © 2018 The Authors. Published by Elsevier Ltd. Selection and peer-review under responsibility of the scientific committee of Technologies andscenarios Materials for Renewable scenarios, the error value increased up to 59.5% (depending on the weather and renovation combination considered). Environment and Sustainability, TMREES18. as a transporter ofSustainability, biological molecules, drugs, and metals. This is an open access article under the CC BY-NC-ND license (https://creativecommons.org/licenses/by-nc-nd/4.0/) Environment and TMREES18. The value of slope coefficient increased on average within the range of 3.8% up to 8% per decade, that corresponds to the Keywords: Nanoparticles; APTES; Coprecipitation; Silanization reaction . of Selection and peer-review responsibility of the scientific committee Technologies andonMaterials for Renewable Energy, decrease in the number ofunder heating hours of 22-139h during the heating season (depending the combination of weather and Keywords: Type your keywords here, separated by semicolons ; Environment and Sustainability, TMREES18. renovation scenarios considered). On the other hand, function intercept increased for 7.8-12.7% per decade (depending on the coupled scenarios). The values suggested could be used to modify the function parameters for the scenarios considered, and
© 2018 The Published byseparated Elsevier Keywords: Type your keywords byLtd. semicolons ; improve theAuthors. accuracy of heathere, demand estimations. Corresponding ; [email protected] This is an openauthor access article under the CC BY-NC-ND license (https://creativecommons.org/licenses/by-nc-nd/4.0/)
Selection and Authors. peer-review under responsibility of the scientific committee of Technologies and Materials for Renewable Energy, © 2017 The Published by Elsevier Ltd. Peer-review under responsibility of the Scientific Committee of The 15th International Symposium on District Heating and Cooling. 1876-6102 © 2018 The Authors. Published by Elsevier Ltd.
Corresponding author ; [email protected] Environment and Sustainability, TMREES18.
Keywords: Type your keywords here, separated by semicolons ; This is an open access article under the CC BY-NC-ND license (https://creativecommons.org/licenses/by-nc-nd/4.0/) Keywords: Heat demand;under Forecast; Climate change Selection peer-review of the scientific 1876-6102and © 2018 The Authors. responsibility Published by Elsevier Ltd. committee of Technologies and Materials for Renewable Energy, Environment and Sustainability, TMREES18. This is an open author access article under the CC BY-NC-ND license (https://creativecommons.org/licenses/by-nc-nd/4.0/) Corresponding ; [email protected] Selection and peer-review under responsibility of the scientific committee of Technologies and Materials for Renewable Energy, Environment and Sustainability, TMREES18.
1876-6102 © 2017 The Authors. Published by Elsevier Ltd. 1876-6102 © 2019 The Authors. Published by Elsevier Ltd. 1876-6102 © 2018 Authors. Published by Elsevier Ltd. of The 15th International Symposium on District Heating and Cooling. Peer-review underThe responsibility of the Scientific Committee This is an open access article under the CC BY-NC-ND license (https://creativecommons.org/licenses/by-nc-nd/4.0/) This is an open article under CC BY-NC-ND (https://creativecommons.org/licenses/by-nc-nd/4.0/) Selection and access peer-review underthe responsibility of license the scientific committee of Technologies and Materials for Renewable Energy, Selection and peer-review under responsibility of the scientific committee of Technologies and Materials for Renewable Energy, Environment Environment and Sustainability, TMREES18. and Sustainability, TMREES18. 10.1016/j.egypro.2018.11.300
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Wajeeh Kachi et al. / Energy Procedia 157 (2019) 1353–1365 Author name / Energy Procedia 00 (2018) 000–000
1. Introduction Amongst magnetic ferrites with the general formula AFe2O4 (A – transition metal), cobalt ferrites have a myriad of applications in the fields of electronics [1], medical therapeutics diagnostics, magnetic devices and magnetic drug carriers[2,3]. Also, Magnetic iron oxide nanoparticles have been extensively investigated for their various biomedical applications [4]. The number of biomedical applications using magnetic iron oxide nanoparticles has been increasing exponentially over the past few years[5]. A few examples are: magnetic biosensor systems[6], local heat sources for cancer treatment by hyperthermia[7], separation immunoassays[8], drug carriers[9],contrast agents for magnetic resonance imaging (MRI)[10] and magnetic particle imaging (MPI)[11], parasite diagnostic assays[11], and nanobridge substances for surgery and wound healing[12].A number of different synthesis methods have been proposed for preparing