• Title/Summary/Keyword: XPS analysis

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The Evaluation of the atomic composition and the surface roughness of Titanium Implants following Various Laser treatment with air-powder abrasive (레이저 처리후 임프란트 표면 변화에 관한 연구)

  • Kim, Tae-Jung;Lim, Sung-Bin;Chung, Chin-Hyung
    • Journal of Periodontal and Implant Science
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    • v.32 no.3
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    • pp.615-630
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    • 2002
  • Various long-term studies have shown that titanium implants as abutments for different types of prostheses have become a predictable adjunct in the treatment of partially or fully edentulous patients. The continuous exposure of dental implants to the oral cavity with all its possible contaminants creates a problem. A lack of attachment, together with or caused by bacterial insult, may lead to peri-implantitis and eventual implant failure. Removal of plaque and calculus deposits from dental titanium implants with procedures and instruments originally made for cleaning natural teeth or roots may cause major alterations of the delicate titanium oxide layer. Therefore, the ultimate goal of a cleaning procedure should be to remove the contaminants and restore the elemental composition of the surface oxide without changing the surface topography and harming the surrounding tissues. Among many chemical and mechanical procedure, air-powder abrasive have been known to be most effective for cleaning and detoxification of implant surface. Most of published studies show that the dental laser may be useful in the treatment of pen-implantitis. $CO_2$ laser and Soft Diode laser were reported to kill bacteria of implant surface. The purpose of this study was to obtain clinical guide by application these laser to implant surface by means of Non-contact Surface profilometer and X-ray photoelectron spectroscopy(XPS) with respect to surface roughness and atomic composition. Experimental rough pure titanium cylinder models were fabricated. All of them was air-powder abraded for 1 minute and they were named control group. And then, the $CO_2$ laser treatment under dry, hydrogen peroxide and wet condition or the Soft Diode laser treatment under Toluidine blue O solution condition was performed on the each of the control models. The results were as follows: 1. Mean Surface roughness(Ra) of all experimental group was decreased than that of control group. But it wasn't statistically significant. 2. XPS analysis showed that in the all experimental group, titanium level were decreased, when compared with control group. 3. XPS analysis showed that the level of oxygen in the experimental group 1, 3($CO_2$ laser treatment under dry and wet condition) and 4(Soft Diode laser was used under toluidine blue O solution) were decreased, when compared with control group. 4. XPS analysis showed that the atomic composition of experimental group 2($CO_2$ laser treatment under hydrogen peroxide) was to be closest to that of control group than the other experimental group. From the result of this study, this may be concluded. Following air-powder abrasive treatment, the $CO_2$ laser in safe d-pulse mode and the Soft Diode laser used with photosensitizer would not change rough titanium surface roughness. Especially, $CO_2$ laser treatment under hydrogen peroxide gave the best results from elemental points of view, and can be used safely to treat peri-implantitis.

Development of novel oxyfluoride glasses and glass ceramics for photoluminescence material by a containerless processing (무용기 용융법을 활용한 형광소재용 결정화 유리 개발)

  • Hyerin Jo;Minsung Hwang;Youngjin Lee;Jaeyeop Chung
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.33 no.5
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    • pp.181-186
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    • 2023
  • In this study, novel Eu2O3-BaF2-La2O3-B2O3 oxyfluoride glasses and glass ceramics were developed by a containerless processing. Differential thermal analysis (DTA) analysis was performed to analyze the thermophysical properties of oxyfluoride glasses doped with Eu2O3, and photoluminescence (PL) characteristics were analyzed to evaluate the luminous efficiency depending on the degree of crystallinity. The glass transition temperature decreased with increasing BaF2 concentration since BaF2 acts as a network modifier in this glass system. In addition, thermal stability which can be estimated by the difference between the glass transition temperature and the onset temperature of the crystallization decreased with increasing BaF2 contents. The peak related to the BaF2 crystal was confirmed after the crystallization by X-ray Diffraction (XRD) analysis. Photoluminescence intensity increased after the crystallization which indicates that the Eu3+ ions are sited in BaF2 crystal. La 3d5/2 x-ray photoelectron spectroscopy (XPS) and F1s XPS spectra were analyzed to precisely understand the behavior of the fluorine ion in the glass structure. Fluorine tends to bond with the network modifying cations such as La3+ and Ba2+ ions and after the crystallization the La-F bonds decreased because F- ions used to form BaF2 crystals.

