• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2015.11a
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• pp.354-354
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• 2015

코팅 층과 소지 사이의 접합력 평가를 위하여 박리 시험법(Peel Off Test), 블리스터 시험법(Blister Test), 압입균열 시험법(Indentation Test), 직접 인장 시험법(Direct Full Off Test), 스카치 테이프 시험법(Scotch Tape Test), 그리고 스크래치 시험법(Scratch Test) 등이 사용되어 왔다. 이 중 박리 시험법과 스카치 테이프 시험법이 산업계에서 일반적으로 사용되고 있다. 전자 산업계에서 많이 사용되고 있는 박리시험법은 금속박막과 절연체 기판 사이의 접합력을 간단하게 측정할 수 있으며, 실험값의 재현성이 뛰어난 장점이 있다. 또한, 측정하는 동안 만들어지는 박리 곡선(Peel Curve)로부터 분석의 신뢰성 여부를 확인할 수 있다. 이러한 장점에도 불구하고 박리 시험법 특성 상 금속 코팅층의 강도가 금속 피막/기판간 접합 강도를 초과하여야 하기 때문에 수백 nm 이하의 박막의 접합력 측정에는 적용하기가 어렵다. 이에 반하여, 스카치 테이프 분석법은 일정길이의 접착 테이프를 박막 표면에 붙인 후 다시 떼어내면서 접착력을 평가하는 방법으로, 박막의 접합력 평가에 적용이 가능하다. 그러나 이 방법은 합격 불합격 여부를 판정하는 정성적인 방법으로 정량평가가 어렵다. 또한, 박막에 접착 테이프를 붙일때의 압력, 테이프를 박리할 때의 각도 및 속도를 일정하게 제어하기가 쉽지 않아 결과의 신뢰성이 높지 않다. 스크래치 테스트는 탐사침(Stylus)을 이용하여 박막의 표면에 하중을 증가시키면서 기판을 이동하여, 피막의 균열이나 박리될 때의 임계 하중값 (Critical Load; Lc)을 측정하는 방법이다. 이 방법은 시편 준비가 쉽고 간단하여 빠른 분석이 가능하고, 수백 nm 이하의 박막에도 적용 가능하다. 또한, 접합력을 정량화 할 수 있기 때문에 변수에 따른 접합력 비교가 용이하다는 장점이 있다. 이와 같은 분석적 장점에도 불구하고, 스크래치 시험을 통한 접합력 측정 방법은 아직까진 산업적으로 널리 활용되지 못하고 있다. 따라서, 본 연구에서는 스크래치 테스트의 원리 및 이론에 대하여 간략히 알아보고, 스크래치 분석을 이용한 접합력 비교에 대한 실제 사례들을 소개하고자 하였다.

• Journal of Adhesion and Interface
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• v.2 no.3
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• pp.1-8
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• 2001

Epoxy composites filled with natural zeolite was prepared to investigate the effects of silane coupling agent, ${\gamma}$-APS (${\gamma}$-aminopropyltriethoxysilane)on the surface free energy, tensile properties and interfacial morphology. The value of Lifshitz-van der Waals component, ${\gamma}{\frac{LW}{SV}}$ for polar was $19.22mJ/m^2$ and increased, while that of Lewis acid-base component, ${\gamma}{\frac{AB}{SV}}$ for polar was $15.27mJ/m^2$ and decreased with the increasing content of ${\gamma}$-APS treatment. It is due that the surface of the zeolite is more coated by hydrophobic of alkyl group than hydrophilic amine or hydroxyl group. The tensile strength and Young's modulus of epoxy system were improved by the treatment with ${\gamma}$-APS due to the strong interface bonding, which was confirmed by SEM.

• Journal of Adhesion and Interface
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• v.23 no.1
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• pp.8-16
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• 2022

In this study, self-healable waterborne polyurethane (SH-WPU) as shoes and coating materials with self-healable disulfide functionalities was synthesized by mixing polyether polyol to impart excellent durability and heat resistance and polycarbonate polyol to impart excellent mechanical properties. The synthesized SH-WPU was characterized by fourier transform-infrared spectroscopy (FT-IR), and physical and self-healing properties were confirmed through universal testing machine (UTM) and scanning electron microscope (SEM) measurements. Tensile strength and hardness were increased and elongation was decreased by using polycarbonate polyol. In addition, as a result of comparison of thermal properties, thermal stability has been increased as the content of polycarbonate polyol increased. The healing efficiency showed the highest efficiency when poly(tetramethylene ether)glycol : polycarbonate polyol = 0.75 : 0.25, and it was confirmed that the damaged part was healed through surface observation using a microscope and SEM.