CoFe2O4, including: ceramic [13], co-precipitation [14], hydrothermal[15], thermal decomposition [16], sol-gel[17] and combustion methods [18].Generally, in most types of nanoparticles prepared by these methods, control of size and size distribution is not possible[19]. The prepared nanoparticles were functionalized for various applications, including drug delivery [22], magnetic resonance imaging (MRI) [23]&[24], bioseparation of proteins, DNA and cells [25],[26]&[27], catalysis[28]&[29], Ferrofluids [30], data storage [31], and adsorption [32]. The modified magnetic materials are composed of a cobalt- iron oxide core coated with organic or inorganic molecules, which form a chemical bond with the core surface. The cobalt iron oxide core is obtained as a fine powder containing nanometer-sized particles. Functional groups tailored for specific tasks are anchored as an organic molecule shell around of the core.[33] The surface of nanoparticles was modified with 3aminopropyltriethoxysilane (APTES) to introduce reactive amine groups on the surface of nanoparticles.[34]. Functionalization of magnetic nanoparticles is a key factor for efficient capture of the target.[35]. The integration of biomolecules with metallic nanoparticles produces new hybrid nanostructures of exceptional structures that combine the properties of the biomolecules and the nano-elements. These exceptional structures of the hybrid biomolecule/nanoparticle systems offer the basis for the rapid development of the area of nanobiotechnology [36]. Moreover, the silane agent is often considered as a candidate for modifying on the surface of iron oxide NPs directly, for the advantages of the biocompatibility as well as high density of surface functional end groups and allowing for connecting to other metal, polymer or biomolecules.[37]&[38]. In general, silane-coated iron oxide NPs still maintains the physical characteristics of naked NPs, the 3-aminopropyltriethyloxysilane (APTES) agent were mostly employed for providing the amino group. The physicochemical mechanism of the silane agent modifying on the surface of iron oxide NPs according to Arkles method [39]. The chemical group (hydroxyl groups) on the iron oxide NPs surface reacted with the methoxy groups of the silane molecules resulting in the formation of Si–O bonds and feat the terminal functional groups accessible for immobilization the other substance. This study aimed at preparation of CoFe2O4 nanoparticles then modified with APTES. The morphology/size and magnetization were determined for these nanoparticles using energy-dispersive X-ray spectroscopy (EDX), X-ray diffractometry, Fourier transformed infrared spectroscopy (FTIR), atomic force microscopy (AFM) and field emission scanning electron microscope (FESEM). 2. Materials & Methods FeCl3.6H2O, CoCl2.4H2O, NaOH, APTES (3-aminopropyl-triethoxysilane), and Sodium dodecyl benzene sulfonate (SDBS) were purchased from (Sigma-Aldrich) Company. The chemicals were used as is without additional purifications. All the glassware (glass bottle and small pieces of glass substrate) was cleaned and sonicated in ethanol for 5 minutes, rinsed with double distilled water, soaked in H2O/HNO3 (65%)/H2O2 (1:1:1, v/v/v) solution, rinsed again with doubly distilled water(DDW), and finally dried in air[40]. 2.1. Preparations of CoFe2O4 nanoparticles Magnetite particles were prepared by the coprecipitation method. By adding a (0.5) ml of (0.1M) SDBS solution (as surfactant,) into a mixed solution of (25) ml of (0.4M) FeCl3.6H2O and (25)ml of (0.2M) CoCl2.6H2O in deionized water. Slowly add 1M of NaOH solution to the salt solution dropwise, and the reactants were constantly stirred using a mechanical stirrer until obtaining pH between (11-12), the reactants were sonicated for 15min and
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then the liquid precipitate was brought to a reaction temperature of 80°C and stirred for one hour. The above steps can be regarded as ferritisation step. The product was cooled to R.T and the precipitate was washed twice with D.W and then with ethanol. The precipitate was then derided overnight at 100°C. The acquired substance was then grinded into a fine powder. At this stage, the product (CoFe2O4) contains some associated water which was then removed by heating to 600oC for 3 hours. 2.2. Cobalt Ferrite (CoFe2O4) Nanoparticles Purification Depending on magnetic properties of CoFe2O4 NPs, these NPs can purify by adding 3 volumes from deionized water to one weight of CoFe2O4 NPs. The mixture was dispersed by bath sonication for 15 min at RT. The suspended NPs were separated magnetically, and the settled product was re-dispersed by deionized water and sonication, then isolated with magnetic decantation for 3 times as cleared in figure (1):
Fig.1.: attracting magnetite nanoparticles by a Magnet.
