Integration of ALD-TaN Liners on Nanoporous Dielectrics

2005 ◽  
Vol 863 ◽  
Author(s):  
Bum Ki Moon ◽  
Tadashi Iijima ◽  
Sandra Malhotra ◽  
Andrew Simon ◽  
Thomas Shaw ◽  
...  

AbstractUltra-thin ALD-TaN/PVD-Ta liners have been developed to prevent Cu diffusion into porous interlayer dielectric (ILD) materials envisioned for future copper interconnections. The porous ultra-lowk(p-ULK) film is prepared using the spin-on method, and typical k-value and the average pore size of p-ULK used in this paper are 2.3 and 2-3 nm, respectively. Interaction and phenomena at the ILD/ALD-TaN interface have been investigated, and the electrical measurements of samples with a bi-layered ALD-TaN/PVD-Ta barrier were performed after completing the metallization and CMP process.A deep penetration of ALD-TaN was observed on the as-deposited p-ULK, which is due to the interconnected pore structures. However, the surface of the p-ULK is drastically changed after the etch process, where changes are attributed to plasma damage and re-deposition of etched species. Pores can therefore be sealed during the etch process. Furthermore, the plasma damage makes the sidewall more hydrophilic, which may promote the growth of ALD-TaN layer. Based on EELS and EDS profiles, there is no signature of TaN penetration into the etched p-ULK at M1 level with a sharp Ta peak, which indicates excellent stability of ultra-thin ALD-TaN liner.An oxidation test in air ambient and at elevated temperature confirmed the barrier properties of the stacked ALD-TaN/PVD-Ta layers. Any weak point in the barrier allows the Cu to oxidize and to make a color change under an optical microscope. However, all of our samples showed no color change, which implies that the barrier is very uniform and stable. Electrical properties measured at M1 showed excellent results. Our results demonstrate the ability to successfully integrate ALD-TaN barriers with a nanoporous ULK film.

2000 ◽  
Author(s):  
K. Thangaraj ◽  
Y. C. Chen ◽  
K. Salama

Abstract Porous equi-atomic NiTi Shape Memory Samples were fabricated using the Elemental Powder Sintering technique for varying starting powder sizes of Ni and Ti. The porosity was primarily dependent on the starting powder sizes, and less dependent on the sintering parameters and compaction loads. Sintering at higher temperatures of 1120°C and 48 hrs resulted in a completion of reaction to equilibrium NiTi. The average pore size was found to be in proportion to the starting powder size. The martensitic-austenitic transformations as determined from the electrical measurements had a broad transformation behavior. Compressive tests performed on the sample showed a recoverable strain of up to 2.5 %.


2009 ◽  
Vol 1156 ◽  
Author(s):  
Ivan Ciofi ◽  
Mikhail R. Baklanov ◽  
Giovanni Calbo ◽  
Zsolt Tőkei ◽  
Gerald Beyer

AbstractWe evaluated Triangular Voltage Sweep (TVS) measurements as a technique to characterize plasma damage in low-k films. Blanket wafers with low-k films of different porosity and k value were prepared. Our samples included an SiOC:H material with 7% porosity and k value of 3.0, deposited on 200mm wafers, and two SiOC:H materials with 25% porosity and k value of 2.5, deposited on 300mm wafers. Before deposition, a thin layer of dry thermal oxide (2 – 5 nm) was grown on the n-type wafers to stabilize the silicon interface. After deposition, low-k films were exposed to N2/H2 plasma for different times in order to induce different degree of plasma damage. Untreated low-k films were always included as a reference. For electrical measurements, metal dots were deposited on pieces to fabricate Metal-Insulator-Semiconductor capacitors.TVS measurements were performed at 190°C on the different samples. On samples exposed to N2/H2 plasma, we detected a current peak in the TVS trace, whose magnitude increased with exposure time to plasma. No peaks were detected on untreated films. This indicates that TVS measurements are sensitive to plasma damage. Furthermore, TVS results correlated well with FTIR spectra that showed increasing damage and H2O uptake with increasing exposure time to plasma. We conclude that TVS measurements are suitable for characterizing the degree of plasma damage in low-k films and complement well materials analysis, because with the help of TVS a link to leakage properties can be made. As an application, we used TVS measurements for evaluating restoration of plasma damaged low-k films by long N2-bake at high temperature. Wafer pieces from each sample were baked at 350°C for 4h30min in N2 atmosphere. A few pieces were measured immediately after baking. The remaining pieces were either left exposed to ambient for a few days or dipped in deionized H2O for a few hours to evaluate recovery of hydrophobic properties. The different treatments (N2-bake, exposure to ambient, H2O dipping) were always performed on blanket wafer pieces. Metal dots for electrical measurements were only deposited after the treatment. CV and FTIR measurements were performed before and after treatments to evaluate change in k-value and material structure, respectively. Our data show that long N2-bake at high temperature can partially restore damaged low-k films. The magnitude of the damage-related TVS peak was significantly reduced after heat treatment and remained stable even after H2O dipping. CV measurements performed on baked pieces after 6 days of exposure to ambient showed a reduced k-value. Consistently, FTIR spectra showed a significant reduction of H2O content soon after baking. The materials remained stable over several days and only minor reincorporation of H2O occurred after exposure to ambient or H2O dipping. Therefore, long N2-bake at high temperature can partially restore leakage (TVS), k-value (CV) and hydrophobic properties (FTIR) of damaged low-k films.