Damages of Etched (Ba, Sr) $TiO_3$Thin Films by Inductively Coupled Plasmas (유도결합 플라즈마에 의한 (Ba,Sr)$TiO_3$박막의 식각 손상에 관한 연구)

  • 최성기;김창일;장의구
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.14 no.10
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    • pp.785-791
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    • 2001
  • High dielectric (Ba, Sr) TiO$_3$ thin films were etched in an inductively coupled plasma (ICP) as a function of Cl$_2$/Ar mixing ration. Under Cl$_2$(20)/Ar(80), the maximum etch rate of the BST films was 400 $\AA$/mim and selectivities of BST to Pt and PR were obtained 0.4 and 0.2, respectively. Etching products were redeposited on the surface of BST and resulted in varying the nature of crystallinity. Therefore, we investigated the etched surface of BST by x-ray photoelectron spectroscopy (XPS) atomic force microscopy (AFM) and x-ray diffraction (XRD). From the result of XPS analysis, we found that residues of Ba-Cl and Ti-Cl bonds remained on the surface of the etched BST for high boiling point. The morphology of the etched surfact was analyzed by AFM. A smoothsurface(roughness ~2.8nm) ws observed under Cl$_2$(20)/Ar(80), rf power of 600 W, dc bias voltage of -250 V and pressure of 10 mTorr. This changed the nature of the crystallinity of BST. From the result of XRD analysis, the crystallinities of the etched BST film under Ar only and Cl$_2$(20)/Ar(80) were maintained as similar to as-deposited BST. However, intensity of BST(100) orientation under Cl$_2$ only plasma was abruptly decreased. This indicated that CI compounds were redeposited on the etched BST surface and resulted in changed of the crystallinity of BST during the etch process.

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Structural Properties of Ammoniated Thin Cr Films with Oxygen Incorporated During Deposition (산소가 혼입된 Cr 박막의 질화처리에 따른 구조적 특성)

  • Kim, Jun;Byun, Changsob;Kim, Seontai
    • Korean Journal of Materials Research
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    • v.24 no.4
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    • pp.194-200
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    • 2014
  • Metallic Cr film coatings of $1.2{\mu}m$ thickness were prepared by DC magnetron sputter deposition method on c-plane sapphire substrates. The thin Cr films were ammoniated during horizontal furnace thermal annealing for 10-240 min in $NH_3$ gas flow conditions between 400 and $900^{\circ}C$. After annealing, changes in the crystal phase and chemical constituents of the films were characterized using X-ray diffraction (XRD) and energy dispersive X-ray photoelectron spectroscopy (XPS) surface analysis. Nitridation of the metallic Cr films begins at $500^{\circ}C$ and with further increases in annealing temperature not only chromium nitrides ($Cr_2N$ and CrN) but also chromium oxide ($Cr_2O_3$) was detected. The oxygen in the films originated from contamination during the film formation. With further increase of temperature above $800^{\circ}C$, the nitrogen species were sufficiently supplied to the film's surface and transformed to the single-phase of CrN. However, the CrN phase was only available in a very small process window owing to the oxygen contamination during the sputter deposition. From the XPS analysis, the atomic concentration of oxygen in the as-deposited film was about 40 at% and decreased to the value of 15 at% with increase in annealing temperature up to $900^{\circ}C$, while the nitrogen concentration was increased to 42 at%.

Surface Characterization of Anodized and Hydrothermal Treated Niobium Metal (양극산화와 열수처리한 니오비움 금속의 표면특성)

  • Won Dae-Hee;Kim Young-Soon;Yoon Dong-Joo;Lee Min-Ho;Bae Tae-Sung
    • Korean Journal of Materials Research
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    • v.15 no.2
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    • pp.134-138
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    • 2005
  • This study was performed to investigate the surface properties of electrochemically oxidized pure niobium by anodic oxide and hydrothermal treatment technique. Niobium specimens of $10mm\times10mm\times1.0mm$ in dimension were polished sequentially from $\#600,\;\#800,\;\#1000$ emery paper. The surface of pure niobium sperimens was anodized in an electrolytic solution that was dissolved calcium and phosphate in water. The electrolytic voltage was set in the range of 250 V and the current density was $10mA/cm^2$. The specimen was hydrothermal treated in high-pressure steam at $300^{\circ}C$ for 2 hours using an autoclave. And all specimens were immersed in the in the Hanks' solution nth pH 7.4 at $37^{\circ}C$ for 30 days. The surface of specimen was characterized by surface roughness, scanning electron microscope(SEM), energy dispersion X-ray analysis(EDX), X-ray photoemission spectroscopy(XPS) test. The value of surface roughness was the highest in the anodized sample and $0.41{\pm}0.04\;{\mu}m$. The results of the SEM observation show that oxide layers of the multi porosity in the anodized sample were piled up on another, and hydroxyapatite crystal was precipitate from the surface of the hydrothermal treated sample. In the XPS analysis, O, Nb, C peak and small amounts of N peak were found in the polished specimens while Ca and P peak in addition to O, Nb, C and peak were observed in the hydrothermal treated sample.

