• Journal of Welding and Joining
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• v.23 no.2
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• pp.52-58
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• 2005

This study was carried out to investigate the effect of bonding temperature and heating rate on transient liquid phase diffusion bonding of Ni-base superalloy. The heating rate was varied by $0.1^{\circ}C$/sec, $1^{\circ}C$/sec, $10^{\circ}C$/sec to the bonding temperatures $1100^{\circ}C,\;1150^{\circ}C,\;1200^{\circ}C$ under vacuum. As bonding temperature increased, maximum dissolution width of base metal increased, but a dissolution finishing time decreased. The eutectic width of insert metal in the bonded interlayer decreased linearly in proportion to the square root of holding time during isothermal solidification stage. The bonding temperature was raised, isothermal solidification rate slightly increased. As the heating rate decreased and the bonding temperature increased, the completion time of dissolution after reaching bonding temperature decreased. When the heating rate was very slow, the solidification proceeded before reaching bonding temperature and the time required for the completion of isothermal solidification became reduced.

• Journal of the Korean Society for Heat Treatment
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• v.29 no.2
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• pp.56-61
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• 2016

Heating experiments using the Ti-3Al-2.5V tube materials in a vacuum furnace have been performed to investigate a pertinent range of working temperatures and holding times for the development of the successive or simultaneous operation of superplastic hydroforming and diffusion bonding. The specimens were heated at $820^{\circ}C$, $870^{\circ}C$ and $920^{\circ}C$ respectively. Holding times at each temperature were varied up to 4 hours. Holding times longer than 1 hour were selected to consider the diffusion bonding process after or during the hydroforming process in the superplastic state. Grain sizes were varied from $5.7{\mu}m$ of the as-received tube to $9.2{\mu}m$ after heating at $870^{\circ}C/4hours$. Homogeneus granular microstructures could be maintained up to $870^{\circ}C$, while microstructures at $920^{\circ}C$ showed no more granular type.

• Proceedings of the Korean Vacuum Society Conference
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• 2012.02a
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• pp.280-280
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• 2012

We examined ammonia diffusion on the surface of amorphous ice film through the measurement of decreasing residual quantity of $NH_3$ molecules compared to $H_2O$. The populations of $NH_3$ molecules on the surface of amorphous ice were monitored by using the techniques of temperature programmed reactive ion scattering (TPRIS) method. The ratio of intensity between ammonia and water was examined as a function of time at controlled temperature. When ammonia molecules were externally added onto an ice film at a temperature of 80 K, ammonia coverage with regard to ice was 0.12-0.16 ML. The intensity of ammonia molecules on the surface of ice decreased as time increased and the extent of decreased intensity of ammonia increased as controlled temperature increased. Moreover, energy barrier was estimated to be $51kJmol^{-1}$ on amorphous ice film. The results of the experiment indicate that ammonia molecules have a property of vertical diffusion into amorphous ice and the energy barrier of ammonia diffusion into bulk of ice is higher than that of hydrogen bonding.

• Journal of Welding and Joining
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• v.21 no.4
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• pp.69-74
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• 2003

The mechanical properties of STD11 Joints by using TLP (Transient Liquid Phase Diffusion) bonding method employing MBF-30 and MBF-80 insert metals were investigated with concerning to the microstructural change. TLP bonding of STD 11 was carried out at 1323∼1423K for 0.6ks∼3.6ks in vacuum. The microstructure and the element distribution of the interlayer between tool steels and insert metals showed specific feature with bonding conditions. It was found that the width of the interlayer increased at initial bonding stage. However, the width of interlayer showed nearly constant value during the isothermal solidification. After isothermal solidification was completed, the joint showed homogeneous element distribution and similar microstructure with base metal because of the grain boundary migration to the bonded interlayer. The bonding strength measured by a tensile test has been varied with the bonding conditions. The maximum joint strength, 760MPa, was obtained with the condition of 1423K for 1.2ks using MBF30 insert metal in this experiment.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.9 no.1
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• pp.9-15
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• 2008

Mokumegane is one of the sophisticated metal craft techniques enabling wood grain surface effect. To embody the mokumegane, an ingot of well-bonded stacked metal plates has been required. Traditionally prepared mokumegane ingots were bonded using charcoal which enables reduction atmosphere, but sometimes end up with collapse of bonding interface due to the lack of reliable process control. We proposed a systematic vacuum direct bonding process for ingots. First, we confirmed copper//copper homogeneous plate bonding at $900^{\circ}C$ by applying uniaxial press of 2.5kg. We observed 80min required to obtain 90%-bonding ratio and the diffusion coefficient would be enhanced up to 100 times due to surface effect. Second, by considering enhanced diffusion behavior, we also obtained optimum bonding condition in copper/silver heterogeneous plates that ensures 90%-bonding ratio at $700^{\circ}C$ for 10min with apply uniaxial press. A 7-layered copper/silver ingot is prepared successfully, and eventually the prototype mokumegane cases for mobile phone were fabricated with these ingot.