2010 ◽  
Vol 177 ◽  
pp. 329-333 ◽  
Author(s):  
Qian Ping Wang ◽  
Xiu Shu Tian ◽  
Shu Xian Liu ◽  
Wei Hua Wu ◽  
Zhuan Hong Huang ◽  
...  

Membrane separation process, which greatly meets the demand of reducing the environmental pollution in the modern industry, has become one of the most important strategies in the durative low carbon economy development.. This paper has studied the transformation structure mechanism of of Al2O3-SiO2-ZrO2 composite membrane produced by the sol-gel method on a porous α-Al2O3 support and the effects of SiO2 and ZrO2 in γ-Al2O3 membrane. Porous Al2O3-SiO2-ZrO2 composite membrane of the average pore size 2~4µm was obtained first time through controlling various factors, The structure crystal type and surface state are characterized by means of optical microscope, XRD, SEM, and IR. The results show that the membrane calcined at 1000°C obtain a composition of γ-Al2O3, t-ZrO2 and amorphous SiO2. The phase transformation has not appeared when heated at 1200°C. As the thermostability of the modified membrane being improved, the phase transformation temperature in the sintering process could be delayed. Therefore, the membranes properties are greatly improved.


2017 ◽  
Vol 54 (3) ◽  
pp. 181-201
Author(s):  
Rebecca Johnson ◽  
Mark Longman ◽  
Brian Ruskin