The precipitated product CoFe2O4 NPs was dried at RT. 2.3. Salinization of CoFe2O4 nanoparticles with 3-aminopropyl triethoxysilane. The CoFe2O4 nanoparticles powder (1 g) was dispersed by 150 mL ethanol/water (volume ratio, 1:1) solution using probe sonication for 30 min, then 6 mL of (99%) (3-aminopropyl) triethoxysilane (APTES) H2N(CH2)3Si(OCH3)3] ) were added to the mixture. The resulting mixture was stirred under mechanical stirring at 40 ºC for 8 hours. The final product was separated from the solution and washed for 5 times by water, acetone and ethanol. The precipitated product (APTES– CoFe2O4) was isolated and purified with magnetic decantation and dried to RT under vacuum. 2.4. Characterization The crystalline phases, chemical composition and morphology of the nanoparticle's before and after the silanization were identified by means by using: energy dispersive X-ray spectroscopy SEM-EDX(Quanta 200 FEG) in order to investigate the morphology and elemental composition of CoFe2O4 nanoparticles, AFM Veeco-dilnnova (Veeco Inc., USA) and field emission scanning electron microscopy (FESEM), Powder X-ray diffraction (XRD) patterns of CoFe2O4 nanoparticles were recorded with a Shimadzu XRD-6000 instrument (Shimadzu Corporation, Kyoto, Japan) in the range of 20°–80° using CuKα as a radiation source (λ = 1.5418 Å) generated at 40 kV and 30 mA. Fourier transform infrared (FTIR) spectra of CoFe2O4 nanoparticle powder were recorded over the range of 400–4000 cm−1 on a Thermo Nicolet Nexus, Smart Orbit spectrometer using a sample of approximately 1% in 200 mg of spectroscopic-grade potassium bromide (KBr) with 10 tons of pressure. 3. Results
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Preparing of CoFe2O4 nanoparticles was carried out by the co-precipitation method in an aqueous medium, through reaction in section (2.2).So the reaction was carried out as in the equations below: 2Fe3+ + Co2+
Fe2Co (OH) 8
…….
(1)
Fe2Co (OH) 8
CoFe2O4 + 4H2O
…….
(2)
Cobalt iron oxide nanoparticles surface modified by the process Silanization. This reaction involves the covering of a surface cobalt iron oxide nanoparticles through self-assembly with (3-aminopropyl)- tri ethoxy silane molecules. During this reaction ,hydroxyl groups on the surface of iron oxide nanoparticles attack and replace ethoxy groups of APTES ,thus is formed a covalent -Si-O-Si- bond and amino propyl-terminated surface. The surface coating of nanoparticles by APTES depends on experimental parameters like silane concentration, temperature and reaction time. 3.1. Characterization of the samples 3.1.1. E – DX analysis The elemental composition of the CoFe2O4 and APTES– CoFe2O4 nanoparticles were estimated by using an EDX detector and the results were shown in Fig.2 (a&b).
Fig,2.: Elemental analysis of NPs by energy dispersive X-ray (EDX) analysis. CoFe2O4 nanoparticles(a), APTES – CoFe2O4 nanoparticles(b).
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This figure indicates that the CoFe2O4 nanoparticles contained 14.30 % of Co, 51.70 % of Fe and 34.01 % of O2, while the APTES– CoFe2O4 nanoparticles contained 8.41 % of Co, 29.62 % of Fe, 5.78 % of O2, 0.02 % of Si, 15.58 % of N2 and 40.59 % of C, the presence Silicon, nitrogen and carbon indicated the successful conjugation of APTES with CoFe2O4 nanoparticles. 3.1.2.X-RD analysis Phase investigation of the crystallized product was performed by XRD analysis for the CoFe2O4 NPs and APTES coated nanoparticles as presented in Figure 3(a&b):
Fig.3.: X-ray powder diffraction patterns.(a) CoFe2O4 nanoparticles, (b) APTES – CoFe2O4 nanoparticles.
All of the observed diffraction peaks were indexed by the cubic structure of CoFe2O4 according to crystallographic standard (JCPDS 22-1086).The peaks appear with high intensity and a high basal width of all reflections observed which indicating that the samples were crystalline and formed nanoparticles. Figure 3 also cleared that after silanization of nanoparticles with silane agent (3-minopropyltrimethoxysilane) there were reduction in crystallinity and increase in crystallite size. The particle size was calculated by using Debye–Scherrer’s equation: � � � ����⁄������
(3)
Where D is the crystalline size, λ is the incident X-ray wavelength, β is the full width at half-maximum, and θ is the diffraction angle. Since the value of the crystalline size was next, ranging from 21.86 to 26.70 nm, with a maximum difference in size of 4.48nm. This indicated good uniformity of sample. It can be observed that the reduction in the amount of crystallinity for the silanized cobalt ferrite nanoparticles was attributed to the presence of silane incorporated with the cobalt ferrite, thus indicating that the silane was effective and that the ferrite structure is preserved. The average crystalline size showed that the values were different for both ferrites and the observation of increase after Silanization. 3.1.3.FESEM analysis The surface morphology of naked CoFe2O4 and APTES-CoFe2O4 nanoparticles was observed by scanning electron microscopy, Figure 4(A & B).
