• 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.

• Korean Journal of Materials Research
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• v.20 no.12
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• pp.629-635
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• 2010

Abstract In this study characteristics of Al-doped ZnO thin film by HIPIMS (High power impulse sputtering) are discussed. Deposition speed of HIPIMS with conventional balanced magnetic field is measured at about 3 nm/min, which is 30% of that of conventional RF sputtering process with the same working pressure. To generate additional magnetic flux and increase sputtering speed, electromagnetic coil is mounted at the back side of target. Under unbalanced magnetic flux from electromagnet with 1.5A coil current, deposition speed of AZO thin film is increased from 3 nm/min to 4.4 nm/min. This new value originates from the decline of particles near target surface due to the local magnetic flux going toward substrate from electromagnet. AZO film sputtered by HIPIMS process shows very smooth and dense film surface for which surface roughness is measured from 0.4 nm to 1 nm. There are no voids or defects in morphology of AZO films with varying of magnetic field. When coil current is increased from 0A to 1A, transmittance of AZO thin film decreases from 80% to 77%. Specific resistance is measured at about $2.9{\times}10-2\Omega{\cdot}cm$. AZO film shows C-axis oriented structure and its grain size is calculated at about 5.3 nm, which is lower than grain size in conventional sputtering.

• Journal of the Korean institute of surface engineering
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• v.47 no.3
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• pp.109-115
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• 2014

High power impulse magnetron sputtering (HIPIMS), also known as the technology is called peak power density in a short period, you can get high, so high ionization sputtering rate can make. Higher ionization of sputtered species to a variety of coating materials conventional in the field of improving the characteristics and self-assisted ion thin film deposition process, which contributes to a superior being. HIPIMS at the same power, but the deposition speed is slow in comparison with DC disadvantages. Since recently as a replacement for HIPIMS modulated pulse power (MPP) has been developed. This ionization rate of the sputtered species can increase the deposition rate is lowered and at the same time to overcome the problems to be reported. The differences between the MPP and the HIPIMS is a simple single pulse with a HIPIMS whereas, MPP is 3 ms in pulse length is adjustable, with the full set of multi-pulses within the pulse period and the pulse is applied can be micro advantages. In this experiment, $In_2O_3$ : $SnO_2$ composition ratio of 9 : 1 wt% target was used, Ar : $O_2$ flow rate ratio is 4.8 to 13.0% of the rate of deposition was carried out at room temperature. Ar 40 sccm and the flow rate of $O_2$ and then fixed 2 ~ 6 sccm was compared against that. The thickness of the thin film deposition is fixed at 60 nm, when the partial pressure of oxygen at 9.1%, the specific resistance value of $4.565{\times}10^{-4}{\Omega}cm$, transmittance 86.6%, mobility $32.29cm^2/Vs$ to obtain the value.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2016.11a
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• pp.105-105
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• 2016

Recently, high power impulse magnetron sputtering (HIPIMS) has attracted considerable attentions due to its high potential for industrial applications. By pulsing the sputtering target with high power density and short duration pulses, a high plasma density and high ionization of the sputtered species can be obtained. HIPIMS has exhibited several merits such as increased coating density, good adhesion, microparticle-free and smooth surface, which make the HIPIMS technique desirable for synthesizing hard coatings. However, hard coatings present intrinsic defects (columnar structures, pinholes, pores, discontinuities) which can affect the corrosion behavior, especially when substrates are active alloys like steel or in a wear-corrosion process. Atomic layer deposition (ALD), a CVD derived method with a broad spectrum of applications, has shown great potential for corrosion protection of high-precision metallic parts or systems. In ALD deposition, the growth proceeds through cyclic repetition of self-limiting surface reactions, which leads to the thin films possess high quality, low defect density, uniformity, low-temperature processing and exquisite thickness control. These merits make ALD an ideal candidate for the fabrication of excellent oxide barrier layer which can block the pinhole and other defects left in the coating structure to improve the corrosion protection of hard coatings. In this work, CrN/Al2O3/CrN multilayered coatings were synthesized by a hybrid process of HIPIMS and ALD techniques, aiming to improve the CrN hard coating properties. The influence of the Al2O3 interlayer addition, the thickness and intercalation position of the Al2O3 layer in the coatings on the microstructure, surface roughness, mechanical properties and corrosion behaviors were investigated. The results indicated that the dense Al2O3 interlayer addition by ALD lead to a significant decrease of the average grain size and surface roughness and greatly improved the mechanical properties and corrosion resistance of the CrN coatings. The thickness increase of the Al2O3 layer and intercalation position change to near the coating surface resulted in improved mechanical properties and corrosion resistance. The mechanism can be explained by that the dense Al2O3 interlayer acted as an excellent barrier for dislocation motion and diffusion of the corrosive substance.

