Results of EDS analysis of nanotube layers obtained by anodizing at 20V for 2h in 1M H3PO4 containing 0.2; 0.3; 0.4% wt. HF [53].
\r\n\t
",isbn:null,printIsbn:"979-953-307-X-X",pdfIsbn:null,doi:null,price:0,priceEur:0,priceUsd:0,slug:null,numberOfPages:0,isOpenForSubmission:!1,hash:"8b3c5c4439c736e81433536f7a5447eb",bookSignature:"Prof. Prof Nasser S Awwad and Dr. Ali Abdullah Shati",publishedDate:null,coverURL:"https://cdn.intechopen.com/books/images_new/9936.jpg",keywords:"Gadolinium Enhancement, Diagnostic Tool, Alloys, Salts, Magnetic Cooling, E. Coli, Bacillus Subtillis, Gadolinium as Burnable, Selective Separation, F-Block Elements, Adsorption, Kinetics",numberOfDownloads:null,numberOfWosCitations:0,numberOfCrossrefCitations:null,numberOfDimensionsCitations:null,numberOfTotalCitations:null,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"September 16th 2020",dateEndSecondStepPublish:"October 14th 2020",dateEndThirdStepPublish:"December 13th 2020",dateEndFourthStepPublish:"March 3rd 2021",dateEndFifthStepPublish:"May 2nd 2021",remainingDaysToSecondStep:"3 months",secondStepPassed:!0,currentStepOfPublishingProcess:4,editedByType:null,kuFlag:!1,biosketch:"Dr. Awwad edited a book for Lanthanides and published more than 25 papers about the elements at f blook, especially Gadolinium. He is a supervisor for 5 Master thesis in the field of Adsorption, removal, purification, kinetics, and modeling of Gadolinium.",coeditorOneBiosketch:"Dr. Shati has a lot of applications about the utilization of gadolinium enhancement. He has published papers about the inhibition of Gadolinium ion for the giant stretch‐activated channels of E. coli and Bacillus subtillis and in use for Kupffer cell depletion ( inactivation).",coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"145209",title:"Prof.",name:"Prof Nasser",middleName:"S",surname:"Awwad",slug:"prof-nasser-awwad",fullName:"Prof Nasser Awwad",profilePictureURL:"https://mts.intechopen.com/storage/users/145209/images/system/145209.jpg",biography:"Dr. Nasser S. Awwad has a PhD in inorganic and radiochemistry (2000) from Ain Shams University and a post-doctorate degree at Sandia National Labs, New Mexico, USA, 2004. Nasser Awwad was an Associate Professor of radiochemistry in 2006 and Professor of inorganic and radiochemistry in 2011 at the Egyptian Atomic Energy Authority. He has been a Professor at King Khalid University, Abha, KSA from 2011 to now. He has published two chapters in the following books ”Natural Gas - Extraction to End Use” and 'Advances in Petrochemicals”. He has been the editor for six books about: uranium, new trends in nuclear sciences, dyes in industry and lanthanides, and nuclear power plants. In addition, he has published 94 papers in ISI journals. He supervised 4 PhD and 16 MSc students in the field of radioactive and wastewater treatment. He participated in 25 international conferences in South Korea, USA, Lebanon, KSA, Egypt and India. He participated in 6 large projects with KACST at KSA and Sandia National Labs at USA on the conditioning of radioactive sealed sources and wastewater treatment. He has been the leader of many research groups about the utilization of nanomaterials for treatment of inorganic and organic pollutants and has also been a member of some research groups. He is a member of the Arab Society of Forensic Sciences and Forensic Medicine and is a member of the Egyptian Society for Nuclear Sciences and its applications. He is on the editorial board of the Journal of Energy and Environmental Research and Technology. He is a rapporteur of the Permanent Committee for Nuclear and Radiological Protection at King Khalid University and a member of the Committee for the Development of International Cooperation Management at KKU.",institutionString:"King Khalid University",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"4",totalChapterViews:"0",totalEditedBooks:"3",institution:{name:"King Khalid University",institutionURL:null,country:{name:"Saudi Arabia"}}}],coeditorOne:{id:"330586",title:"Dr.",name:"Ali",middleName:"Abdullah",surname:"Shati",slug:"ali-shati",fullName:"Ali Shati",profilePictureURL:"https://intech-files.s3.amazonaws.com/a043Y00000cA8q1QAC/Co2_Profile_Picture-1599648357298",biography:"Prof. Dr. Ali Abdullah Shati, a Saudi Biologist, graduated with BSc in Biology from King Saud University, Kingdom of Saudi Arabia in 1998, and MSc in Environmental Sciences from Essex University, the United Kingdom in 2004. He received his Ph.D. in Biology of Vertebrates in 2007 from Aberdeen University, United Kingdom. Since 2000, he has been working at King Khalid University in the Kingdom of Saudi Arabia, where he was promoted to Associate Professor in 2013, Professor in 2017 in the major of Vertebrate Physiology and Toxicology. He has held several positions at King Khalid University, including the head of Research Center at College of Science in 2012, Vice Dean of Scientific Research in 2012, Vice Dean of Academic Affairs in the college of science in 2014, and he is currently the Dean of College of Science. His research interests focus on studying the physiological and molecular changes invertebrates as a result of various environmental impacts, in addition to the cytotoxicity of Nano-materials, the therapeutic and protective effect of different bio-extracts, and antioxidant research, He has published more than eighty-seven online papers in international journals indexed in Clarivate Analytics and Scopus, with high impact factor. He has supervised MSc students specialized in the Physiological and Molecular effects of various components on vertebrate's functions. He participated in fourteen international conferences in the United States, United Kingdom, Canada, Australia, New Zealand, and Brazil. In the last ten years, he has awarded several research grants from the deanship of scientific researches at King Khalid University, as a principal investigator. He is also a member of the American Society of Toxicology, the Association of Arab Biologists, and the Saudi Biological Society.",institutionString:"King Khalid University",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"0",totalChapterViews:"0",totalEditedBooks:"0",institution:{name:"King Khalid University",institutionURL:null,country:{name:"Saudi Arabia"}}},coeditorTwo:null,coeditorThree:null,coeditorFour:null,coeditorFive:null,topics:[{id:"8",title:"Chemistry",slug:"chemistry"}],chapters:null,productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"},personalPublishingAssistant:{id:"259492",firstName:"Sara",lastName:"Gojević-Zrnić",middleName:null,title:"Mrs.",imageUrl:"https://mts.intechopen.com/storage/users/259492/images/7469_n.png",email:"sara.p@intechopen.com",biography:"As an Author Service Manager my responsibilities include monitoring and facilitating all publishing activities for authors and editors. From chapter submission and review, to approval and revision, copyediting and design, until final publication, I work closely with authors and editors to ensure a simple and easy publishing process. I maintain constant and effective communication with authors, editors and reviewers, which allows for a level of personal support that enables contributors to fully commit and concentrate on the chapters they are writing, editing, or reviewing. I assist authors in the preparation of their full chapter submissions and track important deadlines and ensure they are met. I help to coordinate internal processes such as linguistic review, and monitor the technical aspects of the process. As an ASM I am also involved in the acquisition of editors. Whether that be identifying an exceptional author and proposing an editorship collaboration, or contacting researchers who would like the opportunity to work with IntechOpen, I establish and help manage author and editor acquisition and contact."}},relatedBooks:[{type:"book",id:"7287",title:"New Trends in Nuclear Science",subtitle:null,isOpenForSubmission:!1,hash:"2156d3fb99aa1fd640aabf95d1ca9f4c",slug:"new-trends-in-nuclear-science",bookSignature:"Nasser Sayed Awwad and Salem A. AlFaify",coverURL:"https://cdn.intechopen.com/books/images_new/7287.jpg",editedByType:"Edited by",editors:[{id:"145209",title:"Prof.",name:"Prof Nasser",surname:"Awwad",slug:"prof-nasser-awwad",fullName:"Prof Nasser Awwad"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"7512",title:"Lanthanides",subtitle:null,isOpenForSubmission:!1,hash:"f7bcbda594eacb5a3bd7149e94628753",slug:"lanthanides",bookSignature:"Nasser S. Awwad and Ahmed T. 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Venkateswarlu",coverURL:"https://cdn.intechopen.com/books/images_new/371.jpg",editedByType:"Edited by",editors:[{id:"58592",title:"Dr.",name:"Arun",surname:"Shanker",slug:"arun-shanker",fullName:"Arun Shanker"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}}]},chapter:{item:{type:"chapter",id:"32763",title:"Anodic Layer Formation on Titanium and Its Alloys for Biomedical Applications",doi:"10.5772/34395",slug:"anodic-layer-formation-on-titanium-and-its-alloys-for-biomedical-applications",body:'\n\t\tProperties of the oxide layers on titanium and its implant alloys can be tailored to desired applications by anodizing parameters. Electrochemical oxidation in various electrolytes and different polarization regimes may shape the morphology, structure and chemical composition of oxide layers to enhance the use of titanium materials in electronics, photovoltaic and medicine. Phosphate electrolytes play specific role in the anodizing process. Besides forming compact barrier layer they enable also to form porous and nanostructural oxide layers enriched with phosphates, which enhance their bioactivity.
