• Journal of Radiation Industry
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• v.3 no.1
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• pp.7-11
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• 2009

Hard magnet was usually used by coating $SiO_2$ ceramic thick films followed by the thermal annealing process. In this work, the alternative annealing process for NdFeB magnets using e-beam sources (1~2 MeV, 50~400 kGy) was investigated. NdFeB magnets was coated with ceramic thick films using the spray method. The optimal annealing parameter for e-beam source reveals to be 1 MeV and 300 kGy. The sample prepared at 1 MeV and 300 kGy was characterized by the analysis of the surface morphology, film hardness, adhesion and chemical stability. The mechanical property of thick film, especially film hardness, is better than that of thermal annealed samples at $180^{\circ}C$. As a result, e-beam annealing process will be one of candidate and attractive heat treatment process. In future, manufacturing process will be carried out in cooperation with the magnet company.

• Corrosion Science and Technology
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• v.5 no.1
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• pp.15-22
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• 2006

The introduction of two-grid inside a conventional process system produces a reactive coating deposition and increases metal ion ratio in the plasma, resulting in denser and smoother films. The corrosion behaviors of TiN coatings were investigated by electrochemical methods, such as potentiodynamic polarization test and electrochemical impedance spectroscopy (EIS) in deaerated 3.5% NaCl solution. Electrochemical tests were used to evaluate the effect of microstructure on the corrosion behavior of TiN coatings exposed to a corrosive environment. The crystal structure of the coatings was examined by X-ray diffractometry (XRD) and the microstructure of the coatings was investigated by scanning electron microscopy (SEM) and transmission electron spectroscopy (TEM). In the potentiodynamic polarization test and EIS measurement, the corrosion current density of TiN deposited by two grid-attached magnetron sputtering was lower than TiN deposited by conventional magnetron type and also presented higher Rct values during 240 h immersion time. It is attributed to the formation of a dense microstructure, which promotes the compactness of coatings and yields lower porosity.

• Journal of the Korean institute of surface engineering
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• v.49 no.6
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• pp.580-586
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• 2016

Cr-Si-Al-N coating with different Si content were deposited by hybrid physical vapor deposition (PVD) method consisting of unbalanced magnetron (UBM) sputtering and arc ion plating (AIP). The deposition temperature was $300^{\circ}C$, and the gas ratio of $Ar/N_2$ were 9:1. The CrSi alloy and aluminum targets used for arc ion plating and sputtering process, respectively. Si content of the CrSi alloy targets were varied with 1 at%, 5 at%, and 10 at%. The phase analysis, composition and microstructural analysis performed using x-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) including energy dispersive spectroscopy (EDS), respectively. All of the coatings grown with textured CrN phase (200) plane. The thickness of the Cr-Si-Al-N films were measured about $2{\mu}m$. The friction coefficient and removal rate of films were measured by a ball-on-disk test under 20N load. The friction coefficient of all samples were 0.6 ~ 0.8. Among all of the samples, the removal rate of CrSiAlN (10 at% Si) film shows the lowest values, $4.827{\times}10^{-12}mm^3/Nm$. As increasing of Si contents of the CrSiAlN coatings, the hardness and elastic modulus of CrSiAlN coatings were increased. The morphology and composition of wear track of the films was examined by scanning electron microscopy (SEM) and energy dispersive spectroscopy, respectively. The surface energy of the films were obtained by measuring of contact angle of water drop. Among all of the samples, the CrSiAlN (10 at% Si) films shows the highest value of the surface energy, 41 N/m.

• Proceedings of the Korean Vacuum Society Conference
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• 1999.07a
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• pp.211-211
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• 1999