The Study on the Etching Characteristics of (Ba, Sr)TiO$_3$ Film by Inductively Coupled Plasma (유도결합 플라즈마에 의한(Ba, Sr)TiO$_3$ 박막의 식각 특성 연구)

  • 김승범;이영준;염근영;김창일
    • Journal of the Korean Institute of Telematics and Electronics D
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    • v.36D no.4
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    • pp.56-62
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    • 1999
  • In this study, (Ba, Sr)$TiO_3$ thin films were etched with $Cl_2$/Ar gas mixing ratio in an inductively coupled plasma (ICP) by varying the etching parameter such as rf power, dc bias voltage, and chamber pressure. The etch rate was 56 nm/min under $Cl_2$/($Cl_2$+Ar) gas mixing ratio of 0.2, rf power of 600 W, dc bias voltage of 250 V, and chamber pressure of 5 mTorr. At this time, the selectivity of BST to Pt, $SiO_2$ was respectively 0.52, 0.43. The surface reaction of the etched (Ba, Sr)$TiO_3$ thin films was investigated with X-ray photoelectron spectroscopy (XPS). Ba is removed by chemical reaction between Sr and Cl to remove Sr. Ti is removed by chemical reaction such as $TiCl_4$ with ease. The results of secondary ion mass spectrometer (SIMS) analysis compared with the results of XPS analysis and the results were the same.

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X-RAY PHOTOELECTRON SPECTOSCOPIC ANALYSIS OF ALUMINUM COMPOUND ADSORBED ON PULP FIBER SURFACES

  • Takuya Kitaoka;Hiroo Tanaka
    • Proceedings of the Korea Technical Association of the Pulp and Paper Industry Conference
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    • 1999.04b
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    • pp.239-244
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    • 1999
  • aluminum sulfate (alum) as a representative retention aid in papermaking processes was added to pulp suspensions, and the aluminum components adsorbed on the pulp were investigated quantitatively by two types of X-ray elementary analyses with regard to simultaneous changes of their surface charges. X-ray photoelectron spectroscopy (XPS) and X-ray fluorescence analysis (XFA) were applied to determine the aluminum components retained in pulp pads up to ca. 10 nm and 100${\mu}$m depth, respectively. In other words, XPS was utilized to analyze the outermost surface layers of the samples, and XFA was available for measurement of their extensive regions. A particle charge detector (PCD) was used to monitor streaming potentials at various pHs of the pulp mixtures under moderate sharing conditions. At pH 4.5 of pulp suspensions containing alum, surface charges of pulp fibers varied from negative to slight negative (approximately neutral) according to adsorption of aluminum components onto the pulp fibers. Subsequently, when a dilute NaOH solution in limited amounts was added to pulp mixtures, both streaming potentials and surface aluminum content of the pulp fibers increased distinctly although little total aluminum retention increased. Further addition of alkali solutions brought drastic decreases of the surface charges and surface aluminum content, while total aluminum content, on the contrary, increased gradually under neutral conditions. These results indicate that residual aluminum ions remained in pulp suspensions are predominantly adsorbed on surfaces of pulp fibers by adequate alkali additions and they must sufficiently cationize the fiber surfaces with increases of somewhat cationic aluminum complexes formed on the surfaces. On the other hand, aluminum components formed in higher pH ranges have nearly no contribution to improvement of charge properties of the pulp fiber surfaces, even though aluminum retention in pulp pads increases. XPS and XFA analyses combined with streaming potential measurement using a PCD suggest close relationships between aluminum content on the pulp fiber surfaces and their charge properties.