\n\t\t\tThe formation of anodic layers: thick or thin, compact or porous, gel-like and nanostructural on titanium and its alloys Ti6Al4V and Ti6Al7Nb in phosphoric acid solutions of different concentrations is described in this charter. Basing on morphological and chemical composition analysis (SEM, XPS) as well as on the electrochemical examination the influence of electrolyte composition on enrichment of surface oxide layers with phosphates and fluorides, enhancing their bioactivity, is presented. Studies to use Ti/titania systems as the platforms of the electrochemical biosensors to detect H2O2 and glucose proved the opportunity to use the nanotubular titania material as a platform for the 2rd generation biosensors.
\n\t\tAnodic films formed on titanium and its alloys are of great interest due to the industrial applications of metal covered with oxide layers of various and unique properties [1\n\t\t\t\t-7]. These layers have been investigated extensively by many authors [8\n\t\t\t\t-11]. Thick oxide layers on titanium, obtained by anodizing, provide improved resistance to local corrosion [12]. Anodizing can result in the adsorption and incorporation of inorganic and organic, biologically important species, e.g. phosphate ions, into the oxide layer. Such surface layers, desirable for medical implants, are not only corrosion resistant in a biological environment, but also compatible with tissue response [13\n\t\t\t\t-15]. Anodizing titanium and its alloys has been investigated in a wide range of parameters [16\n\t\t\t\t-20], which include also the participation of the electrolyte components, e.g. anions, in the formation of anodic films [21, 22].
\n\t\t\tAt anodizing oxide layers are formed according to the following reaction [17, 23]:
\n\t\t\tStudies in this field [24, 25] have shown that, phosphate ions can be incorporated into the anodic layer on titanium and Ti-6Al-4V, and in turn stimulate the formation of the bio-compatible hydroxyapatite [26].
\n\t\t\tAnodizing in phosphate solutions exhibit some advantages over other acid and base electrolytes. First of all less corrosive attack of phosphoric acid on titanium and its alloys, when compared with other acidic media, is related to the strong adsorption of phosphate anions on the surface [27,28]. Although unalloyed titanium is resistant [11] to naturally aerated pure solutions of phosphoric acid up to 30 % wt. concentration (~3.6 M) in phosphoric acid of lower concentrations (0.5-4 M), mainly non-dissociated acid molecules and H2PO4- of phosphate ions exist [29,30] and they exhibit a strong affinity or complexing power towards most metal cations.
\n\t\t\tAdsorption of phosphates onto TiO2 [28] and effect of pH on phosphoric acid composition [30].
Thus, anodizing in phosphate solutions leads to the incorporation of phosphate ions into the oxide layers on titanium and Ti-6Al-4V [5\n\t\t\t\t-8] influencing their bioactivity and stimulating deposition of the biocompatible hydroxyapatite. The latter may be used to shape properties of titanium implant materials for medical purposes.
\n\t\t\tAnodic layers on pure Ti and its alloys Ti6Al4V ELI and Ti6Al7Nb (ASTM F136-84), alloys in the annealed condition) can be formed by anodizing carried out at ambient pressure and room temperature in non-deaerated electrolyte solutions of 0.5 M H3PO4. Both techniques, the galvanostatic at anodizing current density values varied in the range of 0.1-0.5 Am-2 and the potentiostatic at up to 60V [22] are used. The oxide layers, 30-120nm thick, enriched with phosphorus are formed in these conditions. With mechanical and chemical pre-treatment applied to titanium and its alloys: Ti6Al4V ELI and Ti6Al7Nb (Timet Ltd, UK) [12\n\t\t\t\t\t-20], the layers obtained at 60V in phosphoric acid are golden and porous [11\n\t\t\t\t\t, 24\n\t\t\t\t\t-26] (Fig. 2) and they show very stable values of currents in passive region up to 1 V (SCE) (Fig.3) [11]. At other polarization parameters however layers of different thickness and colorization are formed [11]. Due to the presence of phosphates in the anodic layers they are highly bioactive in comparison to oxides formed in other electrolytes. Just after 9 days in the SBF solution (Simulated Body Fluid) they are covered with hydroxyapatite deposists (Fig. 2) [27].
\n\t\t\t\tPorous titania layers on Ti formed at 0.5 A/m2 in 0.5 M H3PO4 [22] (a,b) and HAp particles on anodic layer after 9 days in SBF solution [21, 25, 27] (c), JEOL JLM 5600 EDS.
The bilayer structure of compact oxide covered with HAp particles can be demonstrated also in the impedance tests (Fig. 3). The first time constant in Bode diagrams in range of the high and intermediate frequencies confirmed the high R\n\t\t\t\t\t\n\t\t\t\t\t\tt\n\t\t\t\t\t resistance of the barrier layer covering the anodized metal, thus giving the evidence of its high corrosion resistance. The second time constant corresponds to porous layer above the barrier one. Its lack in case of the Ti6Al4V ELI indicates the different characteristics of the coating on this implant material.
\n\t\t\t\tEIS spectra recorded after 9 days in SBF solution [21, 25, 27] for anodic layers on Ti, Ti6Al4V and Ti6Al7Nb formed at 0.5 A/m2 in 0.5 M H3PO4 [22].
To investigate the effect of phosphoric acid concentration (0.5 - 4 M) on the anodising of titanium and its alloys the galvanostatic and potentiodynamic techniques have been applied [11,19]. Particularly, the galvanostatic method with low current densities, up to 0.6 Am-2, applied in order to minimize side effects (ie. oxygen evolution), and more importantly to determine processes responsible for the growth of the oxide layer on the anodised metal at the early stages of its formation, allowed to observe the abnormal behaviour of titanium at anodizing. In Fig. 4 the results presenting the minimum rates of potential growth at initial stages of galvanostatic anodising in 2 M H3PO4 solutions are shown.
\n\t\t\t\tSurface response for the investigation of the effect of H3PO4 concentration and polarization current on the rate of potential growth dE/dt at galvanostatic anodizing of titanium [11].
Also the anodic polarization curves for titanium in electrolytes of different concentration show various shapes and different slopes in active-passive region (Fig.5).Potentiodynamic control at a comparable rate in 2 M H3PO4 applied to titanium and two of its implant alloys, Ti6Al4V ELI and Ti6Al7Nb, revealed a shift in corrosion potential toward the anodic direction with the lowest current densities in the passive region. This was possibly due to the effect of adsorption of phosphate ions onto the surface layer.
\n\t\t\tActive-passive transition of titanium in phosphoric acid solutions of 0.5-4 M [11,19] reveals that the growth of anodic layer is affected proportionally by the applied anodic potential, but shows the unusual influence of electrolyte concentration. Under galvanostatic conditions at low current densities (0.1-0.6 Am-2) the slope of dE/dt shows the minimum at the concentration ~2 M H3PO4 (Fig. 4), which is resulted due to a coating of an oxide film by an additional gel-like layer during anodizing, [28, 29], similar to the one observed in other media on aluminum.
\n\t\t\t\tIt was found that the active–passive transition was a process in which an inhibiting effect of phosphate ions on a dissolution of oxide layer was observed during anodizing [29]. Typical examples of voltage vs time transients (dE/dt) during the growth of the galvanostatic anodic oxide film on titanium for the current density of 0.5 A/m2 (Fig. 5a) show that the continuous linear growth of potential to the steady state, demonstrates the lowest value in 2 M H3PO4. Polarization curves (Fig.5b), show that after an initial range of cathodic depassivation, samples reach the corrosion potential E\n\t\t\t\t\t\n\t\t\t\t\t\tcor\n\t\t\t\t\t. Then an active–passive transition is observed with passivating currents the order of a few microamperes, which are typically observed during the passivation of titanium and its alloys. Anodic curves for 0.5 M and 3 M H3PO4 solutions (Fig.5b), illustrate quasi-passive behaviour in active-passive transitions, while curves for 1 and 2 M H3PO4, having the higher corrosion potential E\n\t\t\t\t\t\n\t\t\t\t\t\tcor\n\t\t\t\t\t, do not show linear dependence in this potential region. The differences in anodic Tafel slopes are accompanied by a shift of the E\n\t\t\t\t\t\n\t\t\t\t\t\tcor\n\t\t\t\t\t value in the positive direction by ~0.15V with the increase of H3PO4 concentration to 2 M (Fig. 5b).