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(A)
(B)
Fig,4. Field emission scanning electron microscopy images of (A) CoFe2O4 NPs., (B) APTES –CoFe2O4 NPs.
The FESEM images of the prepared nanoparticles respectively were showed the formation of nanoparticles is nearly uniform and spherical shape. In the other words, during the silanization reaction, morphological properties of nanoparticles do not noticeably change. 3.1.4.AFM images Figure 5 represented the AFM images and the size distribution histogram which presented the films of naked cobalt ferrite NPs and APTES- cobalt ferrite nanoparticles which obtained by depositing a micro volume of the colloidal solution onto high-grade mica and allowing too dry at RT in a clean laminar flow chamber, Particles with an approximate spherical shape and an average diameter of 22.42 nm in the absence of APTES (left) & 28.06 nm in the presence of APTES (right) were observed. This may be considered as indirect evidence that difference of 5.64 nm corresponds to the APTES-coating.
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Fig,5.: AFM images of cobalt Ferrite NPs without (left) and with (right) APTES & size distribution histogram obtained from the AFM images.
3.1.5.FTIR analysis
The surface nature of samples was qualitatively assessed before and after silanization step
by using FTIR spectroscopy. Figure 6 (A&B). (A)
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(B)
3.
Fig.6.: FT-IR spectra of: (A) the naked CoFe2O4, (B) APTES- CoFe2O4
Figure 6(A&B)shown that the vibration spectrum of the infrared region, in the range 4000-400cm-1 using KBr pellet method for the prepared CoFe2O4 and silanized CoFe2O4 .The modification of basic functional group such as amino groups is important because these groups can be used to bind various biomolecules, drugs and metals by covalent bond or chemical interaction. FTIR spectra indicated the existence of these functional groups on MNP, respectively. For the amino groups on the MNP, the presence of N–H (1,533.45 cm-1), C–H (2,930.43 cm-1) and O– H (3,433.43 cm-1) bonding as chemical bonds on the surface of the MNPs was confirmed, as cleared in figure 6(B). The spectra shown two absorption bands below 1000 cm-1,the sharp which revealed peak around (572-435) cm1can be observed in (A) and (B) spectra which is relates to the absorption peak of (Fe- O) bond of nanoparticles. Figure 6(A) showed that there was band also observed in the range of about (3550) cm-1 which characteristic of the (O-H-O) bonds, from the presence of water in the sample, which may be derived from surface adsorption of atmospheric air and due to the use of KBr in the prepared samples. The presence of APTES on the surface of cobalt ferrite nanoparticles is proven by the bands at 1100 and 905 cm1 that dedicated to the Si –O stretching vibrations of APTES on the surface of magnetic NPs, and the broad band at 3433cm-1 and absorption peak at 1533.45cm-1 are attributed to stretching of the N-H (group NH2) and C=O amide groups, respectively Figure 7(B). The presence of the propyl group of APTES was confirmed by C–H stretching vibrations that appeared at 2922 cm-1. 4. Discussion. Cobalt-ferrite nanoparticles were synthesized by coprecipitating Co (II) and metal (Fe III) in alkaline medium. The pure and doped cobalt ferrite nanoparticles were synthesized by coprecipitation method. Due to low cost the coprecipitation method is widely used for the preparation of the nanoparticles for the industry use. The aqueous solution of divalent metal cations (Co2+ and Fe3+) results in precipitation of ferrite nanoparticles. Initially in coprecipitation method, the formation of metal hydroxides occurs in form of colloidal particles in alkaline medium (NaOH), through reaction [1].The next step can be regarded as ferritization. In this step the colloidal solution is heated up to 80oC and the solid solution of metal hydroxides converts into the required ferrite, through reaction [2]. The third step of coprecipitation method is called annealing, in which water from the product is removed through heating. The product contains a small amount of water (10%). This water in product cannot be removed during reaction. To remove this water from the product, it is then annealed at 600 °C Some parameters can affect the size and size distribution of nanoparticles prepared by coprecipitation method.
