In-situtemperature-dependent sheet resistance study of Cu films in oxygen ambient for heterogeneous integrations.

Controlling and preventing Cu oxidation is crucial for improving the performance and reliability of Cu-Cu bonding. Ni-B films were selectively deposited on Cu films to block the Cu oxidation. The resistivity changes of the Cu films in N2and O2ambient were measured by using a four-point probe in thein situtemperature-dependent resistance measurements at the temperature from room temperature to 400 °C. The resistivity changes of the 100 nm thick Cu films without Ni-B increased rapidly at a higher temperature (284 °C) in the O2ambiance. The change of resistivity-increase of 100 nm thick Cu with ∼50 nm thick Ni-B (top) film was lower than the Cu films without Ni-B films due to the blocking diffusion of O2atoms by the Ni-B films. The resistivity-change and oxidation barrier properties were studied using scanning electron microscopy, FIB, transmission electron microscopy, EDX, and secondary ion mass spectroscopy tools. The proposed article will be helpful for the upcoming advancement in Cu-Cu bonding using selected-area deposition.

Thermal, Mechanical, and Electrical Stability of Cu Films in an Integration Process with Photosensitive Polyimide (PSPI) Films.

Photosensitive polyimides (PSPIs) have been widely developed in microelectronics, which is due to their excellent thermal properties and reasonable dielectric properties and can be directly patterned to simplify the processing steps. In this study, 3 µm~7 µm thick PSPI films were deposited on different substrates, including Si, 50 nm SiN, 50 nm SiO2, 100 nm Cu, and 100 nm Al, for the optimization of the process of integration with Cu films. In situ temperature-dependent resistance measurements were conducted by using a four-point probe system to study the changes in resistance of the 70 nm thick Cu films on different dielectrics with thick diffusion films of 30 nm Mn, Co, and W films in a N2 ambient. The lowest possible change in thickness due to annealing at the higher temperature ranges of 325 °C to 375 °C is displayed, which suggests the high stability of PSPI. The PSPI films show good adhesion with each Cu diffusion barrier up to 350 °C, and we believe that this will be helpful for new packaging applications, such as a 3D IC with a Cu interconnect.

Demonstration of TiO2 Based Ultra High-k (k = 30) Metal-Insulator-Semiconductor Capacitor and Its Electrical Properties.

In this paper, we investigated TiO2 as gate dielectric to achieve the large dielectric constant. The ultra high-k value over 30 was obtained by Capacitance-Voltage measurement of Al/Ti/TiO2/Si Metal-Insulator-Semiconductor (MIS) capacitor. Among as deposited, rapid thermal annealing (RTA) at 750 °C and 1000 °C, the RTA at 750 °C showed the lowest gate leakage current. It implies that TiO2 has optimum RTA temperature having the lowest leakage current. When TiO2 is annealed at 750 °C, the phase of TiO2 changes to anatase and interfacial layer between TiOx and Si was formed. While TiO2 is annealed at 1000 °C, the phase of TiO2 changes to rutile and diffusion of silicon atoms was clearly observed and it causes the silicide formation. Based on measurement data, we proposed the energy band diagram of Al/TiO2/Si MIS capacitors. This diagram shows that the energy band gap of RTA at 750 °C is expanded while that of RTA at 1000 °C is contracted. In addition, TiO2 with RTA at 550 °C was tested to confirm leakage current and it shows lower leakage current than RTA at 750 °C as we expected. This result confirmed that optimum RTA temperature of TiO2 would exist under 750 °C.

Highly Fast Response of Pd/Ta2O5/SiC and Pd/Ta2O5/Si Schottky Diode-Based Hydrogen Sensors.