\n\t\t\t\tCorrosion potential values Ecor of Ti anodised at 0.5 A/m2 in 0.5-2 M H3PO4 in SBF solution [11,29] (a) and active-passive transition regions of polarization curves for titanium (scan 3 mV/s)in 0.5-4 M H3PO4 (b).
SEM/EDS examination confirm the evidence of two-layered surface film. Such layers presented in Fig. 6, show the whole surface covered by a gel-like layer of H3PO4×0.5H2O.
\n\t\t\t\tThe SEM/EDS examinations reveal that thin films of anodic titania oxide are covered by gel-like layer with crystalline phosphates nuclei inside. Phosphates deposits are few in layers formed in 0.5 M H3PO4, but numerous and uniformly dispersed in a surface oxide of sample anodised in 2 M H3PO4. However, the oxide and phosphates are covered with the additional layer consisting of 76.3±3.6 wt.% of phosphorus and 23.7±1.5wt.% of oxygen (Fig.6a and 6b).
\n\t\t\t\tSEM micrographs of titanium surface anodized at 0.5 A/m2 in a,b) 0.5 M, c) 2 M H3PO4 [29], and d) HAp particles on anodic layer after 9 days in SBF solution [21, 27].
The EIS spectra of titanium after anodizing at 0.5 A/m2 in 0.5-2 M H3PO4 (Fig. 7), exhibit a behavior typical of a metallic material covered by a porous film which is exposed to an electrolytic environment [6]. Two time constants are seen in the spectra: the first in the high-frequency part arises from the ohmic electrolyte resistance and the impedance resulting from the penetration of the electrolyte through a porous film, and the second in low-frequency part accounts for the processes at the substrate/electrolyte interface.
\n\t\t\t\tImpedance spectra for titanium anodised in 2 M H3PO4 exposed to 0.9% NaCl solution a) Nyquist spectra, b) Bode diagrams and results oftheir fitting to c) equivalent circuit.
The EIS data can be fitted to the equivalent circuit in Fig. 7c, which consists of a solution resistance Rs, the capacitance Cp of the barrier layer, the charge transfer resistance associated with the penetration of the electrolyte through the pores Rp; and the polarization resistance of the barrier Rb as well as the electrical double-layer capacitance at the substrate/electrolyte interface Cb. In the case of surface layer formed in 2 M H3PO4 the specimen is covered by a passive oxide film of higher impedance (Fig.7a). The significant increase of the resistance Rb and Rp values for the 2 M H3PO4 anodized samples, over those determined for the 0.5 M H3PO4 anodized titanium, confirm that the EIS results are complementary to those obtained by E\n\t\t\t\t\t\n\t\t\t\t\t\tcor\n\t\t\t\t\t measurements and potentiodynamic polarization studies [11,31].
\n\t\t\t\tTitanium as metal very sensitive to the pre-treatment [33], due to the polishing, rinsing with water and drying, is usually covered by an air-formed oxide film and on immersion into acid solution shows potentials of the active-transition region [32-34]. However, in solutions of low pH may become active. In sulphate solution the anodic oxide film on titanium dissolves giving Ti3+ ions [11]. Typical activation behaviour and slow decrease in the open-circuit potential (–0.3 V SCE), is observed on immersing titanium into 1M HCl [35,36]. Titanium behaves differently in H3PO4 solutions. Although the values of E\n\t\t\t\t\t\n\t\t\t\t\t\tcor\n\t\t\t\t\t ranging from -0.1V to -0.6V (SCE) indicate in Pourbaix diagram [29] that the oxide film should dissolve to Ti3+, on immersion to H3PO4 solutions titanium shows the continuous shift of potential towards the anodic direction [32]. Such a tendency indicates that the rate of the anodic reactions is continually decreasing, as a result of the presence of an adsorbed, additional layer on the metal surface [37]. Thermodynamic data [11,33] for the potential E ≥ –0.8V (SCE), indicate that the following reactions on titanium are likely:
\n\t\t\t\tIn acidic solutions within the cathodic region, the only oxide dissolution is reaction (1). This reaction determines the potential-current changes in active-passive region of titanium in 0.5 M and 3-4 M H3PO4, whereas due to the shift of the corrosion potential E\n\t\t\t\t\t\n\t\t\t\t\t\tcor\n\t\t\t\t\t towards the anodic direction for titanium immersed in 1-2 M H3PO4 electrolyte, its direct oxidation proceeds according to reactions 3 and 4. These results indicate that, the layer of phosphates (Fig. 6) blocks the oxide dissolution. Insight into the adsorption of phosphates to TiO2 surface revealed the hypothesis according to which they form covalent bonding to oxygen [38], or metal ions react with phosphate anions forming a gel of metal hydrophosphates [39]. Both proposed processes would lead to local increase of pH at the oxide surface and in consequence to the increase of concentration of dihydro-phosphate ions (E-pH diagram) [29]. Then, on phosphates covered titanium oxide electrode, the following gel like layer formation could proceed
\n\t\t\t\tThis attribution agrees with Morligde’s et. al. results on aluminum [40]. Both reactions: the phosphates adsorption and gel-like layer formation are non-faradaic, but are competitive towards the oxide dissolution (reaction 1) with regard to proton consumption. The advantageous effect of these two reactions on the anodizing, may be attributed to an inadequate supply of H+ ions to keeping up with the demand for the reaction (1) of oxide dissolution. The increasing coverage of the anodized titanium surface by phosphates ions with the electrolyte concentration provides the evidence of a direct influence of electrolyte anions in suppressing the formation of dissolved titanium ions. According to potential/pH diagram for P-Ti-H2O system [41], H3PO4×0.5H2O, the product of reaction 5, is stable thermodynamically in solutions of pH ranging to 3.
\n\t\t\t\tThus, due to the applied anodizing conditions formation of either thin and porous oxide layer [11-23] or gel-like phosphates rich layer of H3PO4×0.5H2O [11\n\t\t\t\t\t, 24\n\t\t\t\t\t-29,\n\t\t\t\t\t42], covering thicker oxide layer on titanium can be obtained.
\n\t\t\tApart from mechanical properties and biocompatibility, which make titanium and its alloys the materials of choice for various applications (artificial hip and knee joints, dental prosthetics, vascular stents, heart valves) also enhancement of bone formation is desired feature of a metallic implant developed through adequate surface treatments to obtain proper osseointegration.
\n\t\t\t\tFast deposition of hydroxyapatite (HAp) coatings on titanium and its alloys Ti6Al4V and Ti6Al7Nb substrates anodised in H3PO4 was observed [21,23,25]. Anodizing in 0.5 M H3PO4, which produces phosphates enriched porous sub-surface layer on of titanium and its alloys Ti6Al4V and Ti6Al7N [22] or anodizing in 2 M H3PO4 which generates phosphates rich gel-like layer [31,42] may be used to enhance hydroxyapatite (HAp) deposition (Fig.8). For the latter anodic layers soaking the anodised substrates in simulated body fluid (SBF) resulted in the deposition of a uniform coating in 24 hours (Fig. 9). SEM and EDS investigations revealed that after 9 days thick coating consists of HAp globular of diameter varied from 100 to 300 nm aggregates. The Ca-O-P deposits merge in large clusters and they are seen in large numbers on both alloys, particularly on Ti6Al4V anodized in 2 M H3PO4.
\n\t\t\t\tSEM micrographs of titanium (a,b) and its alloys: Ti6Al4V (c,d) Ti6Al7Nb (e,f) surface anodized at 0.5 A/m2 in 0.5 M H3PO4 after 24 h (abc) and 9 days (b,d,f) in SBF solution [21, 23].
SEM observations (Fig.8) and EDS microanalysis indicate the presence of deposits dispersed on the surface of anodised titanium and its implant alloys. However, deposits are are non-uniformly dispersed on a surface. Titanium and its two alloys anodised in 0.5M H3PO4 are covered with very thin oxide layer, which includes numerous and more scattered Ca-O-P deposits of diameter varied from 200 to 800 nm, suggesting the heterogeneous nucleation of Ca-O-P on TiO2 covered surface. Althogh just after 24 hours deposits are seen on the surface of the 3 materials (more deposists on the Ti6Al4V alloy) the continuous films cover the whole surfaces after 9 days in SBF solution. At higher magnification it is seen that the film on titanium is formed of more flatter layer of deposits and broken layer of titanium oxides with titanium phosphates, whereas film on both alloys comprise small globules of Ca-O-P. The ratio of Ca/P ranging from 1.26 to 1.42 corresponds to non-steochiometric hydroxyapatite.