• Journal of the Microelectronics and Packaging Society
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• v.3 no.1
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• pp.11-24
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• 1996

부분압이 다른 여러 가지 반응성 가스분위기하에서 이른곤 이온을 이용하여 PC, PET PMMA 그리고 PTFE 폴리머 표면의 삼차 증류수에대한 진수성을 증대하였다. 폴리머 표면의 친수성의 변화는 여러 가지 반응성 가스 분위기하에서 아르곤 이온의 조사량을 1014 부터 1x1017cm2까지 변화하면서 조사하였다. 접촉감은 아르곤 이온이 조사되는 폴리머 표면 근처에 유입된 가스의 방응성(O2>N2>H2)에 따라 많이 감소하였다, 폴리머 표면에 형성된 친수성기는 XPS Cls, Ols, 그리고 Nls 스펙트럼을 분석하여 확인하였다. 표면 개질된 PC와 PTFE에 대한 Al 금속의 접착력 증대를 Scotch tape와 인장실험을 통하여 확인하였다. 접착 력 증가는 표면 에너지 중 polar force의 증가에 의한 것으로 입증되었다. 에너지를 가진 아 르곤 입자 폴리머 체인 그리고 반응성 가스 사이의 반응기구는 2단계 모델로 설명가능하였 는데 그 기구는 첫 번째 이온의 조사에 의한 불안정한 폴리머 체인의 형성과 두 번째 단계 로 이렇게 형성된 폴리머 체인과 반응성 가스들 사이의 화학반응으로 이루어진다. 질화아루 미늄의 표면을 산소분위기하에서 아르곤 빔을 조사하여 표면개질한후 AlON층이 새롭게 형 성된 것을 XPS를 이용하여 확인할수 있었다. 개질된 질화알루미늄과 구리금속 박막간의 접 착력을 scratch 실험을 통하여 조사하였다.

• Elastomers and Composites
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• v.36 no.2
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• pp.111-120
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• 2001

Mechanical properties and their adhesion behavior with zinc- and brass-plated steel cords of natural rubber/acrylonitrile-butadiene blend compounds were investigated as a function of blend ratio. The Mooney viscosity and stress relaxation time were found to be lowered with increasing NBR content. Tensile modulus generally increased with increasing NBR content. Tensile stress at break stayed constant up to about 40 phr and showed minimum at $50{\sim}60 phr$, and thereafter increased with increasing NBR content. Strain at break decreased linearly below 50 phr, and above the level it showed nearly constant value. Based on the abrupt drops in elastic modulus and tan ${\delta}$ peak, the glass transition temperature of NR and NBR were found to be -55 and $-10^{\circ}C$, respectively. In the case of NR/NBR blend compounds, two distinct transition points were observed and each transition position was not affected by NBR level indicating an incompatible nature of NR/NBR blend system. The pullout force and rubber coverage decreased to the level of about 40% to that of pure m compound, when the 50 phr of NR was replaced by NBR. However, the pure NBR compound showed the comparable adhesion performance with NR(${\sim}90%$). The sulfur concentration was found to become lower with the increased NBR content at the adhesion interface based on the Auger spectrometer results, representing a lack of adhesion layer formation, and this was explained for a possible cause of low adhesion performance with adding NBR.

• Elastomers and Composites
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• v.34 no.1
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• pp.53-64
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• 1999

The mechanical, electrical, and thermal properties of polyamide-modified poly (vinyl chloride) (PVC)-sol was investigated. PVC-sol was plasticized with dioctyl phthalate (DOP). In this work, the effects of the addition of polyamide on the properties of PVC-sol seal-ants were investigated. Two kinds of polyamide resins having different amine value were used. It was found that the properties of the PVC-sol sealants were significantly affected by the contents and types of the added polyamide rosins. The PVC-sol sealants modified with polyamide A (low amino value) showed higher tensile properties than those modified with polyamide B(high amino value) did, and thermal stability of the sealants showed nearly the same trends. The tensile strength of sealants were decreased with increasing the $CaCO_3$ contents. The dielectric constant were not strongly dependent on the polyamide types and contents.

• Journal of Adhesion and Interface
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• v.22 no.4
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• pp.136-143
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• 2021

Polyurea has been investigated as a polymer matrix for composite materials because of its high mechanical strength. Although polyurea has a similar chemical structure to polyurethane, it has much higher strength and durability. In this study, the fabrication of polyurea composites reinforced with carbon nanotube (CNT) and graphene oxide (GO) is demonstrated to enhance the tensile strength of the glass fibers composite. Using FTIR and Raman spectroscopies, the chemical structures of polyurea, CNT, and GO are investigated. As a result, spectroscopy analysis reveals that the chemical structure of CNT, GO, and polyurea is maintained during the fabrication of the composite structure. Scanning electron microscopy reveals the uniform distribution of CNT and GO across the polyurea matrix. The reinforcement of 1 wt% CNT in polyurea enhances the tensile strength of CNT/polyurea composites. In contrast, the reinforcement of GO in polyurea induces the degradation of the tensile strength of GO/polyurea composites.

