고분자 접착제와 금속 피착재의 접착강도에 미치는 피착재 두께의 영향

하윤근,심준형,백주환,김민균,조영래,Ha, Yungeun,Sim, Jun-Hyung,Baeg, Ju-Hwan,Kim, Min-Kyun,Cho, Young-Rae 한국마이크로전자및패키징학회 2020 마이크로전자 및 패키징학회지 Vol.27 No.4

고분자 재료인 접착제와 금속 피착재 사이의 정량적인 접착강도 측정은 중요하다. 고분자 재료인 접착제와 금속 피착재 사이의 접착강도 측정 시, 피착재의 종류와 두께 변화가 접착강도에 미치는 영향에 대해 연구하였다. 금속 피착재의 종류로는 알루미늄과 스텐리스강 2종류가 선택되었으며, 접착강도의 측정에는 돌리테스트와 전단시험이 사용되었다. 인장응력 방식의 돌리테스트로 고분자 접착제와 금속 피착재 사이의 접착강도 측정 시, 금속 피착재의 두께 변화는 접착강도의 크기에 거의 영향을 미치지 않았으나, 피착재의 종류에 따라 접착강도는 다르게 나타났다. 반면, 전단시험으로 고분자 접착제와 금속 피착재 사이의 접착강도 측정 시, 금속 피착재의 상대적 두께 변화는 접착강도의 크기에 영향을 주었다. 이유는 전단시험 시 접착부의 모서리 부분에서 발생하는 피착재의 휘어짐 현상은 접착부에 추가적인 인장응력을 발생시켜 접착강도를 낮추는데 기여하기 때문이다. 이 연구의 결과, 돌리테스트는 피착재의 두께가 변해도 접착강도의 변화가 거의 없기 때문에 고분자 접착제와 금속 피착재의 정량적인 접착강도 측정 시 널리 사용될 것으로 예상된다. It is important to measure the quantitative adhesive strength between an organic adhesive and a metal adherend. In measuring the adhesive strength between an organic adhesive and a metal adherend, the effect of the kind and thickness of the adherend on the adhesive strength was studied. Two kinds of metal adherends were selected, aluminum (Al1050) and stainless steel (STS304), and a dolly test and a lap shear test were used to measure the adhesive strength. When measuring the adhesive strength between the organic adhesive and the metal adherend by the tensile stress mode of dolly test, the change in the thickness of the metal adherend had little effect on the adhesive strength, however, the adhesive strength was different depending on the kind of the adherend. On the other hand, when measuring the adhesive strength between the organic adhesive and the metal adherend by the lap shear test, the change in the relative thickness of the metal adherend had an effect on the adhesive strength. The reason is that the bending phenomenon of the adherend occurring in the edge of bonding region during the lap shear test contributes to lowering the adhesive strength by generating additional tensile stress in the bonding region. From this work, it is concluded that the dolly test could be widely used when measuring the quantitative adhesive strength of organic adhesives and metal adherend because there is little change in adhesive strength even though the thickness of the adherend is changed.

Adhesion strength of die attach film for thin electronic package at elevated temperature

Mose, Bruno R.,Son, In-Seo,Shin, Dong-Kil Elsevier 2018 Microelectronics and reliability Vol.91 No.1

<P><B>Abstract</B></P> <P>Adhesion strength of a thin film for electronic packaging was investigated. The effects of temperature and loading rate on the adhesion were observed considering the viscoelasticity of adhesive. Various temperature conditions over the glass transition temperature of the adhesive were applied with controlled loading rates. A small hot plate was specially designed to control the temperature. Loading rate was controlled by a servo motor. A cantilever specimen was fabricated by two rectangular silicon chips. The adhesion was measured by a modified single cantilever beam method. Bending force was applied to the cantilever using rotatable jig. Adhesion strength was found to strongly depend on the temperature and loading rate. Below the glass transition temperature (T<SUB>g</SUB>), the adhesion strength was increased with increasing loading rate. Near the Tg, the adhesion strength was decreased with increasing loading rate. Above the T<SUB>g</SUB>, the adhesion strength did not significantly depend on the loading rate.</P> <P><B>Highlights</B></P> <P> <UL> <LI> Single cantilever beam method measures mode-I adhesion of die attach film. </LI> <LI> Hot plate controls the specimen temperature easily. </LI> <LI> Below the glass transition temperature, the adhesion strength increases with increasing loading rate. </LI> <LI> Near the glass transition temperature, the adhesion strength decreases with increasing loading rate. </LI> </UL> </P>