\n\t\t\t\tEIS) spectra recorded during immersion of titanium and Ti6Al6V samples anodized in 0.5 M and 2 M H3PO4 in SBF solution [21,23].
Impedance (EIS) spectra (Fig. 9) recorded during immersion of the anodized titanium and the Ti6Al4V alloy in simulated body fluid (SBF) for titanium and Ti6Al4V alloy show changes in capacitance and structure of surface layers as well as differences between coatings on titanium and its alloy and confirm the SEM observations (Fig. 8). Titanium exhibits two-layered structure: the inner oxide layer is covered by an outer layer of more or less uniformly distributed various size Ca-P-O deposits. On contrary the Ti6Al4V alloy is coated by a more uniform and dense layer of deposits (Fig. 8 c,d) and much lower concentration of titanium oxide on a surface [25].
\n\t\t\tIn the last 20 years anodizing has been also used as a method to form nanooxides on metal surfaces. Formation of self-organized titania nanotubes with high level organization of pores on large surfaces [43\n\t\t\t\t-48] became very useful technology applied to many purposes, i.e. to modification of surgical implant surfaces and to biomedical sensing. Titania nanotubes, just like barrier type titania, combine very well with osseous tissue and can be a perfect basis for osteoblasts in surgical implants. Studies focused on controlling the size and arrangement of pores [49\n\t\t\t\t-54], aiming at bone ingrowth and on use of titania nanotubes platform for biosensing, due to their capability to combine with e.g. enzymes, proteins or biological cells, brought promising results [55,56].
\n\t\t\tFormation of nanotubes at different polarization parameters in various electrolytes [57\n\t\t\t\t-60] as well as various scan rates during the very first seconds of anodizing, may help tailoring the oxides for effective implantation and improve their properties for biomedical and sensor applications. For the latter applications titania nanotubes require better ordering ie. controlled diameter achieved during improved oxide growth kinetics. For the last 5 years in several papers [61\n\t\t\t\t-64] it has been revealed that the value of polarisation determines the diameter of nanotubes. Every additional 5V of potential increases the nanotubes diameter of about 20nm, whereas the time of anodizing determines the length of the nanotube layer. Moreover, the low pH and organic aqueous solutions assure more regular shapes of nanotubes.
\n\t\t\tElectrochemical oxidization of titanium can be carried out in electrolytes with or without HF additives [65\n\t\t\t\t\t-67]. Attempts to assess the optimal scan rate/fluoride concentration ratio for formation of structurally uniform nanotubes [60] revealed that 1M H3PO4+0.3% wt. HF is the most proper electrolyte for anodizing at 0.5Vs-1. To study the effect of phosphates concentration, layers of titania nanotubes were produced in electrolytes of different phosphoric acid concentration. Their properties as the future coatings on titanium for medical uses were characterized by SEM/EDS observations and capacitance tests in simulated body fluids. Formation of oxide layers on titanium in phosphoric acid solutions with additions of fluoride ions [50] at 25ºC, is usually carried out in two stages: the first stage potentiodynamic to the desired potential and the second stage, potentiostatic with fixed potential on electrodes for over 2 hours (Fig. 10).
\n\t\t\t\t\n\t\t\t\t\tFig. 10 shows the behavior of titanium polarized from the OCP (Open Circuit Potential) to 20V with a sweep rate of 0.5Vs−1 in phosphoric acid solutions of different concentration (1M, 2M and 3M H3PO4) containing 0.4 wt.% HF. Flat polarization curve confirm passive behavior of titanium anodized in 2 and 3M H3PO4+0.4 wt.% HF, contrary to current transients recorded in 1M H3PO4+0.4 wt.% HF. The increase of current with potential in that region usually can be explained by the presence of some pores [9]. Polarization curves for more concentrated phosphate solutions show the presence of the anodic peaks, which can be ascribed to the oxygen evolution [6] followed by a broad passive region. By fixing the concentration of HF (fixing the dissolution rate) the decrease of current with potential indicates that oxide formation dominates over oxide dissolution at relatively higher field strengths or/and passive layer of phosphates is formed over nanotube titania in 2 and 3M H3PO4+0.4 wt.% HF solutions.
\n\t\t\t\tTransients for potentiodynamic experiments recorded for titanium anodized to 20V (with scan rate 500mV/s) at various concentration of supporting electrolyte H3PO4, a) 1M, b) 2M, c) 3M with addition of 0.4% wt. HF [53].
Anodic titania nanotubes formed on titanium in 1-3 M H3PO4 with 0.4% wt. HF (Fig. 11) show the morphology of nanotubes on titanium which differ in diameter and the layer thickness due to electrolyte concentration.
\n\t\t\t\tSEM images of titania nanotubes formed anodically prepared at 20V for 2 h in aqueous solutions of H3PO4 ranging from 1 M to 3 M with 0.4% wt. HF (field emission JEOL 7600F) [53,54].
SEM observations (Fig. 11) confirmed formation of a highly organized nano-sized pores, ranging from 90 to 120 nm in all applied electrolytes. As apparent, the average nanotube diameter is slightly affected by the supporting electrolyte concentration. Also, the increase of the latter from 1M to 3M under fixed HF concentration results in significant decrease of nanotube layer thickness, from 760±35 nm to 590±35 nm, respectively.
\n\t\t\t\tDiameters of nanotubes and the thickness of their layer on titanium formed in 1-3 M H3PO4 with 0.4% wt. HF.
The XPS analysis (Fig. 12) revealed that the highest amount of fluorides in oxide surface layer was obtained in 1M H3PO4+0.3% wt. HF, but in this case the lowest amount of phosphates adsorbed above nanotubes was observed. Using higher concentrations of phosphoric acid 2-3 M H3PO4 Judging on the results of XPS analysis, the competition between fluorides and phosphates is observed during anodizing and the higher concentration of the latter is responsible for higher bioactivity of nanotubes formed in 2M H3PO4+0.4% wt. HF [53].
\n\t\t\t\tResults of XPS analysis of nanotubes formed on titanium in 1-3 M H3PO4 solution containing different amount of fluorides, from 0.2% wt to 0.4% wt. HF VSW (Vacuum Systems Workshop, Ltd.) Kα Al (1486.6 eV) X-ray radiation working at power of 210 W (15 kV - voltage, 14 mA – emission current) [53].
The XPS spectra (Ti 2p, O 1s, P 2p and F 1s) revealed that nanotube layers consist of Ti, O, F and P species. The Ti 2p spectra for all samples showed only one doublet line. The position of the Ti 2p3/2 peak on the binding energy scale at 458.8 eV corresponded to titanium dioxide and Ti IV phosphates [16]. One type of phosphorus was revealed by the P 2p3/2 peak position at 133.3 eV associated to phosphate type species, indicating that species from the electrolyte are indeed adsorbed over the oxide film during anodizing. Oxygen was found to exist in two forms. The binding energies of the O 1s spectra corresponded to hydroxyl groups OH- (531.3eV) and oxygen in oxides O2- (529.9 eV). The presence of fluorine in the surface layer was confirmed by the F 1s spectra of binding energy 684.6 eV associated probably with Ti. As it is shown in Fig. 12 the concentrations of titanium corresponding to titanium dioxide and Ti IV phosphates are nearly the same in all tested samples, whereas the concentrations of the other elements vary with the composition of the anodizing electrolyte. Samples anodized in 1M H3PO4+0.3% wt. HF shows the highest amount of O2- (asTiO2) and fluorides, but the lowest amount of phosphates and hydroxyl ions. It means that previously recommended [6] conditions of uniform nanotubes formation on titanium implant materials favor titanium oxidation and enhance transport of fluorides in formed titania. The similarly high concentrations of relevant elements (Ti and O), together with the highest amount of phosphates of all controlled, are observed in samples anodized in 2-3M H3PO4+0.4% wt. HF. It indicates that the use of more concentrated phosphate electrolyte leads to the increase of phosphates adsorbed over the surface layer of nanotubes in competition with much smaller and more mobile fluorides.
\n\t\t\t\tThis is well known that at anodizing a competition between oxide formation and its dissolution exists, and that HF is the key factor, which causes the production of porous oxide layer. However, there is also a competition between phosphates and fluorides in the process of oxide nanotubes formation. These 2 anions differ in size, charge and rates of diffusion in oxides (Tabl. 2)
\n\t\t\t\t\tValues of diffusion coefficients and Van der Waals radius for fluoride and phosphate ions.
Values of the OCP for nanotubes formed in 1M, 2M and 3M H3PO4 [unpublished results].
The effect of the phosphoric acid concentration in fluoride containing electrolytes on the properties of oxide nanotubes formed at anodizing was characterized by SEM/EDS observations and capacitance characteristics when immersed in simulated body fluids (SBF) in order to predict their behavior as the future coatings on titanium for biomaterial applications [53].
