• Title/Summary/Keyword: FE-SEM/EDS

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High Temperature Stability of Nitride Ceramic Materials in LiF-NdF3-Nd2O3 Molten Salts System (LiF-NdF3-Nd2O3 용융염에서 질화물계 세라믹재료의 고온안정성)

  • Kwon, Sukcheol;Lee, Young-Jun;Ryu, Hong-Youl;Lee, Go Gi;Jo, Sung Koo;Lee, Jong-Hyeon
    • Korean Journal of Materials Research
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    • v.25 no.12
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    • pp.694-702
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    • 2015
  • Nd-Fe-B permanent magnets have been used in a wide variety of applications because of their high magnetic flux density. So, demand for neodymium has been increasing in worldwide. In this study, an electrowinning process was performed in $LiF-NdF_3-Nd_2O_3$ high temperature molten salts. However, a corrosion resistant material for use in the molten salt must be found for stable operation because of the harsh corrosion environment of the electrowinning process. Therefore, for this paper, boron nitride(BN), aluminum nitride(AlN), and silicon nitride($Si_3N_4$) were selected as protective and structural materials in the high temperature electrolyte. To investigate the characteristics of BN, AlN, and $Si_3N_4$, in molten salts, materials were immersed in the molten salts for 24, 72, 120, and 192 hours. Also, surface condition and stability were investigated by SEM and EDS and corrosion products were calculated by HSC chemistry. As a result, among BN, AlN, and $Si_3N_4$, AlN was found to show the best protective material properties.

Effects of TiN and ZrN Coating on Surface Characteristics of Orthodontic Wire (교정용 와이어의 표면특성에 미치는 TiN 및 ZrN 코팅영향)

  • Kim, W.G.;Kim, D.Y.;Choe, H.C.
    • Journal of the Korean institute of surface engineering
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    • v.41 no.4
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    • pp.147-155
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    • 2008
  • The dental orthodontic wire provides a good combination of strength, corrosion resistance and moderate cost. The purpose of this study was to investigate the effects of TiN and ZrN coating on corrosion resistance and physical property of orthodontic wire using various instruments. Wires(round type and rectangular type) were used, respectively, for experiment. Ion plating was carried out for wire using Ti and Zr coating materials with nitrogen gas. Ion plated surface of each specimen was observed with field emission scanning electron microscopy(FE-SEM), energy dispersive X-ray spectroscopy(EDS), atomic force microscopy(AFM), vickers hardness tester, and electrochemical tester. The surface of TiN and ZrN coated wire was more smooth than that of other kinds of non-coated wire. TiN and ZrN coated surface showed higher hardness than that of non-coated surface. The corrosion potential of the TiN coated wire was comparatively high. The current density of TiN coated wire was smaller than that of non-coated wire in 0.9% NaCl solution. Pit nucleated at scratch of wire. The pitting corrosion resistance $|E_{pit}-E_{rep}|$ increased in the order of ZrN coated(300 mV), TiN coated(120 mV) and non-coated wire(0 mV).

Morphology of Bone-like Apatite Formation on Sr and Si-doped Hydroxyapatite Surface of Ti-6Al-4V Alloy after Plasma Electrolytic Oxidation

  • Yu, Ji-Min;Choe, Han-Cheol
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2017.05a
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    • pp.79-79
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    • 2017
  • Metallic biomaterials have been mainly used for the fabrication of medical devices for the replacement of hard tissue such as artificial hip joints, bone plates, and dental implants. Because they are very reliable on the viewpoint of mechanical performance. This trend is expected to continue. Especially, Ti and Ti alloys are bioinert. So, they do not chemically bond to the bone, whereas they physically bond with bone tissue. For their poor surface biocompatibility, the surface of Ti alloys has to be modified to improve the surface osteoinductivity. Recently, ceramic-like coatings on titanium, produced by plasma electrolytic oxidation (PEO), have been developed with calciumand phosphorus-enriched surfaces. A lso included the influences of coatings, which can accelerate healing and cell integration, as well as improve tribological properties. However, the adhesions of these coatings to the Ti surface need to be improved for clinical use. Particularly Silicon (Si) has been found to be essential for normal bone, cartilage growth and development. This hydroxyapatite, modified with the inclusion of small concentrations of silicon has been demonstrating to improve the osteoblast proliferation and the bone extracellular matrix production. Strontium-containing hydroxyapatite (Sr-HA) was designed as a filling material to improve the biocompatibility of bone cement. In vitro, the presence of strontium in the coating enhances osteoblast activity and differentiation, whereas it inhibits osteoclast production and proliferation. The objective of this work was to study Morphology of bone-like apatite formation on Sr and Si-doped hydroxyapatite surface of Ti-6Al-4V alloy after plasma electrolytic oxidation. Anodized alloys was prepared at 270V~300V voltages with various concentrations of Si and Sr ions. Bone-like apatite formation was carried out in SBF solution. The morphology of PEO, phase and composition of oxide surface of Ti-6Al-4V alloys were examined by FE-SEM, EDS, and XRD.