The Three Forks Formation, which is about 230 ft thick along the southern Nesson Anticline (McKenzie County, ND), has four “benches” with distinct petrographic and petrophysical characteristics that impact reservoir quality. These relatively clean benches are separated by slightly more illitic (higher gamma-ray) intervals that range in thickness from 10 to 20 ft. Here we compare pore sizes observed in scanning electron microscope (SEM) images of the benches to the total porosity calculated from binned precession decay times from a suite of 13 nuclear magnetic resonance (NMR) logs in the study area as well as the logarithmic mean of the relaxation decay time (T2 Log Mean) from these NMR logs. The results show that the NMR log is a valid tool for quantifying pore sizes and pore size distributions in the Three Forks Formation and that the T2 Log Mean can be correlated to a range of pore sizes within each bench of the Three Forks Formation. The first (shallowest) bench of the Three Forks is about 35 ft thick and consists of tan to green silty and shaly laminated dolomite mudstones. It has good reservoir characteristics in part because it was affected by organic acids and received the highest oil charge from the overlying lower Bakken black shale source rocks. The 13 NMR logs from the study area show that it has an average of 7.5% total porosity (compared to 8% measured core porosity), and ranges from 5% to 10%. SEM study shows that both intercrystalline pores and secondary moldic pores formed by selective partial dissolution of some grains are present. The intercrystalline pores are typically triangular and occur between euhedral dolomite rhombs that range in size from 10 to 20 microns. The dolomite crystals have distinct iron-rich (ferroan) rims. Many of the intercrystalline pores are partly filled with fibrous authigenic illite, but overall pore size typically ranges from 1 to 5 microns. As expected, the first bench has the highest oil saturations in the Three Forks Formation, averaging 50% with a range from 30% to 70%. The second bench is also about 35 ft thick and consists of silty and shaly dolomite mudstones and rip-up clast breccias with euhedral dolomite crystals that range in size from 10 to 25 microns. Its color is quite variable, ranging from green to tan to red. The reservoir quality of the second bench data set appears to change based on proximity to the Nesson anticline. In the wells off the southeast flank of the Nesson anticline, the water saturation averages 75%, ranging from 64% to 91%. On the crest of the Nesson anticline, the water saturation averages 55%, ranging from 40% to 70%. NMR porosity is consistent across the entire area of interest - averaging 7.3% and ranging from 5% to 9%. Porosity observed from samples collected on the southeast flank of the Nesson Anticline is mainly as intercrystalline pores that have been extensively filled with chlorite clay platelets. In the water saturated southeastern Nesson Anticline, this bench contains few or no secondary pores and the iron-rich rims on the dolomite crystals are less developed than those in the first bench. The chlorite platelets in the intercrystalline pores reduce average pore size to 500 to 800 nanometers. The third bench is about 55 ft thick and is the most calcareous of the Three Forks benches with 20 to 40% calcite and a proportionate reduction in dolomite content near its top. It is also quite silty and shaly with a distinct reddish color. Its dolomite crystals are 20 to 50 microns in size and partly abraded and dissolved. Ferroan dolomite rims are absent. This interval averages 7.1% porosity and ranges from 5% to 9%, but the pores average just 200 nanometers in size and occur mainly as microinterparticle pores between illite flakes in intracrystalline pores in the dolomite crystals. This interval has little or no oil saturation on the southern Nesson Anticline. Unlike other porosity tools, the NMR tool is a lithology independent measurement. The alignment of hydrogen nuclei to the applied magnetic field and the subsequent return to incoherence are described by two decay time constants, longitudinal relaxation time (T1) and transverse relaxation time (T2). T2 is essentially the rate at which hydrogen nuclei lose alignment to the external magnetic field. The logarithmic mean of T2 (T2 Log Mean) has been correlated to pore-size distribution. In this study, we show that the assumption that T2 Log Mean can be used as a proxy for pore-size distribution changes is valid in the Three Forks Formation. While the NMR total porosity from T2 remains relatively consistent in the three benches of the Three Forks, there are significant changes in the T2 Log Mean from bench to bench. There is a positive correlation between changes in T2 Log Mean and average pore size measured on SEM samples. Study of a “type” well, QEP’s Ernie 7-2-11 BHD (Sec. 11, T149N, R95W, McKenzie County), shows that the 1- to 5-micron pores in the first bench have a T2 Log Mean relaxation time of 10.2 msec, whereas the 500- to 800-nanometer pores in the chlorite-filled intercrystalline pores in the second bench have a T2 Log Mean of 4.96 msec. This compares with a T2 Log Mean of 2.86 msec in 3rd bench where pores average just 200 nanometers in size. These data suggest that the NMR log is a useful tool for quantifying average pore size in the various benches of the Three Forks Formation.


2006 ◽  
Vol 514-516 ◽  
pp. 1005-1009 ◽  
Author(s):  
José V. Araújo ◽  
J.A. Lopes da Silva ◽  
Margarida M. Almeida ◽  
Maria Elisabete V. Costa

Porous chitosan/brushite composite scaffolds were prepared by a freeze-drying technique, starting from brushite suspensions in chitosan solutions. The obtained scaffolds showed a regular macroporous and interconnected structure with brushite particles uniformly distributed in the chitosan matrix. The variation of the brushite concentration affected the microstructure of the final freeze-dried scaffold, in particular, its porosity and its average pore size. The yield strengths of the composite scaffolds could also be improved by the increase of the brushite content.


2021 ◽  
Vol 13 (14) ◽  
pp. 7593
Author(s):  
Farooq Khan Niazi ◽  
Malik Adeel Umer ◽  
Ashfaq Ahmed ◽  
Muhammad Arslan Hafeez ◽  
Zafar Khan ◽  
...  

Ultrafiltration membranes offer a progressive and efficient means to filter out various process fluids. The prime factor influencing ultrafiltration to a great extent is the porosity of the membranes employed. Regarding membrane development, alumina membranes are extensively studied due to their uniform porosity and mechanical strength. The present research work is specifically aimed towards the investigation of nanoporous alumina membranes, as a function of sintering parameters, on ultrafiltration performance. Alumina membranes are fabricated by sintering at various temperatures ranging from 1200–1300 °C for different holding times between 5–15 h. The morphological analysis, conducted using Scanning electron microscopy (SEM), revealed a homogeneous distribution of pores throughout the surface and cross-section of the membranes developed. It was observed that an increase in the sintering temperature and time resulted in a gradual decrease in the average pore size. A sample with an optimal pore size of 73.65 nm achieved after sintering at 1250 °C for 15 h, was used for the evaluation of ultrafiltration performance. However, the best mechanical strength and highest stress-bearing ability were exhibited by the sample sintered at 1300 °C for 5 h, whereas the sample sintered at 1250 °C for 5 h displayed the highest strain in terms of compression. The selected alumina membrane sample demonstrated excellent performance in the ultrafiltration of sugarcane juice, compared to the other process liquids.