\n\t\t\t\t\tThe values of the OCP (Fig. 13) for nanotubes formed in 1M, 2M and 3M H3PO4, each containing 0.4% wt. HF, measured at 25ºC in SBF solution 1 h after anodizing are -0.140 V, -0.170V and -0.195V (SCE), respectively, indicate the observed earlier [68] decrease of the OCP of oxide produced in more concentrated phosphoric acid solution.
\n\t\t\t\t\tThe impedance spectra for titanium anodized in 1-3M H3PO4+0.4% wt. HF were obtained at the OCP for frequency ranging from 105 to 0.18 Hz with ac amplitude 10 mV. The spectra recorded 1 hour after immersion in SBF solution show that variations in chemical composition of the surface layer over obtained nanotubes are confirmed by variations in capacitance characteristics.
\n\t\t\t\t\tThe results of EIS tests (Fig.14) indicate nearly the same properties (similar impedance and –θ angle values) for ohmic resistance of the electrolyte and its penetration through nanotube films. However in the low frequency range, the impedance values are sensitive to the
\n\t\t\t\t\tEIS spectra (a- Nyquist, b,c- Bode spectra) for titania nanotubes formed on titanium in 1-3 M H3PO4 solutions with addition of 0.4% wt. HF recorded at the OCP in SBF solution at 25ºC [53].
phosphate concentration in anodizing electrolyte, accounting for the processes at the nanotube layer/electrolyte interface which can be associated with deposited products. As the changes between spectra occurred during the first hour of exposure to SBF solution, one can assume that the deposition processes on nanotube layers formed in 2-3M H3PO4+0.4% wt. HF are quick.
\n\t\t\t\t\tThe formation of porous metal oxides, ie. titania and alumina, is explained by a field-enhanced model [11,61,63,69] that depends on the ability of ions to diffuse through the metal oxide. Thus, due to the large size the incorporation of the phosphate ions is difficult, but the increased fluoride concentration in solution leads to its ability to migrate and intercalate into the oxide films during the anodizing [70]. The XPS results show (Fig. 12), that the increased fluoride concentration is accompanied by the decreased phosphates and hydroxyl ions in adsorbed layer over nanotubes [53]. It correlates very well with the results of titanium anodizing in electrolyte not containing fluorides, where the gel-like protective layer of phosphates was formed over the oxide [42].
\n\t\t\t\tTitanium and its implant alloys, mainly ternary alloys of Ti-6Al-7Nb or, are widely used in biomedical implants and dental fields due to their unique mechanical, chemical properties, excellent corrosion resistance and biocompatibility [71\n\t\t\t\t\t-73].
\n\t\t\t\tFurther improvement of the unique properties of nanotube anodic layers for medical applications, particularly for enhancement of bone in-growth [74] and biosensing [75] require not only the development of the formation method on two phase titanium alloys, but also providing the proper morphology and structure. Reported efforts to form anodic nanotube layers on Ti alloys such as Ti-6Al-7Nb, TiAl [76], or Ti45Nb [77] showed the formation of highly inhomogeneous surfaces due to selective dissolution of the less stable phase and/or different reaction rates of the different phases of the alloys.
\n\t\t\t\tStudies on development of nanotubes growth on the Ti6A4V [60] and Ti-6Al-7Nb alloys [54] were focused on varying the HF concentrations in the phosphoric acid media, in order to establish the pore size distribution and estimate the critical scan rate/concentration ratio for the initiation of nanopitting in compact oxide layer, which would be decisive for the formation of uniform nanotubes on both two-phase alloys.
\n\t\t\t\tAmong several parameters influencing the quality of nanotubes formed anodically, such as potential, time of anodizing, fluoride ions concentration and scan rate of polarization, particularly the last two seem to be determiners for nanotubes structure and morphology. As an example to show the effect of fluoride ions concentration on the morphology of nanotubes on the implant alloy, the anodizing of the two phase (α+β) Ti6Al7Nb alloy samples in 1 M H3PO4 containing 0.2%; 0.3% and 0.4 % wt. HF to 20V using scan rate 500mV/s and then holding them at that potential for further 2h in the same electrolyte, was performed. Nanotubes of diameter ranging from 50nm to 80nm, with thicker walls over β-phase grains than over α- phase grains, were obtained. During the formation process, which includes two stages: the first potentiodynamic and the second potentiostatic (20V), different electrochemical behaviour was observed in electrolytes of various fluoride concentration.
\n\t\t\t\tThe implant alloy Ti6Al7Nb (Fig 15) of black α phase (hcp) and white β phase (bcc) irregular shape platelets forming variously oriented colonies, with the surface fraction of α and β phases 78% and 22%, respectively, was enriched with aluminum in oxides over α phase and enriched with niobium over β phase anodic nanotubes.
\n\t\t\t\tMicrostructure of the Ti-6Al-7Nb alloy [54].
Current transient for potentiodymic and potentiostatic stages recorded at anodizing the Ti-6Al-7Nb alloy and titanium (for comparison) at 20V for 2h in 1M H3PO4 containing 0.3% HF (scan rate in the potentiodynamic stage 500mV/s) and current transients recorded during potentiodynamic stage of anodizing of the Ti6Al7Nb alloy in 1 M H3PO4 with different fluoride concentration, a) 0.2%HF b) 0.3%HF c) 0.4%HF [54].
The typical current transients Fig. 16 recorded during the anodizing of the Ti-6Al-7Nb alloy in 1M H3PO4 containing 0.3 wt.% HF are similar to current transients observed during nanotube oxide layers formation on other alloys in other electrolytes [78]. As in previously described process the whole treatment consists of the potentiodynamic polarization from the OCP to 20V with a scan rate of 0.5Vs−1, followed by the potentiostatic polarization at 20V for further 2 h. However, contrary to constant current density increase observed at anodizing of pure Ti [49,50,79], during the potentiodynamic sweep to 20V at the alloy Ti-6Al-7Nb anodizing the current transients show 2 peaks: the first at about 2-3 V due to oxygen evolution and the second at about 4-6V linked probably to Al oxidation. In the potentiostatic stage of anodizing the current density for the alloy decreases until the end of the treatment, while in case of Ti a broad peak is seen at about 900 s of the anodizing (Fig. 16). According to [78,79] the broad peak, typically recorded in the potentiostatic stage of the process, indicates the dissolution of oxide before reaching final balance between both processes: oxide formation and oxide dissolution during nanotubes formation. Such the balance determines a steady-state oxide layer formation stage during anodizing of metals [11].
\n\t\t\t\tSEM images of nanotubes produced on the Ti6Al7Nb (a,c, e α-phase; b, d, f- β-phase) by anodization at 20V for 2h in 1M H3PO4 containing (a),(b) 0.2%HF, (c),(d) 0.3% HF, (e),(f) 0.4% wt. HF.
Small pits on β phase grains and regular nanotubes on α-phase are observed in 0.2 wt.% HF (Fig. 17a,b). Irregular tubes on β-phase and regular tubes on α-phase grains are seen after anodising in 0.3 wt. % HF (Fig. 17c,d). Both phases are covered with regular nanotubes in case of samples anodised in 0.4 wt. % HF (Fig. 17e,f), but on β- phase nanotube walls are thicker than on α- phase. Fig. 16 illustrates the dissolved oxide over α-phase on Ti6Al4V alloy and bigger size of nanotubes over β- phase in more concentrated phosphoric acid solution.
\n\t\t\t\tSEM images of nanotubes produced on the Ti6Al4V by anodization at 20V for 2h in 1M H3PO4 containing (a) 0.2%HF, (b) 0.4% wt. HF.
According to EDS analysis nanotubes formed on the Ti-6Al-7Nb alloy showed that those films are predominately TiO2 with small amounts of Ti2O3, Al or Nb oxides (Table 3). Aluminium and niobium are present in their most stable oxidation states, Al2O3 and Nb2O3. The amount of alloying elements in the nanotube oxide layer was influenced by the underlying metal microstructure, where Nb was present in the β- phase and Al in the α- phase [80].
\n\t\t\t\tResults of XPS examination of surface layer of nanotubes formed on the Ti6Al7Nb alloy in 1 M H3PO4 with different fluoride concentration.
In the combined SEM and XPS examinations [54] (Fig. 17 and 19) the highest intensities for all controlled elements and groups: titanium oxide and titanium phosphates (458.7eV), oxides (530eV), hydroxyl ions (531.6eV), phosphates (133.3eV) and fluorides (648.6eV), clearly confirm that the most advantageous scan rate and electrolyte composition for the formation of uniform nanotube layer on the Ti6Al7Nb alloy, are 0.5Vs-1 during potentiodynamic stage of anodizing in 1M H3PO4 containing 0.3% wt. HF. Interesting is that also the intensity of niobium (207.3eV) in the most stable of the niobium oxides Nb2O5 [81], increases with fluoride concentration, but seems to reach the limit in these conditions for 0.3% wt. HF (Fig. 19). The highest current density (Fig. 14) is linked to the biggest nanotube diameters, as it was observed in case of pure titanium anodised in the same conditions [50].