Herein, the fabrication of a novel highly sensitive and fast hydrogen (H2) gas sensor, based on the Ta2O5 Schottky diode, is described. First, Ta2O5 thin films are deposited on silicon carbide (SiC) and silicon (Si) substrates via a radio frequency (RF) sputtering method. Then, Pd and Ni are respectively deposited on the front and back of the device. The deposited Pd serves as a H2 catalyst, while the Ni functions as an Ohmic contact. The devices are then tested under various concentrations of H2 gas at operating temperatures of 300, 500, and 700 °C. The results indicate that the Pd/Ta2O5 Schottky diode on the SiC substrate exhibits larger concentration and temperature sensitivities than those of the device based on the Si substrate. In addition, the optimum operating temperature of the Pd/Ta2O5 Schottky diode for use in H2 sensing is shown to be about 300 °C. At this optimum temperature, the dynamic responses of the sensors towards various concentrations of H2 gas are then examined under a constant bias current of 1 mA. The results indicate a fast rise time of 7.1 s, and a decay of 18 s, for the sensor based on the SiC substrate.

Effect of Palladium Electrode Patterns on Hydrogen Response Characteristics from a Sensor Based on Ta2O5 Film on SiC at High Temperatures.

Our study aims to fabricate a hydrogen sensor based on thermal stability analysis of Ta2O5 film, and to determine the effect of Pd electrodes on the hydrogen sensor at high temperatures. First, in order to ensure high-temperature stability of silicon carbide (SiC)-based hydrogen sensors, the thermal stability of Ta2O5 dielectric thin film at temperatures above 900 °C was studied. The sensor structure consisted of a metal-insulator-semiconductor (MIS) and a tantalum oxide (Ta2O5) dielectric film was formed by rapid thermal oxidation (RTO). The Ta2O5 film was assessed through SEM, TEM, SIMS, and dielectric breakdown strength to observe thermal stability. Secondly, hydrogen sensors using a SiC substrate were fabricated, with the process considering thermal stability. The response characteristics for hydrogen were evaluated using three types of sensors with different Pd electrode patterns. The patterns of the Pd electrode were designed as squares or grid shapes, and were characterized by 100%, 75%, and 50% area ratios of Pd electrodes covering the Ta2O5 layer. The results showed that the sensor with a 100% area ratio of the Pd electrode had better sensitivity and linear response characteristics compared to sensors with a 50% area ratio of the Pd electrode.

Graphene-coated microballs for a hyper-sensitive vacuum sensor.

Reduced graphene oxide (RGO)-coated microballs of poly (methyl methacrylate) (PMMA) used for fabricating three-dimensional sensor (3D sensor), which are expected to exhibit high sensitivity compared with conventional two-dimensional (2D) sensors, were prepared using a reaction-based assembly process. The sheet resistance and transmittance of the RGO-coated balls decreased with increasing number of coatings, implying that the RGO was well adhered to the ball by the assembly method. Two types of vacuum pressure sensors using multiple balls and a single ball were fabricated using lift-off and air-blowing methods, respectively. At pressures <1 torr, the sensors showed an increased resistance value due to the bending of graphene sheets by the Van der Waals attractive force. Further, the pressure versus resistance values at the logarithmic scale showed a linear relation, with a pressure reading error <6%. Compared with the 2D sensor fabricated using RGO, the multiball sensor exhibited almost 4-5 times higher RRC value. The single-ball sensor showed reasonable reproducibility at various temperatures. Given the size and pressure reading range of the sensor, the sensitivity of the single-ball sensor at 100 °C was approximately 6,000 times greater than that of the sensor with the highest sensitivity reported in the literature. The increase in surface area and the geometric effect of the sensing part of the single-ball sensor appeared to be responsible for its abnormally high sensitivity.

Chemical Vapor Deposition Carbon Film as a Capping Layer in 4H-SiC Based MOSFETs.

Radio-frequency plasma enhanced CVD (RF-PECVD) carbon films were grown directly on 4-inch 4H-SiC substrates as a capping layer for MOSFET device applications. An approximately 50-nm-thick CVD carbon capping layer was found to reduce the surface roughness, as determined by atomic force microscopy (AFM). The secondary ion mass spectroscopy (SIMS) depth profile results revealed that carbon capping layer can suppress the dopant out-diffusion on the implanted surface after annealing even at high temperature (1700 °C) for 30 min. The calculated subthreshold swing (S) values of devices with CVD carbon capping layer and photo-resist process (base) measured at room temperature were 460 ± 50 (mV/dec) and 770 ± 70 (mV/dec), respectively. The lower value of 'S' for the device with carbon capping layer was related to the very low density of interface traps at the SiC-SiO2 interface. These results show the potential of CVD carbon as a capping layer for SiC MOSFET device applications.