• Journal of Welding and Joining
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• v.31 no.3
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• pp.76-83
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• 2013

This study investigated the effect of bonding temperature and holding time on microstructures and mechanical properties of diffusion bonded joint of Haynes230. The diffusion bonds were performed at the temperature of 950, 1050, and $1150^{\circ}C$ for holding times of 30, 60, 120 and 240 minutes at a pressure of 4MPa under high vacuum condition. The amount of non-bonded area and void observed in the bonded interface decreased with increasing bonding temperature and holding time. Cr-rich precipitates at the linear interface region restrained grain migration at $950^{\circ}C$ and $1050^{\circ}C$. However, the grain migration was observed in spite of short holding time due to the dissolution of precipitates to base metal in the interface region at $1150^{\circ}C$. Three types of the fracture surface were observed after tensile test. The region where the coalesce and migration of grain occurred much showed high fracture load because of base metal fracture whereas the region where those did less due to the precipitates demonstrated low fracture load because of interface fracture. The expected fracture load could be derived with the value of fracture area of base metal ($A_{BF}$) and interface ($A_{IF}$), $Load=201A_{BF}+153A_{IF}$. Based on this equation, strength of base metal and interface fracture were calculated as 201MPa and 153MPa, respectively.

• Proceedings of the KWS Conference
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• 2009.11a
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• pp.59-59
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• 2009

The influences of B and Si in the filler metals on microstructure and isothermal solidification during transient liquid-phase (TLP) bonding of a nitrogen-containing duplex stainless steel with MBF-30 (Ni-4.5wt.%Si-3.2wt.%B) and MBF-35 (Ni-7.3wt.%Si-2.2wt.%B), were studied at the temperature range of $1030-1090^{\circ}C$ with various times from 60 s to 3600 s under a vacuum of approximately $10^{-5}$ Torr. In case of the former, BN, $Ni_3B$ and $Ni_3Si$ precipitates were formed in the bonding region. BN and $Ni_3Si$ secondary phases were present in the joint for the latter case. The formation of $Ni_3B$ within the joint centerline is dependent on B content. The morphology of $Ni_3Si$ is dominated by Si concentration. A difference between the times for complete isothermal solidification obtained by the experiments and the conventional TLP bonding diffusion model was observed when using MBF-35. According to the simulated results, the isothermal solidification completion time for MBF-35 case was smaller than that in MBF-30. However, this experimental value obtained using MBF-35 was notably larger than that obtained using MBF-30. Isothermal solidification of liquid MBF-30 is controlled by the first isothermal solidification regime dependent on B diffusion model, whereas that of liquid MBF-35 experiences two isothermal solidification regimes and is mainly controlled by the second isothermal solidification dependent on Si diffusion model. In addition, only if Si content exceeds a critical value, the slower 2nd solidification regime will commence.

• Proceedings of the Korean Powder Metallurgy Institute Conference
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• 2006.09b
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• pp.1130-1131
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• 2006

We found that the """interface reaction between Ni-based alloy bond, diamond, and steel core is very critical in bond strength of diamond tool. None element from metal bond diffuses into the steel core but the Fe element of steel core was easily diffused into the bond. This diffusion depth of Fe has a great effect on the bonding strength. The Cr in steel core accelerated the Fe diffusion and improved the bond strength, on the other hand, carbon decreased the strength. Ni-based alloy bond including Cr was chemically bonded with diamond by forming Cr carbide. However, the Cr and Fe in STS304 were largely interdiffused, the strength was very low. The Cr passivity layer formed at surface of STS304 made worse strength at commissure in brazing process.