\n\t\t\t\tFluoride concentration | \n\t\t\t\t\t\t\t0.2%HF [weight %] | \n\t\t\t\t\t\t\t0.3%HF [weight %] | \n\t\t\t\t\t\t\t0.4%HF [weight %] | \n\t\t\t\t\t\t\tCompact oxide [weight %] | \n\t\t\t\t\t\t|||
Phases | \n\t\t\t\t\t\t\tα | \n\t\t\t\t\t\t\tβ | \n\t\t\t\t\t\t\tα | \n\t\t\t\t\t\t\tβ | \n\t\t\t\t\t\t\tα | \n\t\t\t\t\t\t\tβ | \n\t\t\t\t\t\t|
Titanium | \n\t\t\t\t\t\t\t63.90 | \n\t\t\t\t\t\t\t51.66 | \n\t\t\t\t\t\t\t61.39 | \n\t\t\t\t\t\t\t35.70 | \n\t\t\t\t\t\t\t59.52 | \n\t\t\t\t\t\t\t38.59 | \n\t\t\t\t\t\t\t69.22 | \n\t\t\t\t\t\t
Oxygen | \n\t\t\t\t\t\t\t32.09 | \n\t\t\t\t\t\t\t36.66 | \n\t\t\t\t\t\t\t34.44 | \n\t\t\t\t\t\t\t45.43 | \n\t\t\t\t\t\t\t36.40 | \n\t\t\t\t\t\t\t44.99 | \n\t\t\t\t\t\t\t19.72 | \n\t\t\t\t\t\t
Aluminium | \n\t\t\t\t\t\t\t4.00 | \n\t\t\t\t\t\t\t2.91 | \n\t\t\t\t\t\t\t4.17 | \n\t\t\t\t\t\t\t2.69 | \n\t\t\t\t\t\t\t4.08 | \n\t\t\t\t\t\t\t1.99 | \n\t\t\t\t\t\t\t4.45 | \n\t\t\t\t\t\t
Niobium | \n\t\t\t\t\t\t\t--- | \n\t\t\t\t\t\t\t8.77 | \n\t\t\t\t\t\t\t--- | \n\t\t\t\t\t\t\t16.18 | \n\t\t\t\t\t\t\t--- | \n\t\t\t\t\t\t\t14.43 | \n\t\t\t\t\t\t\t6.53 | \n\t\t\t\t\t\t
Results of EDS analysis of nanotube layers obtained by anodizing at 20V for 2h in 1M H3PO4 containing 0.2; 0.3; 0.4% wt. HF [53].
Due to chemical similarity of titanium and niobium [11, 82] electrochemical behaviour of the Ti-6Al-7Nb electrode should be qualitatively similar to that of the titanium and niobium electrodes in the potential range from -1 to 4V (SCE). Electrochemical oxidation of niobium electrode leads to formation of sub-oxides NbO and NbO2 at the OCP, which partly transform into Nb2O5 oxide at 20V, according to the equations 6-7 [83,84]:
\n\t\t\t\tThe dissolution process of niobium oxide (β-phase) (5) increases with increasing fluoride concentration [85], so the fluoride concentration is a crucial factor for nanotubes growth on Ti-6Al-7Nb. Structural and metallurgical aspects of the formation of self-organized anodic oxide nanotube layers on alloys are crucial for medical application to the advanced techniques of biological media immobilization which require morphologically uniform surface.
\n\t\t\tThe additional advantageous property of phosphate rich compact and nanotubular anodic oxide layers on titanium is its ability to attach enzymes, proteins or biological cells. To test such the possibility in order to apply anodic surfaces for H2O2 biosensing two electrodes were prepared: 1) the first electrode prepared by the electropolymerization of conducting polymer (PANI) on the surface of Ti/TiO2 (compact) electrode [55], 2) the second electrode was prepared by using titania nanotubes on titanium as a platform of the 3rd generation biosensor [56]. In both cases the HRP (horseradish peroxide) enzyme was immobilized on the sensing surface. By using either cyclic voltammetry or amperometric modes the feasibility and electrochemical parameters for H2O2 monitoring on Ti/TiO2 surface were checked in the simulated body fluid (SBF). Both electrodes were sensitive to H2O2, however the second electrode only in the presence of thionine as the mediator [56]. Two peaks seen on cyclic voltammograms (Fig. 18) for the Ti/TiO2 (nanotube) electrode with immobilized HRP, indicate the sensitivity of the prepared platform to the presence of H2O2 in the analyte.
\n\t\t\tSEM of Ti/TiO2 (nanotube) covered with HRP and cyclic voltammograms for Ti/TiO2/HRP in 0.1 M PBS (pH 6.8) in the presence of H2O2, scan rate 100 mV/s [56].
Titanium surfaces can be modified by electrochemical treatment in the phosphoric acid solutions for better corrosion resistance, improved physicochemical and electrochemical properties and bioactivity. The formation of oxide layers enriched with phosphorus of 30-120nm thick can be formed in 0.5 M H3PO4 at both galvanostatic anodizing current density values varied in the range of 0.1-0.5 Am-2 and potentiostatically at up to 60V giving yellowish layers porous on the surface. Due to the presence of phosphates they are highly bioactive in comparison to oxides formed in other electrolytes and are covered with hydroxyapatite deposists after 9 days in the SBF solution.
\n\t\t\tAnodizing in more concentrated 2M solutions of the phosphoric acid generates a gel-like film with thickness of about 100nm on titanium. The film, containing a large number of phosphates nuclei, exhibits its effectiveness to activate titanium surface for biomimetic coating of calcium phosphate. The electrochemically treated titanium was able to form uniform Ca–P coatings on titanium after 48 hour immersions in the SBF solution. The treatment is a simple method to generate bioactive metal surfaces, besides other methods such as alkaline treatment applied to titanium implant materials.
\n\t\t\tElectrochemical treatment in the phosphoric acid solutions with the addition of 0.2-0.4% wt. HF allows to form on titanium and its implant alloys nano-sized pores (nanotubes) in more concentrated phosphoric acid solutions (1-3M). Their morphology, electrochemical properties and chemical composition are in close relation with the anodic polarization parameters and with the concentration of both ions: phosphates and fluorides. The highest amount of fluorides in surface layer is obtained when using 1M H3PO4+0.3% wt. HF, but in this case the lowest amount of phosphates adsorbed above nanotubes is observed. The use of higher concentrations of phosphoric acid (2-3M H3PO4 with 0.4% wt. HF assures the formation of nanotubes containing the high concentration of both bioactivity enhancing elements, fluorides and adsorbed phosphates. The obtained titania nanotubes show the significantly higher bioactivity in vitro during the first hour of immersion in SBF in comparison to barrier titanium oxide.
\n\t\t\tDepending on fluoride ion concentrations in anodizing electrolyte morphologically different nanotubular layers have been obtained on both phases of two titanium alloys: the Ti6Al4V and the Ti6Al7Nb alloys. Self organized nanotubes grow on both phases (α and α+β) in 1M H3PO4 containing 0.4% wt. HF, though smaller pore size and thicker wall tubes are obtained on the β phase. The electrochemical behavior of both phases of the alloys differs due to fluoride concentrations which is the key parameter in controlling their morphology. Uniform nanotubes are obtained in 2M H3PO4 containing 0.3% wt. HF at scan rate of polarization 0.5Vs-1 during potentiodynamic stage of anodizing. Such conditions assure the highest fluoride and phosphate concentrations in surface layer of nanotubes on titanium and nanotubes containing niobium oxide on the Ti6Al7Nb alloy. Both features promise a proper coating for improved osteoblast cell adhesion on artificial implants and for biosensing.
\n\t\tFunding from the Polish Ministry of Science and Higher Education under the N507 082 31/2009 project and by the National Centre of Research and Development under ERA-NET/MNT/TNTBIOSENS/1/2011 Project is gratefully acknowledged. My thanks go also to Professor Patrick Schmuki of University of Erlangen for inspiration on nanotubes and to my coworkers from the Biomedical Engineering Division at University of Zielona Góra.
