Void-free strong bonding of surface activated silicon wafers from room temperature to annealing at 600 °C

In order to investigate the high temperature application of surface activated silicon/silicon wafer bonding, the wafers were bonded at room temperature and annealed up to 600 °C followed by optical, electrical, mechanical and nanostructure characterization of the interface. Void-free interface with high bonding strength was observed that was independent of the annealing temperature. The bonding strength was as high as 20 MPa. The normalized interfacial current density was increased with the increase in the annealing temperature. A thin interfacial amorphous layer with a thickness of 8.3 nm was found before annealing, which was diminished at 600 °C. A correlation between the current density and nanostructure of the interface was observed as a function of the annealing temperature. The high quality silicon/silicon bonding indicates its potential use not only in low temperature microelectronic applications, but also in high temperature harsh environments.     

Influence of microwave annealing on direct bonded silicon wafers

Strong and nearly void free bonding was achieved using direct bonding followed by microwave annealing. Silicon wafers were cleaned, O₂ plasma surface activated, and bonded at room temperature. After microwave annealing at 400 °C, the bond strength of hydrophilic wafers was found to be in the range between 0.2 and 1.6 J/m². Additional heating of bonded wafers was done at elevated temperatures and for prolonged times using either rapid thermal annealing or microwave annealing. In either case, additional annealing showed no impact on wafer separation area, void, or bond strength. Thus, the initial microwave anneal dictated the ultimate bond strength regardless of subsequent annealing method. The mechanism for wafers bonded in this work involved dipole-dipole bonding and, hydrogen bonding. The initial microwave anneals typically required times less than 60 min. As a result, microwave annealing was shown to be a promising low temperature alternative for wafer bonding when compared to the currently used mechanical furnace anneals.     

低温非晶硅/金圆片键合技术(英文)

本文研究了低温非晶硅/金圆片键合技术.具有不同金硅比的键合片在400℃键合温度和1 MPa键合压力下维持30 min,其键合成功区域均高于94%,平均剪切强度均大于10.1 MPa.键合强度测试结果表明键合成品率与金硅比大小无关,平均剪切强度在10～20 MPa范围内.微观结构分析表明键合后单晶硅颗粒随机分布在键合层内,而金则充满其他区域,形成了一个无空洞的键合层.无空洞键合层确保不同金硅比非晶硅/金键合片均具有较高的键合强度,可实现非晶硅/金键合技术在圆片键合领域的应用.     

Interfacial adhesion of polymeric adhesive film on different surfaces in the fabrication of polymer photonic devices

One main critical issue in the fabrication of polymer optical devices is the adhesion strength of polymeric layer to the substrate. High adhesion strength is desirable and critical in order to avoid peeling out of polymeric layer from the substrate due to stress generated during fabrication, handling and lifetime. Therefore, the aim of this study is to investigate the interfacial adhesion of polymeric adhesive film on different possible substrate surfaces such as pure silicon wafer, silica on silicon wafer, and thin metal layer (Chromium–Cr) on silicon wafer under different processing conditions. Surface morphology of the substrates before deposition was characterized by atomic force microscope (AFM). Adhesive shear button was made on those substrates by using photolithography process and the interfacial adhesion was measured by using a Dage D2400 shear tester. The effect of exposing in high temperature and typical damp heat condition on the interfacial adhesion was also studied. We found that the best adhesion performance was obtained for the case using Cr thin in all processing conditions, especially under heat treatment and damp heat test. From this study, we suggest that a thin layer of metal film on silicon wafer can be use to improve the adhesion and the reliability of the polymer photonic devices. The oxidized silica on silicon wafer is an alternative choice at the expense of reducing adhesion performance. Moreover, using silica layer has the advantage over Cr layer that one fabrication step can be reduced since the silica layer itself can effectively act as the lower cladding of the devices.     

Microelectromechanical system pressure sensor integrated onto optical fiber by anodic bonding

Optical microelectromechanical system pressure sensors based on the principle of Fabry-Perot interferometry have been developed and fabricated using the technique of silicon-to-silicon anodic bonding. The pressure sensor is then integrated onto an optical fiber by a novel technique of anodic bonding without use of any adhesives. In this anodic bonding technique we use ultrathin silicon of thickness 10 microm to bond the optical fiber to the sensor head. The ultrathin silicon plays the role of a stress-reducing layer, which helps the bonding of an optical fiber to silicon having conventional wafer thickness. The pressure-sensing membrane is formed by 8 microm thick ultrathin silicon acting as a membrane, thus eliminating the need for bulk silicon etching. The pressure sensor integrated onto an optical fiber is tested for static response, and experimental results indicate degradation in the fringe visibility of the Fabry-Perot interferometer. This effect was mainly due to divergent light rays from the fiber degrading the fringe visibility. This effect is demonstrated in brief by an analytical model.     