Titanium nitride (TiN) thin films have useful properties including high hardness, good electrical conductivity, high melting point, and chemical inertness. The applications have included wear-resistant hard coatings on machine tools and bearings, decorative coating making use of the golden color, thermal control coatings for widows, and erosion resistant coatings for spacecraft plasma probes. For all these applications as feature sizes shrink and aspect ratios grow, the issue of good step coverage becomes increasingly important. It is therefore essential to manufacture conformal coatings of TiN. The growth of TiN thin films by chemical vapor deposition (CVD) is of great interest for achieving conformal deposition. The most widely used precursor for TiN is TiCl4 and NH3. However, chlorine impurity in the as-grown films and relatively high deposition temperature (>$600^{\circ}C$) are considered major drawbacks from actual device fabrication. To overcome these problems, recently, MOCVD processes including plasma assisted have been suggested. In this study, therefore, we have doposited Ti(C, N) thin films on Si(100) and D2 steel substrates in the temperature range of 150-30$0^{\circ}C$ using tetrakis diethylamido titanium (TDEAT) and titanium isopropoxide (TIP) by pulsed DC plamsa enhanced metal-organic chemical vapor deposition (PEMOCVD) method. Polycrystalline Ti(C, N) thin films were successfully grown on either D2 steel or Si(100) surfaces at temperature as low as 15$0^{\circ}C$. Compositions of the as-grown films were determined with XPS and RBS. From XPS analysis, thin films of Ti(C, N) with low oxygen concentration were obtained. RBS data were also confirmed the changes of stoichiometry and microhardness of our films. Radical formation and ionization behaviors in plasma are analyzed by optical emission spectroscopy (OES) at various pulsed bias and gases conditions. H2 and He+H2 gases are used as carrier gases to compare plasma parameter and the effect of N2 and NH3 gases as reactive gas is also evaluated in reduction of C content of the films. In this study, we fond that He and H2 mixture gas is very effective in enhancing ionization of radicals, especially N resulting is high hardness. The higher hardness of film is obtained to be ca. 1700 HK 0.01 but it depends on gas species and bias voltage. The proper process is evident for H and N2 gas atmosphere and bias voltage of 600V. However, NH3 gas highly reduces formation of CN radical, thereby decreasing C content of Ti(C, N) thin films in a great deal. Compared to PVD TiN films, the Ti(C, N) film grown by PEMOCVD has very good conformability; the step coverage exceeds 85% with an aspect ratio of more than 3.

• Journal of the Semiconductor & Display Technology
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• v.2 no.1
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• pp.1-5
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• 2003

Plasma generator based on non-self-sustained low-pressure arc discharge has been examined as a tool for deposition of highly-adhesive hydrogenated amorphous diamond-like carbon(DLC) films. Since the discharge is stable in wide range of gas pressures and currents, this plasma source makes possible to realize both plasma-immersion ion implantation(PIII) and plasma-immersion ion deposition(PIID) in a unified vacuum cycle. The plasma parameters were measured as functions of discharge current. Discharge and substrate bias voltage parameters have been determined for the PIII and PIID modes. For PIID it has been demonstrated that hard and well-adherent DLC coating are produced at 200-500 eV energies per deposited carbon atom. The growth rates of DLC films in this case are about 200-300 nm/h. It was also shown that short(∼60$\mu\textrm{s}$) high-voltage(> 1kV) substrate bias pulses are the most favorable for achieving high hardness and good adhesion of DLC, as well as for reducing of residual intrinsic stress are.

• Proceedings of the Korean Vacuum Society Conference
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• 2012.02a
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• pp.96-97
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• 2012

In nitride and oxide film deposition, sputtered metals react with nitrogen or oxygen gas in a vacuum chamber to form metal nitride or oxide films on a substrate. The physical properties of sputtered films (metals, oxides, and nitrides) are strongly influenced by magnetron plasma density during the deposition process. Typical target power densities on the magnetron during the deposition process are ~ (5-30) W/cm2, which gives a relatively low plasma density. The main challenge in reactive sputtering is the ability to generate a stable, arc free discharge at high plasma densities. Arcs occur due to formation of an insulating layer on the target surface caused by the re-deposition effect. One current method of generating an arc free discharge is to use the commercially available Pinnacle Plus+ Pulsed DC plasma generator manufactured by Advanced Energy Inc. This plasma generator uses a positive voltage pulse between negative pulses to attract electrons and discharge the target surface, thus preventing arc formation. However, this method can only generate low density plasma and therefore cannot allow full control of film properties. Also, after long runs ~ (1-3) hours, depends on duty cycle the stability of the reactive process is reduced due to increased probability of arc formation. Between 1995 and 1999, a new way of magnetron sputtering called HIPIMS (highly ionized pulse impulse magnetron sputtering) was developed. The main idea of this approach is to apply short ${\sim}(50-100){\mu}s$ high power pulses with a target power densities during the pulse between ~ (1-3) kW/cm2. These high power pulses generate high-density magnetron plasma that can significantly improve and control film properties. From the beginning, HIPIMS method has been applied to reactive sputtering processes for deposition of conductive and nonconductive films. However, commercially available HIPIMS plasma generators have not been able to create a stable, arc-free discharge in most reactive magnetron sputtering processes. HIPIMS plasma generators have been successfully used in reactive sputtering of nitrides for hard coating applications and for Al2O3 films. But until now there has been no HIPIMS data presented on reactive sputtering in cluster tools for semiconductors and MEMs applications. In this presentation, a new method of generating an arc free discharge for reactive HIPIMS using the new Cyprium plasma generator from Zpulser LLC will be introduced. Data (or evidence) will be presented showing that arc formation in reactive HIPIMS can be controlled without applying a positive voltage pulse between high power pulses. Arc-free reactive HIPIMS processes for sputtering AlN, TiO2, TiN and Si3N4 on the Applied Materials ENDURA 200 mm cluster tool will be presented. A direct comparison of the properties of films sputtered with the Advanced Energy Pinnacle Plus + plasma generator and the Zpulser Cyprium plasma generator will be presented.

