Dielectric Recovery of Plasma Damaged Organosilicate Low-k Films

2008 ◽  
Vol 1079 ◽  
Author(s):  
Huai Huang ◽  
Junjing Bao ◽  
Huai Huang ◽  
Junjun Liu ◽  
Ryan Scott Smith ◽  
...  
Keyword(s):  
Thermal Activation ◽  
Surface Region ◽  
Surface Hydrophobicity ◽  
Moisture Uptake ◽  
Oh Groups ◽  
Pristine Sample ◽  
Physisorbed Water ◽  
Aging Test ◽  
Carbon Recovery ◽  
Low K

ABSTRACTMethyl depletion and subsequent moisture uptake have been found to be the primary plasma damages leading to dielectric loss in porous organosilicate (OSG) low-k dielectrics. A vacuum vapor silylation process was developed for dielectric recovery of plasma damaged OSG low-k dielectrics. The methyl or phenyl containing silylation agents were used to convert the hydrophilic -OH groups to hydrophobic groups. Compared with Trimethylchlorosilane (TMCS) and Phenyltrimethoxysilane (PTMOS), Dimethyldichlorosilane (DMDCS) was found to be more effective in recovering surface carbon concentration and surface hydrophobicity. But the carbon recovery effect was limited to the surface region.Alternatively, UV radiation with thermal activation was applied for dielectric recovery of plasma damaged OSG low-k dielectrics. The combined UV/thermal process was found to be efficient in reducing −OH, physisorbed water, and C=O bonds. The dielectric constant was recovered within 5% of the pristine sample and the leakage current was also much reduced. Aging test in air showed that no moisture retake was observed, indicating the repaired film was stable.

Effect of CH4 Plasma Treatment on O2 Plasma Ashed Organosilicate Low-k Dielectrics

2007 ◽  
Vol 990 ◽  
Author(s):  
Hualiang Shi ◽  
Junjing Bao ◽  
Junjun liu ◽  
Huai Huang ◽  
Paul S. Ho ◽  
...  
Keyword(s):  
Plasma Treatment ◽  
Leakage Current ◽  
Photoelectron Spectroscopy ◽  
Depth Profiling ◽  
Surface Region ◽  
Surface Hydrophobicity ◽  
Moisture Uptake ◽  
Recovery Effect ◽  
X Ray ◽  
Low K

ABSTRACTDuring an O2 plasma ashing process, carbon depletion and subsequent moisture uptake caused increase of keff and the leakage current in an organosilicate (OSG) low-k dielectric. For dielectric restoration, additional CH4 plasma treatment on the O2 plasma ashed OSG low-k dielectric was investigated using angle resolved x-ray photoelectron spectroscopy (ARXPS), XPS depth profiling, x-ray reflectivity (XRR), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, and contact angle goniometer. After CH4 plasma treatment on the O2 plasma ashed OSG, the surface carbon concentration and surface hydrophobicity were partially recovered. A dense surface layer containing C=C bonds was found to have formed on the top of the damaged OSG. The C-V hysteresis and the leakage current were reduced as a result of the CH4 plasma treatment. XPS depth profiling revealed that the recovery effect was limited to the surface region.

scholarly journals Moisture Induced Degradation of Porous Low-k Materials

2006 ◽  
Vol 914 ◽  
Author(s):  
Mikhail Baklanov ◽  
David O'Dwyer ◽  
Adam M Urbanowicz ◽  
Quoc Toan Le ◽  
Steven Demuynck ◽  
...  
Keyword(s):  
Water Film ◽  
Internal Surface ◽  
Hydrophobic Surface ◽  
Adsorbed Water ◽  
Bulk Water ◽  
Oh Groups ◽  
Film Bulk ◽  
Low K

AbstractInteraction of moisture with porous low-k films is evaluated by using in situ ellipsometry setup. The adsorbed water amount is calculated from change of refractive index measured during the adsorption. Pristine low-k films reversibly adsorb 2 - 5% of water that reflects presence of constitutive hydrophilic centrums. Plasma and thermal treatments increase the number of hydrophilic centrums. Once the amount of these centrums has reached a certain critical value sufficient to form a continuous water film, bulk water condensation is observed. Change of properties during the water adsorption in the damaged films is not fully reversible. Each additional adsorption cycle increases the dielectric function of the film because of decreasing porosity, increasing skeleton density and shrinkage. The pressure corresponding to the bulk condensation allows us to calculate internal contact angle (internal surface energy) of low-k materials. The water molecules adsorbed on separate OH groups play the role of a catalyst that hydrolyses the siloxane bridges initially present on hydrophobic surface.