TENSILE BOND STRENGTH BETWEEN ELASTOMERIC IMPRESSION MATERIALS AND TRAY RESINS DEPENDING ON THE THICKNESS OF THE TRAY ADHESIVE

Kim, Tae-Won,Moon, Hong-Seok,Lee, Keun-Woo,Chung, Moon-Kyu The Korean Academy of Prosthodonitics 2006 대한치과보철학회지 Vol.44 No.6

Statement of problem. Elastomeric impression materials have been widely used to obtain an accurate impression. However there have not been enough studies on the influence of the thickness of the tray adhesives on the bonding strength between the trays and the elastomeric impression materials. Purpose. In order to understand the relationship between the thickness of the tray adhesive and the tensile bond strength and to suggest the thickness at which the bonding strength is strongest, tensile bond strength related to the thickness of adhesives of 3 different elastomeric impression materials were tested. Materials and methods. 3 impression materials, $Permlastic^{(R)}$. Regular Set(Kerr Corp., Romulus, Michigan, U.S.A.), $Impregum^{TM}$ $Penta^{TM}$(3M ESPE, Seefeld, Germany), and Aquasil Ultra Monophase Regular Set Smart Wetting.(Dentsply Caulk, Milford, Delaware, U.S.A.), were used in this study, and tray adhesives from the same manufacturers of the impression materials were used, which were Rubber Base Adhesive, Polyether Adhesive, and Silfix, respectively. The tray specimens were prepared by autopolymerizing the tray material(Instant Tray Mix, Lang, Wheeling, Illinois, U.S.A.), and a PVC pipe was used to house the impression material. In group A, tray adhesives were applied in multiple thin layers of 1 to 5 and in group B, adhesives were applied only once, in the thickness equivalent to several applications. Lightness($L^*$) of the adhesion surface was measured with a spectrophotometer(CM-3500d, Konica Minolta, Sakai, Osaka, Japan). The tensile bond strength of the elastomeric impression material and the tray resin was measured with universal materials testing machines(Instron, Model 3366, Instron Corp, Nowood, Massachusetts, U.S.A.). A formula between the number of adhesive application layers and the lightness of the adhesion surface was deduced in group A, and the number of adhesive layers in group B was estimated by applying the lightness($L^*$) to the deduced formula. Results. 1. In group A, a statistically significant increase in tensile bond strength appeared when the number of application layers increased from 1 to 2 and from 4 to 5, and no significant difference was present between 2, 3, and 4 layers in Permlastic. In Impregum, the tensile bond strength was significantly increased when the number of adhesive layers increased from 1 to 3, but no significant difference after 3 layers. In Aquasil, the tensile bond strength significantly increased as the number of application layers increased up to 4 but showed no significant difference between 4 and 5. 2. In group B, the tensile bond strength was decreased when the thickness of the adhesive increased in Permlastic. Impregum showed an increased tensile bond strength when the thickness of the adhesive was increased. In Aquasil, the tensile bond strength increased as the number of adhesive application layers increased up to approximately 2.5 layers but it sharply decreased after approximately 4.5. Conclusion. From the study, the common idea that it is better to apply a thin and single coat of tray adhesive needs correction in more detailed ways, and instructions on some of the tray adhesives should be reconsidered since there were several cases in which the tensile bond strength increased according to the increase in the thickness of the adhesives.