Wafer Scale Solventless Adhesive Bonding with iCVD Polyglycidylmethacrylate: Effects of Bonding Parameters on Adhesion Energies

Initiated chemical vapor deposition (iCVD) polyglycidylmethacrylate (PGMA) thin films are investigated as adhesives for wafer‐scale bonding of 300 mm silicon substrates and demonstrated to form highly uniform, void‐free bond interfaces. The effects of bonding temperature and pressure on critical adhesion energy (G_c) between iCVD PGMA and silicon are studied using the four‐point bend technique. G_c values can be varied over an order of magnitude (0.59–41.6 J m⁻²) by controlling the bonding temperature and the observed dependence is attributed to changes in the physical (diffusion) and chemical (crosslinking) properties of the film. Thermal degradation studies using spectroscopic ellipsometry reveal that the iCVD PGMA films can crosslink when annealed above 120 °C in air. Further, changes in polymer behavior associated with annealing temperature are demonstrated to influence the crack propagation interface between the bonded substrates. These findings demonstrate the feasibility of iCVD polymer films for both temporary “thermoplastic,” and permanent “thermoset” bonding with potential applications in 3D integrated circuit technologies.     

Effect of electrospark deposited surface layers on bond strength of titanium–porcelain

Abstract

Casting of titanium can be successfully used in prosthodontic applications, but it demands special machines and protection gas to avoid oxidation of the metal. The aims of this study are to investigate the bond compatibility between porcelain and titanium using three-point bending, oxide adherence and thermal expansion tests, and to compare the results with those of a conventional titanium–porcelain system. Titanium alloy surfaces were modified with Nb, YG8 and silicon electrode by electrospark surface modification process. The effect of electrospark surface depositing (ESD) layers on bond strength of titanium to porcelain was evaluated comparatively. Some reasons about bond strength of titanium to porcelain were discussed. Results indicate that ESD modified layer prepared in atmosphere using Si electrode can obtain the strongest bonding to porcelain. The ESD modified layer show metallurgical bond to Ti substrate. In addition, the facts that rough surface can help to improve physic bond, similar nature can also help to chemical link and compact ESD layer represent good high temperature oxidation resistance are the reasons that enhance good bond strength of titanium to porcelain.     

Anodic bonding of silicon onto glass by ion-cut technique and their characterization using high resolution X-ray diffraction studies

Anodic bonding of single crystal silicon wafer with glass and subsequent splitting of the silicon wafer is done by ion-cut technique that involves proton bombardment at desired energies at a dose level > 5 × 10¹⁶ cm^− 2 and then subjected to the bond pair for heat treatment at ∼ 550 °C. Details of the bonding and splitting processes have been discussed in the present study. The high resolution X-ray diffractometry studies have been performed and found that transferred single crystalline thin silicon layer has less crystalline perfection than the original wafer. It suggests that some improvement is still required in the ion-cut technique to improve the crystalline quality of the transferred layer before going to be used for the device applications.     

Diffusion bonding of zirconia to silicon nitride using nickel interlayers

The possibilities of diffusion bonding of zirconia to silicon nitride using a nickel interlayer were studied by carrying out bonding experiments under various processing conditions. The process parameters considered were temperature, bonding pressure and interlayer thickness. The optimal process conditions were determined by evaluating the mechanical strength using shear strength testing. It was found that the bonding is optimal in the temperature range 1000–1100°C. The bond strength appears to be independent of the bonding pressure and interlayer thickness if threshold values are exceeded (bonding pressure >14 MPa, interlayer thickness >0.2 mm). At the Si3N4 Ni interface, Si3N4 decomposes, forming a solid solution of silicon in nickel. At the ZrO2–Ni interface, no reaction was observed. © 1998 Kluwer Academic Publishers     

The effect of water desorption and organosilane coupling agents on the adhesion of poly(p-xylylene) films to a silicon wafer surface

The adhesion strength of a poly(p-xylylene) (PPX) film to a silicon wafer surface deposited from the vapor was studied using a peel test method. It was found that, within the time and the temperature range studied in this work, the adhesion strength increases with the time and the temperature of the vacuum desiccation of the surface prior to the deposition of the film. This shows that the presence of water adsorbed on the surface strongly decreases the adhesion strength of the film. The effect of organosilane coupling agents on the adhesion of the film to the silicon wafer surface was studied for organosilane derivatives of different chemical compositions. It was found that the adhesion strength can be significantly improved by the presence of 3-(trimethoxysilyl)propyl methacrylate vapor before or during the poly(p-xylylene) deposition. No significant effect on PPX film adhesion was observed for other organosilanes having the propylmethacrylate group replaced by phenyl or alkyl groups. It was found that, in contrast to the other organosilanes, the recrystallization of the PPX from solution did not remove the methacrylate organosilane which remained bonded to the PPX crystals. It is suggested that chemical bonding between the methacrylic group and the PPX chain end radicals is responsible for the improved adhesion of the PPX films.     