• Proceedings of the Korean Vacuum Society Conference
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• 2010.02a
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• pp.193-193
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• 2010

HIPIMS(High sputtering impulse magnetron sputtering)은 수십 ${\mu}s$의 짧은 pulse 동안 수kw의 매우 높은 파워를 인가할 수 있어 밀도 $10^{13}/cm^3$ 이상의 고밀도 플라즈마 방전이 가능하여 스퍼터된 타겟 이온들의 이온화율이 매우 높은 특징을 가진다. HIPIMS를 통해 증착한 박막의 경우 매우 치밀한 조직을 가지고 있어 기존 DC, Pulsed DC, RF 증착을 통한 박막에 비해 우수한 물성을 보여준다. 본 실험에서는 대면적의 고품위 Al:ZnO 박막을 증착하기위하여 HIPIMS 증착법을 사용하였다. 1000mm폭 타겟상에서 균일한 증착을 위하여 Balanced B-field, Unbalanced field를 각각 인가하여 실험하였다. 시뮬레이션을 통하여 타겟 중심부와 가장자리의 자기장을 결정하였으며, target edge에서의 증착율과 cathode erosion 방지를 위하여 원형 트랙형으로 보조 자석을 설치하였다. $Al_2O_3$(2wt%)가 첨가된 planar target을 사용하였고, power는 700 W~2 kW, 그리고 pulse 폭은 $50-150 {\mu}s$정도로 변화시켜 가면서 상온에서 증착하였다. 플라즈마 가스로는 Ar만을 사용하여 두께는 60-100 nm정도로 증착하였다. Plasma emission monitoring을 통해 측정한 결과 Balanced B-field 에 비해 Unbalanced B-field 조건 에서 스퍼터된 이온들의 균일도가 우수하였으며 증착된 박막의 균일도 또한 증가하였다.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2012.05a
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• pp.3-35
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• 2012

• Proceedings of the Korean Vacuum Society Conference
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• 2012.08a
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• pp.151-151
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• 2012

A new plasma process, i.e., the combination of PIII&D and HIPIMS, was developed to implant non-gaseous ions into materials surface. HIPIMS is a special mode of operation of pulsed-DC magnetron sputtering, in which high pulsed DC power exceeding ~1 kW/$cm^2$ of its peak power density is applied to the magnetron sputtering target while the average power density remains manageable to the cooling capacity of the equipment by using a very small duty ratio of operation. Due to the high peak power density applied to the sputtering target, a large fraction of sputtered atoms is ionized. If the negative high voltage pulse applied to the sample stage in PIII&D system is synchronized with the pulsed plasma of sputtered target material by HIPIMS operation, the implantation of non-gaseous ions can be successfully accomplished. The new process has great advantage that thin film deposition and non-gaseous ion implantation along with in-situ film modification can be achieved in a single plasma chamber. Even broader application areas of PIII&D technology are believed to be envisaged by this newly developed process. In one application of non-gaseous plasma immersion ion implantation, Ge ions were implanted into SiO2 thin film at 60 keV to form Ge quantum dots embedded in SiO2 dielectric material. The crystalline Ge quantum dots were shown to be 5~10 nm in size and well dispersed in SiO2 matrix. In another application, Ag ions were implanted into SS-304 substrate to endow the anti-microbial property of the surface. Yet another bio-application was Mg ion implantation into Ti to improve its osteointegration property for bone implants. Catalyst is another promising application field of nongaseous plasma immersion ion implantation because ion implantation results in atomically dispersed catalytic agents with high surface to volume ratio. Pt ions were implanted into the surface of Al2O3 catalytic supporter and its H2 generation property was measured for DME reforming catalyst. In this talk, a newly developed, non-gaseous plasma immersion ion implantation technique and its applications would be shown and discussed.