• Journal of Welding and Joining
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• v.13 no.3
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• pp.106-115
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• 1995

To know the bonding phenomena of Ti/Cu brazed joint, a characteristic of microstructures in bonding interlayer of vacuum brazed pure Ti to Cu has been studied in the temperature range from 1088 to 1133K for various bonding times using Ag-28wt%Cu filler metal. Also intermediate phases formed in bonded interlayer and behavior of layer growth have been investigated. The obtained results in this study are as follows: 1) Liquid insert metal width at the each brazing temperature was proportional to the square root of brazing time, and it was considered that the liquid insert metal width was controlled by the diffusion rate process of primary .alpha.-Cu formed at the Ti side. 2) Intermediate phases formed near the Ti interface were .betha.-Ti and intermetallic compounds TiCu, Ti$_{2}$Cu, Ti$_{3}$Cu, and TiCu. 3) .betha.-Ti formed in Ti base metal durig brazing transformed to lamellar structure, .alpha.-Ti + Ti$_{2}$Cu. The structure came from the eutectoil decomposition reaction in cooling. And the width of .betha.-Ti layer was proportional to the square root of brazing time, and it was considered that the growth of .betha.-Ti layer was controlled by interdiffusion rate process in .betha.-Ti. 4) The layer growth of TiCu, Ti$_{3}$Cu$_{4}$ and TiCu, phases formed near the Ti interface was linerface was linearly proportional to the brazing time, and it was considered that the layer growth of these phases was controlled by the chemical reaction rate at the interface.

• Proceedings of the Korean Vacuum Society Conference
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• 2013.02a
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• pp.338-338
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• 2013

Monolithic three-dimensional integrated circuits (3D-ICs) 구현 시 bonding 과정에서 발생되는 aluminum (Al) 이나 copper (Cu) 등의 interconnect metal의 확산, 열적 스트레스, 결함의 발생, 도펀트 재분포와 같은 문제들을 피하기 위해서는 저온 공정이 필수적이다. 지금까지는 polymer 기반의 bonding이나 Cu/Cu와 같은 metal 기반의 bonding 등과 같은 저온 bonding 방법이 연구되어 왔다. 그러나 이와 같은 bonding 공정들은 공정 시 void와 같은 문제가 발생하거나 공정을 위한 특수한 장비가 필수적이다. 반면, 두 물질의 합금을 이용해 녹는점을 낮추는 eutectic bonding 공정은 저온에서 공정이 가능할 뿐만 아니라 void의 발생 없이 강한 bonding 강도를 얻을 수 있다. Aluminum-germanium (Al-Ge) 및 aluminum-indium (Al-In) 등의 조합이 eutectic bonding에 이용되어 각각 $424^{\circ}C$ 및 $454^{\circ}C$의 저온 공정을 성취하였으나 여전히 $400^{\circ}C$이상의 eutectic 온도로 인해 3D-ICs의 구현 시에는 적용이 불가능하다. 이러한 metal 조합들에 비해 indium (In)과 tin (Sn)은 각각 $156^{\circ}C$ 및 $232^{\circ}C$로 굉장히 낮은 녹는점을 가지고 있기 때문에 In-Sn 조합은 약 $120^{\circ}C$ 정도의 상당히 낮은eutectic 온도를 갖는다. 따라서 본 연구팀은 In-Sn 조합을 이용하여 $200^{\circ}C$ 이하에서monolithic 3D-IC 구현 시 사용될 eutectic bonding 공정을 개발하였다. 100 nm SiO2가 증착된 Si wafer 위에 50 nm Ti 및 410 nm In을 증착하고, 다른Si wafer 위에 50 nm Ti 및 500 nm Sn을 증착하였다. Ti는 adhesion 향상 및 diffusion barrier 역할을 위해 증착되었다. In과 Sn의 두께는 binary phase diagram을 통해 In-Sn의 eutectic 온도인 $120^{\circ}C$ 지점의 조성 비율인 48 at% Sn과 52 at% In에 해당되는 410 nm (In) 그리고 500 nm (Sn)로 결정되었다. Bonding은 Tbon-100 장비를 이용하여 $140^{\circ}C$, $170^{\circ}C$ 그리고 $200^{\circ}C$에서 2,000 N의 압력으로 진행되었으며 각각의 샘플들은 scanning electron microscope (SEM)을 통해 확인된 후, 접합 강도 테스트를 진행하였다. 추가로 bonding 층의 In 및 Sn 분포를 확인하기 위하여 Si wafer 위에 Ti/In/Sn/Ti를 차례로 증착시킨 뒤 bonding 조건과 같은 온도에서 열처리하고secondary ion mass spectrometry (SIMS) profile 분석을 시행하였다. 결론적으로 본 연구를 통하여 충분히 높은 접합 강도를 갖는 In-Sn eutectic bonding 공정을 $140^{\circ}C$의 낮은 공정온도에서 성공적으로 개발하였다.