液相连接氮化硅陶瓷的结合强度研究

本文用玻璃焊料研究了氮化硅陶瓷的液相连接,探讨了组份（0～10wt％α－Si₃N₄）、温度（1450～1650℃）和保温时间（10～120min）对结合强度的影响规律．结果表明,α－Si₃N₄的加入提高了液态焊料的粘度,降低了焊料的流动性,导致结合强度下降．采用组份为不含α－Si₃N₄的纯氧化物玻璃焊料在1600℃、保温30min可以得到较为理想的结合强度．     

Effect of rolling temperature on interface and bond strength development of roll bonded copper/aluminium metal laminates

Copper/aluminium laminates were prepared by roll bonding at different temperatures between 350 and 500°C. The effect of the roll bonding temperature on the interface reactions and bond strength development of the laminates was investigated. It was found that the bond strength of the laminates was generally enhanced with increased roll bonding temperature up to 430°C. Optimum roll bonding conditions, in terms of maximum bond strength were identified. It is shown that the development of the optimum bonding between the metal laminates is related to the creation of physical contact between the metals in the roll bonding stage and the formation of various intermetallic phases at the interface during the subsequent sintering process. The formation of intermetallic phases is greatly affected by the diffusivity of the metallic elements across the interface. It has been identified that dissolution of the interfacial oxide layer, formed in the roll bonding stage, has a great influence on the diffusivity of metallic elements across the interface which in turn determines the bond strength development of the material.     

Fluxless bonding of silicon wafers to molybdenum substrates using electroplated tin-rich solder

A novel fluxless bonding process of silicon wafer on molybdenum substrate is successfully developed. Si-to-Mo bonding can be used for packaging power devices, especially when a device consists of an entire wafer. 300 Å Cr layer and 1,000 Å Au layer are first deposited on Si wafers and Mo substrates. The Cr/Au dual layer is used as underbump metallurgy and seed layer of electroplating. To reduce plastic shear strain on the solder in a bonded pair, thick Sn layer (70 μm) is electroplated over Mo substrates having Cr/Au structure, followed immediately by thin (0.1 μm) Ag layer. This Ag layer acts as the capping layer to prevent inner Sn from oxidation. The bonding process is performed in 50 millitorrs vacuum to inhibit oxidation. The bonding condition is 290 °C for 15 min without the use of any flux. The bonding layer thickness is controlled at 50 μm by small spacers placed between Si wafer and Mo substrate. Microstructure and composition of the joints are studied under scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX). Scanning acoustic microscopy (SAM) is also used to verify the quality of joints over the entire sample. Without using any flux, high quality and uniform bonding layer is achieved. The composition of the joint is more than 97 at.% Sn. No intermetallic compound layers exist in the joint. This novel fluxless bonding process should be valuable in packaging large high power devices.     

Interfacial microstructure and strength of partial transient liquid-phase bonding of silicon nitride with Ti/Ni multi-interlayer

Partial transient liquid-phase bonding (PTLP bonding) of silicon nitride (Si₃N₄) ceramic has been performed using Ti/Ni multi-interlayer in vacuum at 1273–1423 K. Interfacial microstructures were examined by scanning electron microscope, electron probe micro-analysis, and X-ray diffraction. The joint strength has been measured by four-point bending tests from room temperature up to 1000 °C. Interfacial structure of Si₃N₄/TiN/Ti₅Si₃ + Ti₅Si₄ + Ni₃Si/(NiTi)/Ni₃Ti/Ni is formed after bonding process. The NiTi layer is gradually consumed with simultaneous growth of the reaction layer and the Ni₃Ti layer. The room temperature joint strength is significantly affected by the reaction layer thickness, whereas the elevated temperature joint strength significantly depends on whether the low melting point NiTi layer exists in the joint. The joint strength of more than 100 MPa is retained up to 800 °C as the NiTi layer is completely consumed. A model is proposed to optimize the PTLP bonding parameters for optimizing joint strength at both room temperature and elevated temperature.     