Self-assembled and intercalated film of reduced graphene oxide for a novel vacuum pressure sensor.

We report a new method for measuring vacuum pressures using Van der Waals (VDW) interactions between reduced graphene oxide (RGO) sheets. For this purpose, we utilized a reaction-based self-assembly process to fabricate various intercalated RGO (i-RGO) films, and monitored their electrical behavior with changing pressure and temperature. Pumping to remove gas from a vacuum chamber produced a decrease in the sheet resistance of i-RGO. With further pumping, distinctly different sheet resistance behaivors were observed depending on the measurement temperature. With increasing vacuum pressure, the resistance increased at 100 °C, whereas it decreased at 30 °C. Two types of VDW interactions are proposed to explain these features: a local VDW interaction between RGO sheets that resulted in V-shaped curves of sheet resistance with pressure changes and broad VDW interactions that occur between RGO sheets when the elastic force required to bend carbon clusters on an RGO sheet exceeds their vibrational energy at low temperatures. On the basis of the results, we propose that the resistance behavior of i-RGO as a function of vacuum pressure can be interpreted as the sum of the two different VDW interactions.

Effect of hydrogen plasma on electroless-plating Ni-B films and its Cu diffusion barrier property.

Electroless-plating Ni-B films have been evaluated for the application as the diffusion barrier and metal cap for copper integration. The effect of post plasma treatment in a hydrogen environment on the characteristics of Ni-B films such as chemical composition, surface roughness, crystallinity, and resistivity was investigated. By treating electroless-plating Ni-B films with H2 plasma, the resistance and the roughness of the films decreased. The leakage current of Ni-B bottom electrode/30-nm-thick Al2O3/Al top electrode structures improved after the H2 plasma treatment on the Ni-B films. 40 nm-thick electroless-plating Ni-B film was able to block Cu diffusion up to 350 degrees C.

Antigenotoxicity of Enzymatic Browning Reaction Products of Potatoes in the Micronucleus Test.

This study investigated the antigenotoxic effects of enzymatic browning reaction products (PEBRPs) obtained by reaction of polyphenol compounds with oxidase extracted from potato. Each of the PEBRPs by themselves at 100 mg/kg did not induce an increased frequency of micronucleated polychromatic erythrocytes (MNPCEs) irrespective of the sampling time (up to 72 h), while the treatment with benzo[a]pyrene (B[a]P) significantly increased the incidence of MNPCEs (P < 0.05). Significant reductions were observed in the frequencies of MNPCEs (P < 0.05) when all PEBRPs were given to the mice 12 h before they were exposed to 100 mg/kg of B[a]P and inhibitory effects were 60%, 70%, and 60% in the catechol (Ca)-PEBRPs, hydroxyhydroquinone (HHQ)-PEBRPs, and pyrogallol (Py)-PEBRPs, respectively. When three kinds of PEBRPs were fed to mice 12 h before injecting 100 mg/kg of B[a]P, the most significant decrease (P < 0.05) in the frequencies of MNPCEs induced by B[a]P were observed and the relative frequency inhibitions by Ca-PEBRPs, HHQ-PEBRPs, and Py-PEBRPs were 70%, 70%, and 60%, respectively. Also, when each type of PEBRP was given to mice one time every day for 5 days, significant reductions were observed in the frequencies of MNPCEs induced by B[a]P (P < 0.05). The strongest relative frequency inhibitions were 60% and 70%, respectively, at 200 mg/kg for Ca-PEBRPs and HHQ-PEBRPs, but Py-PEBRPs had their strongest inhibitory effect at a concentration of 100 mg/kg. These results indicates that enzymatic browning reaction products of potatoes have a strong modulatory effect on B[a]P-induced MNPCEs.