Effect of plasma treatment on adhesion strength and moisture absorption characteristics between epoxy molding compound/silicon chip (EMC/chip) interface

Oh, Gyung-Hwan,Joo, Sung-Jun,Jeong, Jae-Woo,Kim, Hak-Sung Elsevier 2019 Microelectronics and reliability Vol.92 No.-

<P><B>Abstract</B></P> <P>Reliability of interface between two dissimilar materials becomes an important issue due to increasing demands of high-density integrated circuits. Most of failures of semiconductor package occur at the interface between two dissimilar materials in high temperature reflow process, thus, adhesion strength under high temperature should be investigated. In this study, an adhesion shear test jig was newly devised to measure the adhesion strength of epoxy molding compound/Si chip (EMC/chip) interface at high temperature (200 °C). In order to investigate the effect of plasma treatment on adhesion strength and moisture absorption characteristics, the number of plasma treatments was varied. Also, moisture absorption time was varied to observe the moisture uptake and degradation of adhesion strength with respect to plasma treatment number. Atomic force microscope (AFM) was analyzed to verify the surface roughness of silicon chip, and scanning electron microscopy (SEM) was used to observe cross-sectional fractured morphology after adhesion strength test. From this study, it was found that the plasma treatments affect much the adhesion strength and moisture uptake at the interface between the EMC/Chip interface.</P> <P><B>Highlights</B></P> <P> <UL> <LI> Measures the adhesion strength of the real semiconductor at high temperature. </LI> <LI> Stronger chemical bonding at the interface prevents the moisture absorption. </LI> <LI> Excessive plasma treatment degrades the adhesion strength by effective area reduction. </LI> <LI> Optimization of plasma treatment for enhancing the adhesion strength. </LI> </UL> </P>

A Study on Bracket-Adhesive Combinations in Aspect of Shear Bond Strength and Bond Failure