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In coprecipitation method two processes are important, namely nucleation and growth of the nuclei (center of crystallization). The rate of mixing of reactants is extremely important. Uniform and small particles are formed when the nucleation rate is faster than growth rate. The condition for the synthesis of uniform and small particles can be obtained by quick addition and fast stirring of reagents [41]. Increase in temperature in the range from (20 to 100) °C, is directly related to the rate of formation of ferrite. Different ferrites are formed at different activation energies. The yield of ferrite tends to grow when pH of the reaction becomes within the range from (7 to 10). The yield grows drastically when pH of the reaction reaches 12.5. Variation of pH of the reaction also affects the particle size [42]. Thus, the size variation and control has been achieved by both the rate of reaction and the annealing conditions. This work also includes coated the prepared cobalt ferrite NPs with APTES by development of a physical mixing procedure using a temperature without any initiator. This approach was more convenient, cheaper and less time consuming. Apart from this, using APTES as ligand and it was introduced to cobalt ferrite nanoparticles. The APTES has silane and amino terminals, the silane end covalently attached with nanoparticle surface and the amino ends are freely exposed [43].The process of surface modification by silanization reaction is very complex. Several parameters such as reaction time, temperature and silane concentration influence the reactivity of the silane molecule to the inorganic surface. The reaction between an alkoxy silane and a solid material does not involve a single mechanism, and many different intermediates are possible [44]. The silanization reaction occurs with two steps: First, the organo silane is placed into an aqueous solution of an acid that acts as a catalyst. It is hydrolyzed, and a condensation reaction occurs to form a silane polymer [45]. The following equation represents the simplified reaction of hydrolysis and condensation with production of silane polymer, as in the equation below:
The above equation cleared that alkoxide groups (-OC2H5) are replaced by hydroxyl groups (OH) to form reactive silanol groups, which condense with other silanol groups to produce siloxane bonds (Si–O–Si). Alcohol (C2H5OH) and water are produced as by-products of condensation [46]. In the second step, the polymer associates with the NPs forming a covalent bond with OH groups. Dehydration as well as adsorption of silane polymers to the metal oxide occurs [47], as in the equation below :
The cobalt ferrite nanoparticles core was using as template and it showed very high affinity towards the hybrid network. After that, the surface was modified with aminopropyl triethoxy silane (APTES). The ligands offered free amino functional group for binding. The below scheme clears the preparation steps for fabricating APTES-functionalized magnetic CoFe2O4 NPs:
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Schematic image of preparations of the APTES-CoFe3O4 nanoparticles The EDX analysis, figure (2) cleared the elemental composition which also revealed that the APTES molecules were successfully coated with nanoparticles, since the presence Silicon, nitrogen and carbon in the modification NPs and absent in necked NPs indicated the successful conjugation of APTES with CoFe2O4 nanoparticles, also, figure (3) cleared the variation between the values of the crystalline size, this difference may be attributed to the presence of the silane. The increase in crystalline size is due to the presence of silane agent which decreases the base width of reflections. However, since this reduction was slightly found that the presence of silane agent did not alter the structure of ferrite. Figures (4&5) showed the formation of nanoparticles is nearly uniform and spherical shape. In other words, during the silanization reaction morphological properties of nanoparticles do not noticeably change. Also, the figures showed the increase in the size between necked and modified NPs in AFM and FESEM images. In addition to the successful APTES coating onto nanoparticles, the surface nature of synthesized nanoparticles was qualitatively assessed by using FTIR spectroscopy. The FTIR spectra showed stretch the N-H (group NH2) and C=O amide groups, and the presence of the propyl group of APTES was confirmed by C–H stretching vibrations that appeared clearly indicated that the APTES was successfully coated to nanoparticles. Conclusions In conclusions this paper presented the preparation of CoFe2O4 nanoparticles with the range between (22-28) nm. The size of the nanoparticles was measured both by XRD and AFM and were in a good agreement with each other indicating that there was no agglomeration and the size distribution of the prepared nanoparticles was small. Also, the data indicated easy and effective method for the preparation of a modified cobalt ferrite nanoparticles with APTES to bind organo silane to a metal oxide nanoparticle by adsorption or covalent bonding, and the active amino group in its structure can combine with biomolecules, drugs and metals. The results showed that the heating of magnetite nanoparticles during the silanization reaction did not affect particle size; these were roughly spherical in shape and were around 28 nm in diameter. This value is very close to the size of magnetite crystalline, suggesting the formation of a continuous and very fine layer of silane on the surface of the magnetite core. So, finally the results in this study cleared the fact that the final product exhibited basic groups of amino and hydroxyl anchored on the external surface which can be used in many technological applications especially in various bio processes.
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