• 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.

• Journal of the Korean Ceramic Society
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• v.54 no.6
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• pp.511-517
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• 2017

With different working pressures and substrate biases, Cr-Al-N coatings were deposited by hybrid physical vapor deposition (PVD) method, consisting of unbalanced magnetron (UBM) sputtering and arc ion plating (AIP) processes. Cr and Al targets were used for the arc ion plating and the sputtering process, respectively. Phase analysis, and composition, binding energy, and microstructural analyses were performed using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and field emission scanning electron microscopy (FESEM), respectively. Surface droplet size of Cr-Al-N coatings was found to decrease with increasing substrate bias. A decrease of the deposition rate of Cr-Al-N films was expected due to the increase of substrate bias. The coatings were grown with textured CrN phase and (111), (200), and (220) planes. X-ray diffraction data show that all Cr-Al-N coatings shifted to lower diffraction angles due to the addition of Al. The XPS results were used to determine the $Cr_2N$, CrN, and (Cr,Al)N binding energies. The compositions of the Cr-Al-N films were measured by XPS to be Cr 23.2~36.9 at%, Al 30.1~40.3 at%, and N 31.3~38.6 at%.

• Korean Chemical Engineering Research
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• v.47 no.4
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• pp.430-435
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• 2009

Spiropyran-doped organic-inorganic hybrid coatings were prepared starting from glycidoxypropyl triethoxysilane and vinyltriethoxysilane by a sol-gel method. They were applied as a thin layer to polycarbonate sheets and their photochromic properties were investigated. The effect of polarity of solvents dissolving the spiropyran was investigated on the photochromic properties. The decoloration rate of the spiropyran decreased with increasing the polarity of solvents dissolving the spiropyran because the open form of the spiropyran was easily stabilized in the polar gel matrix.

• Proceedings of the Korean Vacuum Society Conference
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• 2011.02a
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• pp.335-335
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• 2011

Instability of a thin film attached to a compliant substrate often leads to emergence of exquisite wrinkle patterns with length scales that depend on the system geometry and applied stresses. However, the patterns that are created using the current techniques in polymer surface engineering, generally have low aspect ratio of undulation amplitude to wavelength, thus, limiting their application. Here, we present a novel and effective method that enables us to create wrinkles with a desired wavelength and high aspect ratio of amplitude over wavelength as large as to 2.5:1. First, we create buckle patterns with high aspect ratio of amplitude to wavelength by deposition of an amorphous carbon film on a surface of a soft polymer poly(dimethylsiloxane) (PDMS). Amorphous carbon films are used as a protective layer in structural systems and biomedical components, due to their low friction coefficient, strong wear resistance against, and high elastic modulus and hardness. The deposited carbon layer is generally under high residual compressive stresses (~1 GPa), making it susceptible to buckle delamination on a hard substrate (e.g. silicon or glass) and to wrinkle on a flexible or soft substrate. Then, we employ glancing angle deposition (GLAD) for deposition of a high aspect ratio patterns with amorphous carbon coating on a PDMS surface. Using this method, pattern amplitudes of several nm to submicron size can be achieved by varying the carbon deposition time, allowing us to harness patterned polymers substrates for variety of application. Specifically, we demonstrate a potential application of the high aspect wrinkles for changing the surface structures with low surface energy materials of amorphous carbon coatings, increasing the water wettability.