Han, Jae-Ik,Son, Woo-Sung 대한치과교정학회 1998 대한치과교정학회지 Vol.28 No.6

적절한 전단접착강도를 가지면서 법랑질손상과 브라켓파절을 적게 일으키는 브라켓-접착제의 그룹을 찾아내기 위하여 전단접착강도, 법랑질손상, 브라켓탈락양상, 브라켓 주위의 밀봉과 법랑질-접착제-브라켓 사이의 긴밀도를 연구하였다. 교정치료목적으로 발치한 240개의 치아를 각각 10개씩 24개 군으로 나누어서 브라켓을 접착한 후 48시간후에 전단접착강도를 측정하고 브라켓 탈락 양상을 조사하였다. 또한 브라켓주위의 밀봉과 법랑질-접착제-브라켓 사이의 긴밀도를 평가하기 위해서 브라켓이 접착된 치아를 반으로 자른후 주사전자현미경상에서 관찰하였다. 6종류의 브라켓과 4종류의 접착제가 사용되었으며 브라켓은 Image, Plastic, Crystaline, Fascination, Transcend, metal bracket을 사용하였으며 접착제로는 No-mix, Light-Bond, OrthoLC, Superbond C&B가 사용되었다. 이와같은 연구로 부터 다음과 같은 결론을 내렸다. 1. 전단접착강도는 Fascination-Light Bond 군에서 36.58Kg(410.07Kg/㎠)으로 가장 높았으며 Image-OrthoLC군에서 8.93Kg(75.51Kg/㎠)으로 가장 낮았다. OrthoLC를 접착제로 사용하였을 때 전단접착강도는 다른 접착제를 사용하였을 때 보다 비교적 낮았다. 2. 접착제의 종류에 관계없이 Fascination bracket의 전단접착강도는 비교적 높았으며 Image, Plastic bracket의 전단접착강도는 비교적 낮았다. Crystaline, Transcond bracket의 전단접착강도는 metal bracket의 전단접착강도와 비슷하거나 낮았다. 3. 전단접착강도와 법랑질 파절, 브라켓 파절은 상관관계가 있었으며, 접착강도가 증가할수록 법랑질 파절과 브라켓 파절은 증가하였다. 4. OrthoLC를 접착제로 사용하였을 때 법랑질 파절과 브라켓 파절은 일어나지 않았으나 Superbond C&B를 접착제로 사용하였을 때는 법랑질 파절과 브라켓 파절의 빈도가 높았다. 5. No-mix, Light-Bond를 접착제로 사용하였을 때 브라켓 주위의 밀봉과 법랑질-접착제-브라켓의 긴밀도는 양호하였다. 접착제의 종류에 관계없이 Ceramic bracket에서 접착제-브라켓의 긴밀도는 양호하였다. 6. 적절한 전단접착강도를 가지면서 법랑질 파절과 브라켓 파절을 일으키지 않은 군은 Crystaline-No mix, Crystaline-Light Bond, Crystaline-OrthoLC, metal-No mix, metal-Light Bond, metal-OrthoLC 군이였다. The purpose of the present study was to seek bracket-adhesive combinations which have adequate bond strength with no enamel and bracket fracture. The shear bond strengths were measured, the sites of failure and the enamel damage were investigated and the peripheral sealing and adaptation between enamel surface, bonging adhesive and bracket were evaluated, 240 noncarious human premolars were divided into twenty four groups of ten teeth. Shear bond strengths of each group were determined in an universal testing machine after two days passed and the debonded specimens were inspected to determine the predominant bond failure sites. To evaluate peripheral sealing and adaption between enamel surface adhesive and bracket, each specimen was cut longitudinally into two halves which included the midsection of the bracket, adhesive and enamel and examined in scanning electron microscope. Six different types of brackets were bonded to the tooth with four different type of adhesives. Six different types of brackets were Image, Plastic, Crystaline, Fascination, Transcend 2000 and metal bracket and four different adhesives were No-mix, Light-Bond, OrthoLC and Superbond C&B. From this study, it may be concluded that(1) The mean shear bond strength varied from a high of 36.58Kg(410.07Kg/㎠) with the Fascination-Light Bond combination group to a low 8.93Kg(75.51Kg/㎠) with the Image-OrthoLC combination group. When using OrthoLC as adhesive, the mean shear bond strength was significantly lower than that of other combination groups, (2) Regardless of adhesives, the mean shear bond strength of Fascination brackets was relatively high whereas Plastic and Image brackets had low shear bonding strength. The shear bond strength of Crystaline bracket and Transcend 2000 was relatively equal to or lower than that of metal bracket, (3) There was a correlation between bond strength, enamel damage and bracket fractrue. As the shear bond strength was increased, the rate of enamel damage and bracket fractrue were increased, (4) The combination groups that use OrthoLC as adhesive were debonded in shear stress without enamel fracture and bracket fracture, whereas the combination groups that use Superbond C&B as adhesive experienced a relative high enamel fracture rate and bracket fracture rate, (5) Peripheral sealing and adaptation between enamel-adhesive-bracket were relatively good when using Light-Bond or No-Mix as adhesive, Regardless of adhesives, adaptation between bracket-adhesive were relatively good in Ceramic brackets, (6) The combination groups which had adequate bonding strength with no enamel and bracket fracture were Crystaline-No mix, Crystaline-Light Bond, Crystaline-OrthoLC, metal-No mix, metal-Light Bond and metal-OrthoLC combination groups.

The effect of different adhesive system applications on push-out bond strengths of glass fiber posts

Kivanc, Bagdagul Helvacioglu,Arisu, Hacer Deniz,Uctasli, Mine Betul,Okay, Tufan Can The Korean Academy of Prosthodonitics 2013 The Journal of Advanced Prosthodontics Vol.5 No.3