• Restorative Dentistry and Endodontics
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• v.32 no.1
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• pp.9-18
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• 2007

The purposes of this study were to examine the variability of adhesive thickness on the different site of the cavity wall when used total-etch system without filler and simplified self-etch system with filler and to evaluate the relationship between variable adhesive thickness and microtensile bond strength to the cavity wall. A class I cavity in six human molars was prepared to expose all dentinal walls. Three teeth were bonded with a filled adhesive, $Clearfil^{TM}$ SE bond ana the other three teeth were bonded with unfilled adhesives, $Scotchbond^{TM}$ Multi Purpose. Morphology and thickness of adhesive layer were examined using fluorescence microscope. Bonding agent thickness was measured at three points along the axial cavity wall edge of cavity margin (rim). halfway down each cavity wall (h1f), internal angle of the cavity (ang). After reproducing the adhesive thickness at rim, h1f and ang, micro-tensile bond strength were evaluated. For both bonding agents, adhesive thickness of ang was significantly thicker than that of rim and h1f (P <0.05). As reproduced the adhesive thickness, microtensile bond strength was increased as adhesive thickness was increased in two bonding agents. Adhesive thickness of internal angle of the cavity was significantly thicker than that of the cavity margin and the halfway cavity wall for both bonding agents. Microtensile bond strength of the thick adhesive layer at the internal angle of the cavity was higher than that of the thin adhesive layer at 1,he cavity margin and the halfway cavity in the two bonding systems.

• Restorative Dentistry and Endodontics
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• v.29 no.1
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• pp.13-22
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• 2004

본 연구는 치수강 상아질 부위 및 상아질 접착제 종류에 따른 결합 강도를 측정하고 이들 사이의 상관관계를 구명하고자 시행되었다 45개의 대구치를 포매 후, 대조군에서는 교합면 법랑질 제거 후 ＃600 SiC paper까지 순차연마하여 상아질을 노출시켰고, 실험군에서는 치수강 개방 후 1시간동안 NaOCl에 보관 후 axial wall과 pulpal floor를 노출시켰다. 노출된 상아질 면에 상아질 접착제를 적용한 후 Z-100을 충전한 다음 40초간 광중합하였다. 사용된 상아질 접착제는 Scotchbond Multi-Purpose와 Single Bond, Clearfil SE Bond였다. $37^{\circ}C$ 증류수에 24시간 보관 후, 저속 diamond saw를 이용하여 0.7mm 두께로 수직절단하고 고속 diamond point(#104)로 단면적 $1{mm}^2$가 되도록 시편을 제작하고, Universal testing machine에서 미세인장 결합강도를 측정하였다. 1. 모든 상아질 접착제의 미세인장강도는 대조군, axial wall군, pulpal floor군 순으로 감소하는 경향을 보였다. 2. 대조군에서 SM과 BB는 SE에 비해 유의성 있게 높은 결합강도를 나타내었다(p<0.05). 3. SM과 SB는 대조군에 비해 axial wall군과 pulpal floor군에서 유의성있게 낮은 결합강도를 보였으나, SE에서는 pulpal floor군만이 유의성 있게 낮은 결합강도를 보였다(p<0.05). 4. Axial wall군과 pulpal floor군에서는 상아질 접착제의 종류에 따른 유의차를 보이지 않았다. 5. 전자현미경 소견에서는 대조군에 비해 axial wall군과 pulpal floor군이 더 부드러운 접착 계면을 나타내었다. 혼성층의 두께는 결합강도의 감소와는 관련이 없었다.

• Restorative Dentistry and Endodontics
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• v.32 no.3
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• pp.222-235
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• 2007

The objectives of this study was to evaluate the effect of thermocycling on the ${\mu}TBS$ (microtensile bond strength) to dentin with four different adhesive systems to examine the bonding durability. Freshly extracted $3^{rd}$ molar teeth were exposed occlusal dentin surfaces, and randomly distributed into 8 adhesive groups 3-steps total-etching (Scotchbond Multi-Purpose Plus; SM, All Bond-2; AB), 2-steps total-etching (Single Bond; SB, One Step plus; OS), 2-steps self-etching (Clearfil SE Bond; SE, AdheSE AD) and single-step self-etching systems (Promp L-Pop; PL, Xeno III; XE) Each adhesive system in 8 adhesives groups was applied on prepared dentin surface as an instruction and resin composite (Z250) was placed incrementally and light-cured. The bonded specimens were sectioned with low-speed diamond saw to obtain $1\times1mm$ sticks after 24 hours of storage at $37^{\circ}C$ distilled water and proceeded thermocycling at the pre-determined cycles of 0, 1,000 and 2,000. The ${\mu}TBS$ test was carried out with EZ-tester at 1mm/min. The results of bond strength test were statistically analyzed using one-way ANOVA/ Duncan's test at the a < 0.05 confidence level. Also, the fracture mode of debonded surface and the interface were examined under SEM. The results of this study were as follows ; 1. 3-step total etching adhesives showed stable, but bond strength of 2-step adhesives were decreased as thermocycling stress. 2. SE showed the highest bond strength, but single step adhesives (PL, XE) had the lowest value both before and after thermocycling. 3 Most of adhesives showed adhesive failure. The total-etching systems were prone to adhesive failure and the single-step systems were mixed failure after thermocycling. Within limited results of this study, the bond strength of adhesive system was material specific and the bonding durability was affected by the bonding step/ procedure of adhesive Simplified bonding procedures do not necessarily imply improved bonding performance.