\n\t\tIron is one of the most abundant elements in the earth’s crust. It always coexists with metals in the ore, mainly exists in the form of hematite, magnetite and muscovite on the surface of particles or in the inclusions inside crystals [1]. In hydrometallurgy, iron, although is converted into insoluble precipitates and removed in advance by sulfation roasting, soda roasting, acid leaching, etc. during ore pretreatment, still inevitably goes to the aqueous solution with the dissolution of the target metal during the leaching process [2, 3, 4]. The classical methods for removing iron in the leaching solution are precipitation, extraction, ion exchange, displacement, and electrowinning [4]. The commonly used method is the precipitation method, which separates iron ions by converting to iron precipitation compounds. According to the different iron precipitation compounds, it can be divided into jarosite [5, 6], hematite [7], iron(III) oxide-hydroxide [8] and goethite [9, 10] method, etc. The jarosite method produces a large amount of low-grade iron-bearing slag in the application, which is difficult to handle, consumes a large amount of sulfate, and causes certain environmental problems [5, 6]; the hematite method needs to be carried out under high temperature and pressure, which consumes large energy and high CAPEX (capital expenditure) [7]. The filtration efficiency of Fe(OH)3 colloid precipitation method is low, and it is easy to adsorb a large amount of other valuable metals, causing large metal loss [8].
\nThe goethite method is widely used in hydrometallurgical plants for zinc, copper and nickel as the main process for removing iron because of its low CAPEX and environmentally friendly products [9, 10]. In order to ensure the effect and efficiency of iron removal, the goethite process must strictly control the concentration of Fe3+ below 1 g/L, and thus developed the two commonly used processes - VM method and EZ method [8, 9, 11]. The former firstly reduces all the iron ions to Fe2+, and then slowly oxidizes the Fe2+ to Fe3+ under hydrolysis conditions to control the content of Fe3+ [9], and the latter slowly adds the concentrated pressure leachate containing Fe3+ in the precipitation vessel with addition rate of less than the Fe3+ hydrolysis rate, thereby forming goethite precipitation [11]. The pH in goethite process is common lower than 4.0, and calcium hydroxide or calcium carbonate is usually used as neutralizer, which will result in a large amount of calcium sulfate mixed with the goethite residue [12]. These mixed residues reduce the filtration efficiency and cause the loss of valuable metals such as Zn and Ni [5, 13, 14]. In addition, the residue mixture accumulated in the tailings pond contains heavy metals such as Pb, As, and Cr, which causes pollution of local water and soil. Therefore, improving filtration performance and reducing the loss of valuable metals are two problems that need to be solved urgently in the traditional goethite precipitation method.
\nThis article summarizes the new improvements in iron removal by precipitation methods in recent years, and on this basis, proposes a novel iron removal process - magnetic seeding and separation. A core-shell structure is formed by precipitating and growing iron on the magnetic seeds surface, and achieves high-efficiency solid-liquid separation by magnetic separation. The new process remarkably reduces the loss of valuable metals in iron removal. Magnetic seeding and separation processes have not only been successfully used in the removal of iron from hydrometallurgical leachate, but also shown good application prospects in wastewater and soil pollution treatment.
\nMagnetic flocculation and separation based on the magnetic difference of materials can easily separate magnetic solids from mixtures. It shows higher selectivity and efficiency than centrifugation and filtration, and has been widely used in water treatment, biotechnology and minerals separation [15, 16, 17, 18]. As is shown in Figure 1, Han et al. [3] studied the feasibility of magnetite precipitation in the hydrometallurgical nickel leaching solution. Under lower oxidation potential, at pH 2.0–2.2 and 90–100°C, the iron ions in the leachate may slowly oxidize and partially precipitate in the form of magnetite. Magnetic flocculation and separation can effectively separate the precipitate from the solution. Unfortunately, the iron precipitation from solution is still dominated by goethite, the magnetite composition is relatively small, and it is difficult to truly achieve effective magnetic separation in industrial applications. But this research of magnetite process of iron removal provides other new ideas of magnetic separation.
\nPotential/pH diagram for Fe-H2O system at 100°C.
The goethite process can be divided into four stages: (a) hydrolysis to monomers and dimers; (b) the reversible stage involving rapid growth to small polymers; (c) formation of slowly reacting large polymers; and (d) precipitation of a solid phase [19, 20]. The goethite precipitation system is a complex system, and the presence and content of different components and iron phases have a greater impact on the precipitation and filtration performance of goethite. As shown in Figure 2, the pH and temperature conditions of the sulfate-containing solution determine the existence and content of different iron phases such as hematite, goethite, iron hydroxide and hydroxyl salt [21]. The goethite residues that cause filtration difficulties and metal loss are composed of amorphous iron phase, six-line ferrihydrite, poor crystalline goethite, solid solution jarosite phase and silica [2, 22]. Therefore, the crystallinity, size and content of the goethite particles can be controlled by adjusting the pH, thereby improving the separation performance and the loss of valuable metals.
\nTemperature and pH conditions for the precipitation of hematite, goethite, ferric hydroxide, and hydroxy salts (including jarosites) from 0.5 M ferric sulfate solution [21, 23].
Yue and Han [23] study that as the pH value decreases from 5.0 to 2.0, as shown in Figure 3, the crystallinity of goethite decreases, the goethite particles tend to agglomerate, the particle size increases significantly, and the filterability of the precipitate improves. Nickel is lost in the iron precipitate by being incorporated into the crystal lattice and adsorbed on the surface of the goethite particles, and the nickel adsorption loss are related to the specific surface area of the goethite particles. When goethite is in an intermediate transition state at low pH (2.5–3.3), which is between the crystalline state and the colloidal state, the loss of nickel is the least. However, the improvement by only adjusting the pH of the goethite precipitation process is minimal. Chang et al. [24] carefully reduced the pH from 4.0 to 2.5, and the loss of nickel is only reduced by about 10% in the iron precipitation. Moreover, it is not realistic to achieve such detailed condition control in actual industrial applications.
\n(a) SEM images of the goethite precipitate at different pHs and (b) pH effect for the nickel loss, the crystallinity, and the specific surface area of the precipitate [23, 25].
The traditional goethite precipitation method needs to overcome high barriers to the formation of crystals, and often requires a few days of reaction time. The amorphous iron phase appears at this stage, making precipitation separation difficult. Seed induced crystallization can make crystals precipitate and crystallize from the solution at lower solution saturation, pH value and temperature, and has been widely used in the preparation and production of drugs and nanomaterials [26, 27, 28, 29]. Han [30] choose natural limonite as the seed crystal of goethite and induce crystallization to improve the problem of poor filterability at the low pH goethite precipitate. As is shown in Figure 4, by adding limonite seeds, the particle size of the goethite precipitate is significantly increased. The goethite particles in the particle size range of 37–74 μm have the largest yield and the smallest specific surface area, which can result iron precipitates with a nickel grade of <1%. However, the reduction of metal loss and improvement of filterability are difficult to achieve at the same time by pH control and induced crystallization, one of them must be sacrificed. The intermediate transition state goethite with good filtration performance and minimum metal loss is difficult to accurately induce formation in the actual field industry. It is a need to find other ideas to achieve qualitative progress.
\nThe specific surface area and the nickel grade of iron precipitates with limonite seeds in different size ranges (2 g/L limonite seeds, pH 2.1–2.5, 85°C) [30].
Han et al. [25, 31, 32] combined seed induced crystallization and magnetic separation, and proposed a novel magnetic seeding and separation process, as shown in Figure 5. Before the iron is precipitated as goethite, fine-grained maghemite or magnetite particles are added to the leaching solution to make the goethite precipitate and grow on the surface of the magnetic particles, thereby avoiding mixing with the calcium sulfate precipitation in the solution. The iron precipitates on the surface of the goethite to form large magnetic particles with a core-shell structure, and the precipitates are efficiently settled and separated by magnetic separation. The results show that the iron content in the dry iron residue is more than 52% and the Ni content is less than 0.6%, which can be used in industrial applications to deal with a large amount of iron precipitation. After the calcium sulfate precipitation is roasted, 99% of S and As can be removed, and the roasting residue can be respectively used as raw materials for ironmaking and building materials.
\nThe process of iron precipitation on the magnetic seeds and the magnetic flocculation in magnetic field [3, 25].
Yue et al. [31] applied magnetic iron seeding and separation to separate goethite from calcium sulfate in zinc leaching with maghemite fine particles as carrier. As is shown in Figure 6, the magnetic goethite-maghemite aggregates were separated effectively from calcium sulfate precipitates by magnetic drum separator, and 90% of Fe and Ca is respectively recovered in two corresponding products. Roasting goethite precipitate with coal powder under the optimum conditions removed 99% of S and As. Goethite products can be directly used in the ironmaking industry, and calcium sulfate precipitation can also be used to produce cement and building materials.
\nSchematic illustration of magnetic separation and production of desired goethite and gypsum product [31].