Room temperature photoluminescence property of boron-doped sol-gel silica

Room temperature photoluminescence (PL) of boron-doped silica synthesized by a combined sol-gel and heating process has been investigated. The broad PL band has been resolved into three components centered at 3.7, 3.35 and 2.7 eV, which are assigned to non-bridging oxygen hole centers (NBOHC), carbon-related impurity, and two-fold coordinated silicon atoms, respectively. The intensities of the 3.35 and 2.7 eV bands decrease with the heating temperature increasing, due to oxidation of the corresponding luminescent centers. The effect of boron doping on the formation of intrinsic defects in silica is discussed.     

Ultra-high vacuum direct bonding of a p-n junction GaAs wafer using low-energy hydrogen ion beam surface cleaning

Low-energy hydrogen ion bombardment is used to clean GaAs surfaces. The hydrogen ions produce contamination-free surfaces without changes in surface composition (stoichiometry) and surface roughness. The wafers were brought into contact at room temperature after cleaning under ultra-high vacuum (UHV), and bonded over the whole area (2 inches) without application of external mechanical pressure. After bonding, the p-GaAs/n-GaAs wafer pair was annealed at 200 °C for 30 min under UHV conditions (<5×10⁻¹⁰ mbar) to improve the interface bonding strength and to achieve a full-area wafer bonding.Infrared (IR) imaging of the as-bonded wafers directly reveal the real bonding behaviour. High-resolution transmission electron microscopy images reveal that the wafers have been directly bonded without damage of the crystal lattice or intermediate layer and the interface is smooth. Current-voltage characterization shows near-ideal forward characteristics and the recombination in p-n junction space charge region.     

Investigation on the bond strength of Al-1100/St-12 roll bonded sheets,optimization and characterization

Al-1100/St-12 aluminum clad steel sheets were produced using roll bonding process at different reductions in thickness and with various supplemental annealing treatments. Experiments were conducted by applying the Taguchi method to obtain optimum condition for maximizing the joint strength. The joint strengths of the bi-layer sheets were evaluated by peel test. The Al/Fe intermetallic phases at the joint interface and the peeled surfaces were examined using scanning electron microscopy (SEM). Energy dispersive spectroscopy (EDS) and Vickers microhardness test were performed to characterize the intermetallic compounds. The results indicate that at the optimum condition of 0.50 reduction in thickness, 450 °C annealing temperature and 90 min annealing time, the bond strength reaches to the base aluminum sheet strength. In comparison to the reduction in thickness and annealing time, the annealing temperature has the most influence on the joint strength changes. In general, raising the annealing temperature up to 450 °C, increases the joint strength. However, annealing treatment at 500 °C reduces the strength due to the formation of brittle Al/Fe intermetallic layer at the bond interface. Additionally, increasing the reduction in thickness improves the joint strength.     

水热法制备不同形貌的氧化锌纳米结构

采用水热法,用甲酰胺水溶液和锌片建立反应体系,在不同种晶层上制备出不同形貌的ZnO纳米结构,所用基底有Si片、镀有ZnO薄膜的Si片、镀有ITO薄膜的Si片、涂有ZnO粉末的Si片等,研究了不同的种晶层对ZnO纳米结构的形貌的影响。在不同温度下,分别在镀有ZnO薄膜和ITO薄膜的医用载玻片衬底上生长ZnO纳米结构,研究了温度在水热法中的作用及种晶层对纳米杆长度的影响。实验中用扫描电子显微镜（SEM）和X射线衍射仪（XRD）对纳米聚集体进行了表征。SEM表征结果表明不同种晶层上获得的ZnO纳米结构形貌差异很大;反应时间、甲酰胺水溶液浓度以及反应温度对ZnO纳米阵列形貌都有着一定的影响;在ZnO薄膜上生长的纳米杆较在ITO薄膜上生长的纳米杆长。SEM图像同时表明氧化锌纳米杆随着温度的增大,纳米杆的长度和杆径增大。X射线衍射峰在34.6℃有很强的（002）纤锌矿衍射峰,该峰表明衬底上有高度c轴取向的大面积纳米杆阵列和较好的结晶质量。     

Silicon-to-indium tin oxide coated glass bonding for packaging of field emission arrays fabricated on silicon wafer

A silicon-to-In₂O₃:Sn coated glass bonding has been developed for the package of field emission arrays fabricated on the silicon wafer, utilizing a conventional silicon-to- silicon anodic bonding using the glass layer. A 1.8 m Pyrex #7740 glass layer was deposited on the In₂O₃:Sn coated glass by an electron beam evaporation. It was confirmed that the composition of the glass layer was nearly the same as that of the bulk Pyrex #7740 glass plate. In this work, bonding the silicon and In₂O₃:Sn coated glass was achieved at a temperature of 190 °C with an applied voltage of 60 V_dc. A secondary ion mass spectroscopy analysis was used to confirm the modeled bonding kinetics of the silicon-to-In₂O₃:Sn coated glass.