PURPOSE. Over the past years, the adhesion of fiber posts luted with simplified adhesive systems has been a matter of great interest. The aim of this study was to assess the post retentive potential of a self-adhesive resin cement using different adhesive systems to compare the push-out bond strengths of fiber posts. MATERIALS AND METHODS. The post spaces of 56 mandibular premolar roots were prepared and divided into 4 experimental groups and further divided into 2 subgroups according to testing time (n=7). The fiber posts (Rely X Fiber Post) were luted with a self-adhesive resin cement (RelyX Unicem) and one of the following adhesive systems: no adhesive, a total-etch adhesive resin (Single Bond), a two-step self-etch adhesive resin (Clearfil SE Bond) and a one-step self-etch adhesive resin (Clearfil S3 Bond). Each root was cut horizontally, and 1.5 mm thick six root segments were prepared. Push-out tests were performed after one week or three months (0.5 mm/min). Statistical analysis were performed with three-way ANOVA (${\alpha}$=.05). RESULTS. Cervical root segments showed higher bond strength values than middle segments. Adhesive application increased the bond strength. For one week group, the total-etch adhesive resin Single Bond showed higher bond strength than the self-adhesive resin cement RelyX Unicem applied without adhesive resin at middle region. For 3 months group, the two-step self-etch adhesive resin Clearfil SE Bond showed the highest bond strength for both regions. Regarding the time considered, Clearfil SE Bond 3 months group showed higher bond strength values than one week group. CONCLUSION. Using the adhesive resins in combination with the self-adhesive resin cement improves the bond strengths. The bond strength values of two-step self-etch adhesive resin Clearfil SE Bond improved as time passes.

Influence of Heat-Treatment on the Adhesive Strength between a Micro-Sized Bonded Component and a Silicon Substrate under Bend and Shear Loading Conditions

Chiemi Ishiyama 한국비파괴검사학회 2012 한국비파괴검사학회지 Vol.32 No.2

Adhesive bend and shear tests of micro-sized bonded component have been performed to clarify the relationship between effects of heat-treatment on the adhesive strength and the bonded specimen shape using Weibull analysis. Multiple micro-sized SU-8 columns with four different diameters were fabricated on a Si substrate under the same fabrication condition. Heat-treatment can improve both of the adhesive bend and shear strength. The improvement rate of the adhesive shear strength is much larger than that of the adhesive bend strength, because the residual stress, which must change by heat-treatment, should effect more strongly on the shear loading. In case of bend type test, the adhesive bend strength in the smaller diameters (50 and 75 ㎛) widely vary, because the critical size of the natural defect (micro-crack) should vary more widely in the smaller diameters. In contrast, in case of shear type test, the adhesive shear strengths in each diameter of the columns little vary. This suggests that the size of the natural defects may not strongly influence on the adhesive shear strength. All the result suggests that both of the adhesive bend and shear strengths should be complicatedly affected by heat-treatment and the bonded columnar diameter.

Influence of Heat-Treatment on the Adhesive Strength between a Micro-Sized Bonded Component and a Silicon Substrate under Bend and Shear Loading Conditions

Ishiyama, Chiemi The Korean Society for Nondestructive Testing 2012 한국비파괴검사학회지 Vol.32 No.2

Adhesive bend and shear tests of micro-sized bonded component have been performed to clarify the relationship between effects of heat-treatment on the adhesive strength and the bonded specimen shape using Weibull analysis. Multiple micro-sized SU-8 columns with four different diameters were fabricated on a Si substrate under the same fabrication condition. Heat-treatment can improve both of the adhesive bend and shear strength. The improvement rate of the adhesive shear strength is much larger than that of the adhesive bend strength, because the residual stress, which must change by heat-treatment, should effect more strongly on the shear loading. In case of bend type test, the adhesive bend strength in the smaller diameters (50 and $75\;{\mu}m$) widely vary, because the critical size of the natural defect (micro-crack) should vary more widely in the smaller diameters. In contrast, in case of shear type test, the adhesive shear strengths in each diameter of the columns little vary. This suggests that the size of the natural defects may not strongly influence on the adhesive shear strength. All the result suggests that both of the adhesive bend and shear strengths should be complicatedly affected by heat-treatment and the bonded columnar diameter.

The effect of different adhesive system applications on push-out bond strengths of glass fiber posts

Mine Betul uctaslı,Hacer Deniz Arısu,Tufan Can Okay,Bagdagul Helvacıoglu Kıvanc 대한치과보철학회 2013 The Journal of Advanced Prosthodontics Vol.5 No.3