Yue et al. [32] establish the surface complex and precipitation model of goethite on magnetite and maghemite magnetic nanoparticles, as shown in Figure 7. The formation of Fe (III) surface complexes are directly related to the nucleation and precipitation of goethite on the solid surfaces of the two magnetic nanoparticles. The more polynuclear surface complexes produced on the particle surface, the more precipitation of heterogeneous forms. Fundamentally, it is possible to screen out the best material as the crystal nucleus to separate goethite from calcium sulfate or other heterogeneous precipitation.
\nSurface precipitation model modeling (a) of Fe3+ adsorption/precipitation on magnetite and maghemite with corresponding magnetic separation of goethite, images of the suspensions in a magnetic field with 2 g/L (b) magnetite and (c) maghemite NPs, and SEM images of goethite precipitates with (d) magnetite and (e) maghemite NPs [32].
The Cr-bearing electroplating sludge is produced from the treatment of Cr wastewater and metallurgical processes [33, 34, 35, 36]. It contains excessive amounts of heavy metals, such as Cr, Fe, Ni, Cu, Pb and Zn, or potential dioxin pollutants [37, 38], therefore must be treated before stacking. Many methods have been applied to recover Cr from the acid leaching solution of electroplating sludge, such as electrochemical precipitation (ECP) [39], selective extraction [35, 40], adsorption or biosorption [41, 42, 43, 44] and Cr-Fe coprecipitation [45, 46, 47, 48]. Compared with other methods, recovering Cr by Cr-Fe coprecipitation is simple, economical and practical for industrial applications. In addition, the advance coprecipitation of Fe and Cr can avoid their interference on the recovery of Ni, Cu and Zn.
\nYue et al. [49] use the novel magnetic seeding and separation process to recover Cr(III) and Fe(II) synchronously by forming the Cr(III)-Fe(III) coprecipitates on the surface of maghemite (γ-Fe2O3) fine particles. The active hydroxide radicals on the surface of magnetic seeds induce the nucleation and growth of goethite, which results in enhanced Cr (III)-Fe(III) coprecipitation. As shown in Figure 8, the maghemite particles, served as the crystal nuclei, could induce the formation of the core-shell structured Cr (III)-Fe(III) coprecipitates on its surface and accelerate the sedimentation of the coprecipitates in the magnetic field. The results of the two-stage coprecipitation showed that the total recoveries of Cr and Fe were 96.17 and 99.39%, respectively, and the grades of Ni, Cu, and Zn in the precipitates were 0.41, 0.38, and 0.22%, respectively. The obtained coprecipitates can be recycled as the feed material of chromium smelting after heat treatment. This method is simple and efficient for high-concentration Cr3+ solution treatment, which is beneficial for the sustainable development of resources and environment.
\nSEM images of the Cr(III)-Fe(III) coprecipitates without maghemite fine particles (a) and with maghemite fine particles (b), respectively; scheme (c) of the formation of γ-Fe2O3/Crx Fe1-xOOH with core-shell structure [49].
Arsenic (As) is contained in most metal deposits, and therefore a large amount of arsenic-containing wastewater, flue gas and residues will be produced in mineral processing and smelting, posing a huge threat to the environment [50, 51, 52]. Commonly used methods for removing arsenic from solution include precipitation, electrocoagulation, ion exchange, membrane technology and adsorption [53, 54, 55, 56]. In order to remove arsenic and recover valuable metals at the same time, these methods all require acid leaching of the waste, which will produce highly toxic and deadly arsine gas [54, 57]. As is shown in Figure 9(a), Yue [58] developed a safer alkaline leaching method - oxidation alkali leaching of the wastes to transform arsenic compounds into arsenate (\n
(a) Flow diagram of the comprehensive treatment of the arsenic alkali residue and (b) arsenic removal from arsenic alkali solution with different HFG samples synthesized at pH 3(I), 7(II), and 11(III) [58].
There are a large number of reports that iron oxides have excellent adsorption and precipitation effects on heavy metal ions impurities in aqueous solutions, such as CrU and As. Garcı́a-Sanchez et al. [59, 60] found that goethite has a special adsorption effect and capacity for As ions. Wei Jiang [61] considers that arsenic [\n
Phosphorus and starch reportedly are the main wastewater contaminants that are difficult to remove efficiently [63, 64]. When the phosphorus concentration in water exceeds 0.02 mg/L, phosphorus becomes a polluting element and causes eutrophication of water bodies [65, 66, 67]. Starch is a commonly used and cheap material, widely used in many chemical and material industries, but it produces high concentration of organic wastewater, which will affect the environment [68, 69, 70]. Therefore, phosphate and starch removal from wastewater has become the focus of many studies. The main phosphate and starch removal methods are similar, such as chemical precipitation [71, 72, 73, 74], biological methods [75, 76, 77, 78, 79] and adsorption techniques [80, 81, 82, 83]. Among them, Chemical precipitation and adsorption technology is commonly used in wastewater treatment due to the simple operation with low cost and large processing capacity compared to other methods [84, 85, 86]. However, chemical precipitation inevitably produces a large amount of fine precipitation and suspended solids, which seriously affect the sedimentation and filtration efficiency [84, 87]. And the adsorbents currently used in adsorption technology, such as activated carbon [70, 88], silica gel [89, 90], membranes [91, 92, 93], etc., have high production costs and poor adsorption performance, which greatly limits the adsorption effect and industrial applications.
\nMagnetic flocculation is an effective way to remove ultrafine suspended solids in water treatment [94, 95]. It adds magnetic seeds to the aqueous solution to form magnetic flocs with the ultrafine suspended solids in the wastewater, and then passes through a magnetic separator to achieve rapid precipitation and separation [3, 95, 96]. The combination of magnetic flocculation and chemical precipitation can make up for the shortcomings of ultrafine suspended solids and low separation efficiency of chemical precipitation. Magnetic flocculation has been widely used to treat wastewater with high pollution concentration [71], high turbidity [96] and high chemical oxygen demand (COD) [97]. It is worth noting that in many studies, iron-bearing minerals have shown the characteristics of removing phosphorus from aqueous solutions [98, 99]. The iron-bearing minerals can be coordinated with phosphate and therefore have the potential to be used as adsorption materials for phosphorus and starch in wastewater [100, 101].
\nDu et al. [102, 103] combined the magnetic flocculation technology with iron-containing materials to prepare porous magnetic seeds with core-shell structure, which achieved simultaneous removal of starch and phosphate in wastewater. As shown in Figure 10, the core-shell magnetic seeds prepared by sulfation roasting of fine magnetite particles have a porous α-Fe2O3 structure on the surface, and the specific surface area is three times larger [103, 104, 105, 106]. As shown in Figure 10, the phosphate and starch in the wastewater can be adsorbed on magnetic seeds surface, and then separated from the wastewater by magnetic separation. The phosphorus and starch content in the wastewater are reduced to 1.51 and 9.51 mg/L, respectively, and the removal rate reaches more than 75% [102].
\nThe chemical precipitation and magnetic flocculation of removed hydroxyapatite contaminants [103].
The iron removal method of the hydrometallurgical leachate is still dominated by the goethite process. The goethite process faces the disadvantages of high loss rate of valuable metals and difficulty in separation and filtration, which must be solved to get qualitative improvement. Careful adjustment of the pH value can help reduce metal loss, and inducing crystallization can increase the crystallinity of goethite and improve the separation and filtration efficiency. However, both methods can only focus on solving one of the problems and cannot reduce loss and promote filtration at the same time. The magnetite produced during the precipitation (crystallization) process opened a new path for magnetic separation, while the magnetite method is currently limited to laboratory research. In the present paper, the authors combined the goethite precipitation (crystallization) method with magnetic seed separation technology and developed a novel route. Goethite precipitates on the surface of the external magnetic seeds to form core-shell structured particles, which are efficiently separated by magnetic separation, and at the same time solve the two major problems of the traditional goethite process. This new method also shows advantages in the fields of arsenic and chromium removal from the leachate, phosphorus, and starch removal from wastewater and other fields. Goethite is the most common and stable crystalline iron oxide in soil and sediment. We expect that the goethite method combined with magnetic seed separation technology will show better results in the removal of organic dyeing, heavy metal ions, anions in wastewater and soil, and the adsorption and passivation of chemicals, nutrients, and harmful compounds in environments.
\nThis work was supported by the Hunan Natural Science Foundation of China (No. 2020JJ5727), Innovation Driven Plan of Central South University (No. 2018CX036), National 111 Project (No. B14034), and Collaborative Innovation Center for Clean and Efficient Utilization of Strategic Metal Mineral Resources, Key Laboratory of Hunan Province for Clean and Efficient Utilization of Strategic Calcium-containing Mineral Resources (No. 2018TP1002).
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