• Proceedings of the Korean Vacuum Society Conference
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• 2014.02a
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• pp.168.2-168.2
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• 2014

반사방지막 코팅(Anti-reflection coating)은 태양전지(Solar cell), 발광다이오드(LED) 등의 반사율을 낮추어 효율을 증대시키기 위하여 사용되고 있다. 본 실험에서는 유리 기판 위에 실리콘 타겟을 이용한 반응성 high power impulse magnetron sputtering (HIPIMS) 장비를 활용하여, 높은 공정 압력(High-pressure)에서 펄스폭(Pulse width)을 조절하여 $SiO_2$ 반사방지막 코팅층을 형성하였다. 또한, 기공이 더 많은 박막을 제작하기 위해 빗각증착(Oblique-angle deposition)을 적용하여 더 좋은 광학 특성을 갖는 반사방지막 코팅층을 형성하였다. UV-Vis spectrometer를 이용하여, 380~800 nm 파장에서 투과율(Transmittance)을 측정하여 비교, 분석하였다. Ellipsometer를 이용하여 $SiO_2$ 박막층의 굴절률(Refractive index)을 측정한 결과, 반사방지막 코팅층 내부 기공에 따라 다양한 굴절률을 가지는 것을 확인할 수 있었다. 또한, 코팅층 내부 기공의 형상을 확인하기 위해 SEM(Secondary electron microscopy)을 활용하여 코팅층 단면(Cross section)을 측정하였다. 이를 활용하여 낮은 굴절률을 갖는 반사방지용 $SiO_2$ 코팅층을 형성하여 태양전지의 광 변환 효율을 상승 시킬 수 있고, 발광다이오드의 광 추출 효율을 증가시킬 있을 것으로 여겨진다.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2016.11a
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• pp.102-102
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• 2016