Etching Mechanism of $YMnO_3$ Thin Films in High Density $CF_4$/Ar Plasma ($CF_4$/Ar 가스 플라즈마를 이용한 $YMnO_3$ 박막의 식각 반응연구)

  • 김동표;김창일;이철인
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.14 no.12
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    • pp.959-964
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    • 2001
  • We investigated the etching characteristics of YMnO$_3$ thin films in high-density plasma etching system. In this study, YMnO$_3$ thin films were etched with CF$_4$/Ar gas chemistries in inductively coupled plasma(ICP). Etch rates of YMnO$_3$ increased up to 20% CF$_4$ in CF$_4$/(CF$_4$+Ar), but decreased with furthermore increasing CF$_4$ in CF$_4$/(CF$_4$+Ar). In optical emission spectroscopy (OES) analysis, F radical and Ar* ions in plasma at various gas chemistries decreased with increasing CF$_4$ content. Chemical states of YMnO$_3$ films exposed in plasma were investigated with x-ray photoelectron spectroscopy (XPS) and secondary ion mass spectrometry (SIMS). There is a chemical reaction between metal (Y, Mn) and F and metal-fluorides were removed effectively by Ar ion sputtering. YF$_{x}$, MnF$_{x}$ such as YF, YF$_2$, YF$_3$ and MnF$_3$ were detected using SIMS analysis. The etch slope is about 65$^{\circ}$ and cleasn surface. surface of the etched YMnO$_3$ thin films was investigated with X-ray photoelectron spectroscopy (XPS) and secondary ion mass spectrometry (SIMS). The etch profile was also investigated by scanning electron microscopy (SEM).EM).

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Etching characteristics of gold thin films using inductively coupled Ar/$CF_4/Cl_2$ plasma (Ar/$CF_4/Cl_2$ 유도 결합 플라즈마에 의한 gold 박막의 식각특성)

  • Kim, Nam-Kyu;Chang, Yun-Seong;Kim, Dong-Pyo;Kim, Chang-Il;Chang, Eui-Goo;Lee, Byeong-Ki
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2002.11a
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    • pp.190-194
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    • 2002
  • In this study, the etching of Au thin films have been performed in an inductively coupled CF4/Cl2/Ar plasma. The etch properties were measured as the CF4 adds from 0 % to 30 % to the Cl2/(Cl2 + Ar) gas mixing ratio of 0.2. Other parameters were fixed at a rf power of 700 W, a dc bias voltage of 150 V, a chamber pressure of 15 mTorr, and a substrate temperature of $30^{\circ}C$. The highest etch rate of the Au thin film was 370 nm/min at a 10 % additive CF4 into Cl2/(Cl2 + Ar) gas mixing ratio of 0.2. The surface reaction of the etched Au thin films was investigated using x-ray photoelectron spectroscopy (XPS) analysis. From x-ray photoelectron spectroscopy (XPS) analysis, the intensities of Au peaks are changed. There is a chemical reaction between Cl and Au. Au-Cl is hard to remove on the surface because of its high melting point and the etching products can be sputtered by Ar ion bombardment. We obtained the cleaned and steep profile.

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Surface Characterization of Poly(vinylidene fluoride) and Poly(methyl methacrylate) Blend Coatings Prepared by Dispersion Coating (분산코팅에 의해 형성된 Poly(vinylidene fluoride)와 Poly(methyl methacrylate) 블렌드 코팅층의 표면 특성)

  • Seok, Kwang Hee;Ha, Jong-Wook;Lee, Soo-Bok;Park, In Jun;Kim, Hyung Joong
    • Polymer(Korea)
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    • v.37 no.2
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    • pp.177-183
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    • 2013
  • Surface properties such as morphology, crystalline structure, and chemical composition of poly(vinylidene fluoride) (PVDF)/poly(methyl methacrylate) (PMMA) blend coatings prepared by dispersion coating on poly(ethylene terephthalate) (PET) film have been investigated. It was observed that the surface properties were greatly influenced by the coating temperature and blend composition according to SEM, ATR-FTIR and XPS analysis. The typical surface morphology of ${\alpha}$-crystalline structure of PVDF could be observed when the coating temperature was lower than $120^{\circ}C$ or the amount of PVDF was higher than 80 wt% in the blend. Otherwise, the crystalline structure was changed from ${\alpha}$-crystal to ${\gamma}$-crystal or amorphous state. Based on the XPS analysis, the surface segregation of PVDF chains in the blend coating was confirmed.