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Bone-like Apatite Formation on Ultrafine-Structure in Modified Electrolytic Solution

  • Jang, Jae-Myung;Choe, Han-Cheol
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2017.05a
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    • pp.155-155
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    • 2017
  • Surface modifications are commonly utilized to adjust the properties of the titanium and its alloy surface to the specific needs of the medical applications, but there are disadvantages such as poor osteoconductive properties and low adhesion of bone cell to implant surface. In order to improve these disadvantages, changes in surface properties have an important effect on osseointegration during implantation. In this paper we applied new technological method for improving a unique surface modification using the characteristic of an electrolytic Solution. Thus, in the electrolyte containing NaF in Na2SO4, TiO2 nanoporous was uniformly formed, and HAp nanoparticles were electrodeposited around the TiO2 nanopores, but in the electrolyte containing NH4F in (NH4)H2PO4, the coarse protrusions including HAp nano particles were regularly deposited onto the TiO2 barrier layer. The surface characteristics and the distributed elements and have been investigated by EDS analysis, and ultra-fine structure of surface are carried out using FE-SEM. To investigate the behavior of the anion, the analysis of chemical states was performed by XPS, and the narrow spectrums for Ti2P, Ca 2p, and P 2p seems to be almost similar depending on the characteristics of the electrolyte solution respectively. In addition, Ca 2p spectrum could be resolved into two peaks for Ca 2p3/2 and 2p1/2 at 347.4 and 351.3 eV, which are related to hydroxyapatite. And, the P peak can also be deconvoluted into two peaks for P1/2 and P3/2 levels with binding energy 134.2 and 133.4 eV, respectively. From the result of soaking test, the apatite morphologys were well-formed onto the modified surface according to the different conditions.

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Bone-like Apatite Formation on Ti-6Al-4V in Solution Containing Mn, Mg, and Si Ions after Plasma Electrolytic Oxidation in the SBF Solution

  • Lim, Sang-Gyu;Choe, Han Cheol
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2017.05a
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    • pp.157-157
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    • 2017
  • Titanium and its alloys that have a good biocompatibility, corrosion resistance, and mechanical properties such as hardness and wear resistance are widely used in dental and orthopedic implant applications. They can directly connect to bone. However, they do not form a chemical bond with bone tissue. Plasma electrolytic oxidation (PEO) that combines the high voltage spark and electrochemical oxidation is a novel method to form ceramic coatings on light metals such as titanium and its alloys. This is an excellent reproducibility and economical, because the size and shape control of the nano-structure is relatively easy. Silicon (Si), manganese (Mn), and magnesium (Mg) has a useful to bone. Particularly, Si has been found to be essential for normal bone, cartilage growth and development. Manganese influences regulation of bone remodeling because its low content in body is connected with the rise of the concentration of calcium, phosphates and phosphatase out of cells. Insufficience of Mn in human body is probably contributing cause of osteoporosis. Pre-studies have shown that Mg plays very important roles in essential for normal growth and metabolism of skeletal tissue in vertebrates and can be detected as minor constituents in teeth and bone. The objective of this work was to study nucleation and growth of bone-like apatite formation on Ti-6Al-4V in solution containing Mn, Mg, and Si ions after plasma electrolytic oxidation. Anodized alloys was prepared at 270V~300V voltages. And bone-like apatite formation was carried out in SBF solution for 1, 3, 5, and 7 days. The morphologies of PEO-treated Ti-6Al-4V alloy in containing Mn, Mg, and Si ions were examined by FE-SEM, EDS, and XRD.