PURPOSE Over the past years, the adhesion of fiber posts luted with simplified adhesive systems has been a matter of great interest. The aim of this study was to assess the post retentive potential of a self-adhesive resin cement using different adhesive systems to compare the push-out bond strengths of fiber posts. MATERIALS AND METHODS The post spaces of 56 mandibular premolar roots were prepared and divided into 4 experimental groups and further divided into 2 subgroups according to testing time (n=7). The fiber posts (Rely X Fiber Post) were luted with a self-adhesive resin cement (RelyX Unicem) and one of the following adhesive systems: no adhesive, a total-etch adhesive resin (Single Bond), a two-step self-etch adhesive resin (Clearfil SE Bond) and a one-step self-etch adhesive resin (Clearfil S3 Bond). Each root was cut horizontally, and 1.5 mm thick six root segments were prepared. Push-out tests were performed after one week or three months (0.5 mm/min). Statistical analysis were performed with three-way ANOVA (α=.05). RESULTS Cervical root segments showed higher bond strength values than middle segments. Adhesive application increased the bond strength. For one week group, the total-etch adhesive resin Single Bond showed higher bond strength than the self-adhesive resin cement RelyX Unicem applied without adhesive resin at middle region. For 3 months group, the two-step self-etch adhesive resin Clearfil SE Bond showed the highest bond strength for both regions. Regarding the time considered, Clearfil SE Bond 3 months group showed higher bond strength values than one week group. CONCLUSION Using the adhesive resins in combination with the self-adhesive resin cement improves the bond strengths. The bond strength values of two-step self-etch adhesive resin Clearfil SE Bond improved as time passes.

Drying time of tray adhesive for adequate tensile bond strength between polyvinylsiloxane impression and tray resin material

Yi, Myong-Hee,Shim, Joon-Sung,Lee, Keun-Woo,Chung, Moon-Kyu 대한치과보철학회 2009 The Journal of Advanced Prosthodontics Vol.1 No.2

STATEMENT OF PROBLEM. Use of custom tray and tray adhesive is clinically recommended for elastomeric impression material. However there is not clear mention of drying time of tray adhesive in achieving appropriate bonding strength of tray material and impression material. PURPOSE. This study is to investigate an appropriate drying time of tray adhesives by evaluating tensile bonding strength between two types of polyvinylsiloxane impression materials and resin tray, according to various drying time intervals of tray adhesives, and with different manufacturing company combination of impression material and tray adhesive. MATERIAL AND METHODS. Adhesives used in this study were Silfix (Dentsply Caulk, Milford, Del, USA) and VPS Tray Adhesive (3M ESPE, Seefeld, Germany) and impression materials were Aquasil Ultra (monophase regular set, Dentsply Caulk, Milford, Del, USA) and Imprint Ⅱ Gai-ant (regular body, 3M ESPE, Seefeld, Germany). They were used combinations from the same manufacture and exchanged combinations of the two. The drying time was designed to air dry, 5 minutes, 10 minutes, 15 minutes, 20 minutes, and 25 minutes. Total 240 of test specimens were prepared by auto-polymerizing tray material(Instant Tray Mix, Lang, Wheeling, Ⅱ, USA) with 10 specimens in each group. The specimens were placed in the Universal Testing machine(Instron, model 3366, Instron Corp, University avenue, Nowood, MA, USA) to perform the tensile test (cross head speed 5 mm/min). The statistically efficient drying time was evaluated through ANOVA and Scheffe test. All the tests were performed at 95% confidence level. RESULTS. The results revealed that at least 10 minutes is needed for Silfix-Aquasil, and 15 minutes for VPS Tray Adhesive-lmprint Ⅱ, to attain an appropriate tensile bonding strength. VPS Tray Adhesive-lmprint II had a superior tensile bonding strength when compared to Silfix-Aquasil over 15 minutes. Silfix-Aquasil had a superior bonding strength to VPS Tray Adhesive-Aquasil, and VPS Tray Adhesive-lmprint Ⅱ had a superior tensile bonding strength to Silfix-lmprint Ⅱ at all drying periods. CONCLUSION. Significant increase in tensile bonding strength with Silfix-Aquasil and VPS Tray adhesive-Imprint Ⅱ combination until 10 and 15 minutes respectively. Tray adhesive-impression material combination from the same company presented higher tensile bonding strength at all drying time intervals than when using tray adhesive-impression material of different manufactures.