Molecules ◽  
2021 ◽  
Vol 26 (2) ◽  
pp. 257
Author(s):  
Jie Ren ◽  
Nanwei Chen ◽  
Li Wan ◽  
Guojian Li ◽  
Tao Chen ◽  
...  

In this study, a new method for economical utilization of coffee grounds was developed and tested. The resulting materials were characterized by proximate and elemental analyses, thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and N2 adsorption–desorption at 77 K. The experimental data show bio-oil yields reaching 42.3%. The optimal activated carbon was obtained under vacuum pyrolysis self-activation at an operating temperature of 450 °C, an activation temperature of 600 °C, an activation time of 30 min, and an impregnation ratio with phosphoric acid of 150 wt.%. Under these conditions, the yield of activated carbon reached 27.4% with a BET surface area of 1420 m2·g−1, an average pore size of 2.1 nm, a total pore volume of 0.747 cm3·g−1, and a t-Plot micropore volume of 0.428 cm3·g−1. In addition, the surface of activated carbon looked relatively rough, containing mesopores and micropores with large amounts of corrosion pits.


2005 ◽  
Vol 885 ◽  
Author(s):  
Krithi Shetty ◽  
Shihuai Zhao ◽  
Wei Cao ◽  
Naidu V. Seetala ◽  
Debasish Kuila

ABSTRACTThe goal of this research is to investigate the activities of a non-noble nano-catalyst (Ni/SiO2) using Si-microreactors for steam reforming of methanol to produce hydrogen for fuel cells. The supported catalyst was synthesized by sol-gel method using Ni (II) salts and Si(C2H5O)4 as starting materials. EDX results indicate that the actual loading of Ni (5-6%) is lower than the intended loading of 12 %. The specific surface area of the silica sol-gel encapsulated Ni nano-catalyst is 452 m2/g with an average pore size of ∼ 3 nm. Steam reforming reactions have been carried out in a microreactor with 50 µm channels in the temperature range of 180-240 °C and atmospheric pressure. Results show 53% conversion of methanol with a selectivity of 74 % to hydrogen at 5 l/min and 200 °C. The magnetic properties of the catalysts were performed using a Vibrating Sample Magnetometer (VSM) to study the activity of the catalysts before and after the steam reforming reactions. The VSM results indicate much higher activity in the microreactor compared to macro-reactor and Ni forms non-ferromagnetic species faster in the microreactor.


2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
Huaxing Xu ◽  
Biao Gao ◽  
Hao Cao ◽  
Xueyang Chen ◽  
Ling Yu ◽  
...  

Nanoporous activated carbon material was produced from the waste rice husks (RHs) by precarbonizing RHs and activating with KOH. The morphology, structure, and specific surface area were investigated. The nanoporous carbon has the average pore size of 2.2 nm and high specific area of 2523.4 m2 g−1. The specific capacitance of the nanoporous carbon is calculated to be 250 F g−1at the current density of 1 A g−1and remains 80% for 198 F g−1at the current density of 20 A g−1. The nanoporous carbon electrode exhibits long-term cycle life and could keep stable capacitance till 10,000 cycles. The consistently high specific capacitance, rate capacity, and long-term cycle life ability makes it a potential candidate as electrode material for supercapacitor.


2000 ◽  
Vol 612 ◽  
Author(s):  
Sylvie Acosta ◽  
André Ayral ◽  
Christian Guizard ◽  
Charles Lecornec ◽  
Gérard Passemard ◽  
...  

AbstractPorous silica exhibits attractive dielectric properties, which make it a potential candidate for use as insulator into interconnect structures. A new way of preparation of highly porous silica layers by the sol-gel route was investigated and is presented. The synthesis strategy was based on the use of common and low toxicity reagents and on the development of a simple process without gaseous ammonia post-treatment or supercritical drying step. Defect free layers were deposited by spin coating on 200 mm silicon wafers and characterized. Thin layers with a total porosity larger than 70% and an average pore size of 5 nm were produced. The dielectric constant measured under nitrogen flow on these highly porous layers is equal to ∼ 2.5, which can be compared to the value calculated from the measured porosity, ∼ 1.9. This difference is explained by the presence of water adsorbed on the hydrophilic surface of the unmodified silica.


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