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Corrosion Behavior of Si,Zn and Mn-doped Hydroxyapatite on the PEO-treated Surface

  • Park, Min-Gyu;Choe, Han-Cheol
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2017.05a
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    • pp.78-78
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    • 2017
  • Pure Titanium and alloy have been widely used in dental implants and orthopedics due to their excellent mechanical properties, biocompatibility and corrosion resistance. However, due to the biologically inactive nature of Ti metal implants, it cannot bind to the living bone immediately after transplantation into the body. In order to improve the bone bonding ability of titanium implants, many attempts have been made to alter the structure, composition and chemical properties of titanium surfaces, including the deposition of bioactive coatings. The PEO method has the advantages of short experiment time and low cost. These advantages have attracted attention recently. Recently, many metal ions such as silicon, magnesium, zinc, strontium, and manganese have received attention in this field due to their impact on bone regeneration. Silicon (Si) in particular has been found to be essential for normal bone and cartilage growth and development. Zinc (Zn) plays very important roles in bone formation and immune system regulation and promotes bone metabolism and growth. Manganese (Mn) is an essential trace metal found in all tissues and is required for normal amino acid, lipid, protein and carbohydrate metabolism. The objective of this work was research on the corrosion behavior of Si, Zn and Mn-doped hydroxyapatite on the PEO-treated surface. Anodized alloys was prepared at 270V~300V voltage in the solution containig Zn, Si, and Mn ions. Ion release test was carried out using potentidynamic and AC impedance method in 0.9% NaCl solution. The surface characteristics of PEO treated Ti-6Al-4V alloy were investigated using XRD, FE-SEM, AFM and EDS.

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Bone-like Apatite Morphology on Si-Zn-Mn-hydroxyapatite Coating on Ti-6Al-4V Alloy by Plasma Electrolytic Oxidation

  • Park, Min-Gyu;Choe, Han-Cheol
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2017.05a
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    • pp.158-158
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    • 2017
  • Titanium and its alloys have been used in the field dental and orthopedic implants because of their excellent mechanical properties and biocompatibility. Despite these attractive properties, their passive films were somewhat bioinert in nature so that sufficient adhesion of bone cells to implant surface was delayed after surgical treatment. Recently, plasma electrolyte oxidation (PEO) of titanium metal has attracted a great deal of attention is a comparatively convenient and effective technique and good adhesion to substrates and it enhances wear and corrosion resistances and produces thick, hard, and strong oxide coatings. Silicon(Si), Zinc(Zn), and Manganese(Mn) have a beneficial effect on bone. Si in particular has been found to be essential for normal bone and cartilage growth and development. And, Zn has been shown to be responsible for variations in body weight, bone length and bone biomechanical properties. Also, Mn influences regulation of bone remodeling because its low content in body is connected with the rise of the concentration of calcium, phosphates and phosphatase out of cells. The objective of this work was research on bone-like apatite morphology on Si-Zn-Mn-hydroxyapatite coating on Ti-6Al-4V alloy by plasma electrolytic oxidation. Anodized alloys were prepared at 280V voltage in the solution containing Si, Zn, and Mn ions. The surface characteristics of PEO treated Ti-6Al-4V alloy were investigated using XRD, FE-SEM, and EDS.

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Si and Mg Coatings on the Hydroxyapatite Film Formed Ti-29Nb-xHf Alloys by Plasma Electrolyte Oxidation

  • Park, Seon-Yeong;Choe, Han-Cheol
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2017.05a
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    • pp.152-152
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    • 2017
  • Titanium and its alloys have been widely used for biomedical applications. However, the use of the Ti-6Al-4V alloy in biomaterial is then a subject of controversy because aluminum ions and vanadium oxide have potential detrimental influence on the human body due to vanadium and aluminum. Hence, recent works showed that the synthesis of new Ti-based alloys for implant application involves more biocompatible metallic alloying element,such as, Nb, Hf, Zr and Mo. In particular, Nb and Hf are one of the most effective Ti ${\beta}$-stabilizer and reducing the elastic modulus. Plasma electrolyte oxidation (PEO) is known as excellent method in the biocompatibility of biomaterial due to quickly coating time and controlled coating condition. The anodized oxide layer and diameter modulation of Ti alloys can be obtained function of improvement of cell adhesion. Silicon (Si) and magnesium (Mg) has a beneficial effect on bone. Si in particular has been found to be essential for normal bone and cartilage growth and development. In vitro studies have shown that Mg plays very important roles in essential for normal growth and metabolism of skeletal tissue in vertebrates and can be detected as minor constituents in teeth and bone. Therefore, in this study, Si and Mg coatings on the hydroxyapatite film formed Ti-29Nb-xHf alloys by plasma electrolyte oxidation has been investigated using several experimental techniques. Ti-29Nb-xHf (x= 0, 3, 7 and 15wt%, mass fraction) alloys were prepared Ti-29Nb-xHf alloys of containing Hf up from 0 wt% to 15 wt% were melted by using a vacuum furnace. Ti-29Nb-xHf alloys were homogenized for 2 hr at $1050^{\circ}C$. The electrolyte was Si and Mg ions containing calcium acetate monohydrate + calcium glycerophosphate at room temperature. The microstructure, phase and composition of Si and Mg coated oxide surface of Ti-29Nb-xHf alloys were examined by FE-SEM, EDS, and XRD.