본 연구에서는 직류 전원(direct current; DC)을 이용한 스퍼터링과 고전력펄스 마그네트론 스퍼터링(high-power impulse magentron sputtering; HIPIMS)의 두 가지 방법과 빗각 증착을 적용하여 제조한 티타늄 질화물(TiN) 박막의 미세구조 변화가 물성에 미치는 영향을 확인하였다. TiN 박막은 99.5%의 Ti 타겟을 사용하고, Ar가스와 $N_2$ 분위기에서 스테인리스(SUS304)와 초경(cdmented carbide; WC-10wt.%Co) 기판위에 코팅하였다. 기판은 알코올과 아세톤으로 초음파 세척을 실시한 후 진공용기에 장착하고 기본 진공도인 ${\sim}2.0{\times}10^{-5}Torr$ 까지 진공배기를 실시하였다. 기판과 타겟 간의 거리는 DC 스퍼터링은 10 cm, HIPIMS 스퍼터링은 8.5 cm 이었다. 진공용기의 압력이 기본 진공도까지 배기되면 Ar 가스를 ${\sim}10^{-2}Torr$로 주입한 후 기판에 라디오 주파수(radio frequency; RF) 전원으로 약 -800 V의 전압을 인가하여 글로우 방전을 발생시키고 약 30 분간 청정을 실시하였다. 기판의 청정이 끝난 후 기본 진공도까지 배기한 후 Ar와 $N_2$ 가스를 ${\sim}10^{-3}Torr$로 주입하여 TiN 코팅을 실시하였다. 빗각의 크기는 $45^{\circ}$와 $-45^{\circ}$이며, TiN 박막의 총 두께는 약 $2.5{\sim}4.0{\mu}m$ 로 유지하였다. 공정조건에 따라 TiN 박막의 주상정은 형태와 기울어진 각도가 다른 것을 확인하였다. DC 스퍼터링으로 제조된 TiN 박막은 기판홀더에 약 -100 V 의 bias 전압을 인가하면 인가하지 않은 박막에 비해 치밀한 박막의 성장과 경도 값도 증가하는 사실을 확인하였다. 또한 빗각을 적용하고 bias 전압을 인가하지 않은 시편에서 박리현상이 일어났다. HIPIMS로 제조한 TiN 박막은 bias 전압을 인가한 박막과 인가하지 않은 박막의 주상정 형상과 경도 값에 큰 차이가 없었으며, 박막의 박리현상은 모든 시편에서 일어나지 않았다. DC 스퍼터링으로 제조한 TiN 박막은 bias 전압을 인가하지 않으면 색상이 노란색이 아닌 갈색으로 나타났으며, HIPIMS으로 제조한 박막은 bias 전압 인가 유무에 상관없이 노란색 색상을 나타냈다. 앞서 설명한 DC 스퍼터링과 HIPIMS의 공정조건에 따라 나타난 박막의 경도, 색상, 물성변화 차이는 DC 스퍼터링보다 높은 HIPIMS의 이온화율에서 기인한 것으로 생각된다. 본 연구결과를 이용하면 다양한 형태의 박막 구조 제어가 가능하고 이러한 미세구조 제어를 통해서 박막의 물성도 제어가 가능할 것으로 판단된다.

• Proceedings of the Korean Vacuum Society Conference
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• 2012.02a
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• pp.144-144
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• 2012

최근 폴리머를 기판으로 하는 고속 Flexible TFT (Thin film transistor)나 고효율의 박막 태양전지(Thin film solar cell)를 실현시키기 위해 낮은 비저항(resistivity)을 가지며, 높은 홀 속도(carrier hall mobility)와 긴 이동거리를 가지는 다결정 반도체 박막(poly-crystalline semiconductor thin film)을 만들고자 하고 있다. 지금까지 다결정 박막 반도체를 만들기 위해서는 비교적 높은 온도에서 장시간의 열처리가 필요했으며, 이는 폴리머 기판의 문제점을 야기시킬 뿐 아니라 공정시간이 길다는 단점이 있었다. 이에 반도체 박막의 재결정화 온도를 낮추어 주는 metal (Al, Ni, Co, Cu, Ag, Pd, etc.)을 이용하여 결정화시키는 방법(MIC)이 많이 연구되어지고 있지만, 이 또한 재결정화가 이루어진 반도체 박막 안에 잔류 금속(residual metal)이 존재하게 되어 비저항을 높이고, 홀 속도와 이동거리를 감소시키는 단점이 있다. 이에 본 실험은, 종래의 MIC 결정화 방법에서 이용되어진 금속 증착막을 이용하는 대신, HIPIMS (High power impulse magnetron sputtering)와 PIII&D (Plasma immersion ion implantation and deposition) 공정을 복합시킨 방법으로 적은 양의 알루미늄을 이온주입함으로써 재결정화 온도를 낮추었을 뿐 아니라, 잔류하는 금속의 양도 매우 적은 다결정 반도체 박막을 만들 수 있었다. 분석 장비로는 박막의 결정화도를 측정하기 위해 GIXRD (Glazing incident x-ray diffraction analysis)와 Raman 분광분석법을 사용하였고, 잔류하는 금속의 양과 화학적 결합 상태를 알아보기 위해 XPS (X-ray photoelectron spectroscopy)를 통한 분석을 하였다. 또한, 표면 상태와 막의 성장 상태를 확인하기 위하여 HRTEM(High resolution transmission electron microscopy)를 통하여 관찰하였다.