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Electrochemical characteristics of Ca, P, Sr, and Si Ions from PEO-treated Ti-6Al-4V Alloy Surface

  • Yu, Ji-Min;Choe, Han-Cheol
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2017.05a
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    • pp.154-154
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    • 2017
  • Ti-6Al-4V alloys are widely used as metal-lic biomaterials in dentistry and orthopedics due to its excellent biocompatibility and me-chanical properties. However, because of low biological activity, it is difficult to form bone growth directly on the surface of titanium implants. For this reason, surface treatment of plasma electrolytic oxidation(PEO) was used for dental implants. To enhance bioac-tivity on the surface, strontium(Sr) and sili-con(Si) ions can be added to PEO treated sur-face in the electrolyte containing these ions. The presence of Sr in the coating enhances osteoblast activity and differentiation, where-as it inhibits osteoclast production and prolif-eration. And Si has been found to be essen-tial for normal bone, cartilage growth, and development. In this study, electrochemical characteristics of Ca, P, Sr, and Si ions from PEO-treated Ti-6Al-4V alloy surface was re-searched using various experimental instruments. DC power is used and Ti-6Al-4V al-loy was subjected to a voltage of 280 V for 3 minutes in the electrolyte containing 5, 10, 20M% Sr ion and 5M% Si ion. The morphol-ogies of PEO-treated Ti-6Al-4V alloy by electrochemical anodization were examined by field-emission scanning electron micro-scopes (FE-SEM), energy dispersive x-ray spectroscopy (EDS), x-ray diffraction (XRD) and corrosion analysis using AC impedance and potentiodynamic polarization test in 0.9% NaCl solution at similar body tempera-ture using a potentiostat with a scan rate of 1.67mV/s and potential range from -1500mV to + 2000mV.

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Formation of Bioactive Surface by PEO-treatment after 2nd ATO Technique of Ti-6Al-4V Alloy (Ti-6Al-4V 합금에 2nd ATO 처리 후 플라즈마 전해 산화법에 의한 생체활성표면형성)

  • Lim, Sang-Gyu;Cho, Han-Cheol
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2018.06a
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    • pp.74-74
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    • 2018
  • Ti-6Al-4V alloys have been widely used as orthopedic materials because of their excellent corrosion resistance and mechanical properties. However, it does not bind directly to the bone, so it requires a surface modification. This problem can be solved by nanotube and micropore formation. Plasma electrolytic oxidation (PEO) treatment for micropore, which combines high-voltage spark and electrochemical oxidation, is a new way of forming a ceramic coating on light metals such as titanium and its alloys. This method has excellent reproducibility and can easily control the shape and size of the Ti alloy. In this study, formation of bioactive surface by PEO-treatment after $2^{nd}$ ATO technique of Ti-6Al-4V alloy was invesgated by various instrument. Nanotube oxide surface structure was formed on the surface by anodic oxidation treatment in 0.8 wt.% NaF and 1M $H_3PO_4$ electrolytes. After nanotube formation, nanotube layer was removed by ultrasonic cleaning. PEO-treatment was carried out at 280V for 3 minutes in the electrolytic solution containing the bioactive substance (Mg, Zn, Mn, Sr, and Si). The surface of Ti-6Al-4V alloy was observed by field emission scanning electron microscopy (FE-SEM, S-4800 Hitachi, Japan). An energy dispersive X-ray spectrometer (EDS, Inca program, Oxford, UK) was used to analyze the spectra of physiologically active Si, Mn, Mg, Zn, and Sr ions. The PEO film formed on the Ti-6Al-4V alloy surface was characterized using an X-ray diffractometer (TF-XRD, X'pert Philips, Netherlands). It is confirmed that bioactive ions play an essential role in the normal bone growth and metabolism of the human skeletal tissues.

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