Observation of Intrusion Rates of Hexamethyldisilazane During Supercritical Carbon Dioxide Functionalization of Triethoxyfluorosilane Low-k Films

2005 ◽  
Vol 863 ◽  
Author(s):  
P.M. Capani ◽  
P.D. Matz ◽  
D.W. Mueller ◽  
M.J. Kim ◽  
E.R. Walter ◽  
...  
Keyword(s):  
Average Pore Size ◽  
Film Surface ◽  
Adsorbed Water ◽  
Surface Hydrophobicity ◽  
Dielectric Constants ◽  
Average Pore ◽  
Silica Films ◽  
Silylating Agents ◽  
Penetration Behavior ◽  
Low K

AbstractWater adsorption by porous low-k silica films results in increased dielectric constants and is often due to silanol groups on the pore surfaces. Reacting the silanols with silylating agents (e.g., hexamethyldisilazane (HMDS) and trimethylchlorosilane (TMCS)) in supercritical CO2 (SC-CO2) can increase film hydrophobicity and can remove adsorbed water. In porous methylsilsesquioxane (MSQ) films (average pore size ∼ 3-4nm), it has been determined that supercritical silylation reactions do not substantially penetrate beyond the film surface.1,2 In this work we have examined the supercritical penetration behavior of silylating agents in low-k films with larger pore sizes (5-10nm). The depth and extent of reactants was determined by in situ infrared spectroscopy (FTIR), and surface hydrophobicity was examined by contact angle experiments.

The Effect of Ar/H2 Plasma Pretreatments on Porous K=2.0 Dielectrics for Pore Sealing by Self-Assembled Monolayers Deposition

2012 ◽  
Vol 195 ◽  
pp. 146-149 ◽  
Author(s):  
Y. Sun ◽  
J. Swerts ◽  
P. Verdonck ◽  
A. Maheshwari ◽  
J.L. Prado ◽  
...  
Keyword(s):  
Plasma Temperature ◽  
Self Assembled Monolayers ◽  
Hydroxyl Groups ◽  
K Value ◽  
Oh Groups ◽  
Surface Hydroxyl ◽  
Pore Sealing ◽  
Assembled Monolayers ◽  
Self Assembled ◽  
Low K

Self-assembled monolayers (SAMs) deposition is being recently explored to help sealing the pores of a k=2.0 material. In order to enable a covalent chemical low-k surface functionalization by SAMs, a hydroxyl groups density as high as 1 to 2.5 OH groups/nm2 is required. This surface modification must be carefully controlled to confine the k below 10%. In this paper, the effects of plasma temperature, time and power on the SAMs deposition and plasma-induced damage are investigated. The main findings are that there is always a trade-off between surface hydroxyl groups density and bulk damage. A thick modified layer allows the SAM molecules to penetrate inside the pores which results in a decreased porosity and an increased k value with respect to correspondent plasma-treated pristine substrates.

scholarly journals Sorption behavior and hydroxyl accessibility of wood treated with different cyclic N-methylol compounds

2020 ◽  
Vol 55 (35) ◽  
pp. 16561-16575
Author(s):  
Lukas Emmerich ◽  
Michael Altgen ◽  
Lauri Rautkari ◽  
Holger Militz
Keyword(s):  
Cell Wall ◽  
Treated Wood ◽  
Covalent Bond ◽  
Water Vapor Sorption ◽  
Adjacent Cell ◽  
Sorption Behavior ◽  
Moisture Uptake ◽  
Negative Effects ◽  
Oh Groups ◽  
Dimensional Changes

Abstract Cyclic N-methylol compounds such as 1,3-dimethylol-4,5-dihydroxyethyleneurea (DMDHEU) have been used to modify wood and prevent negative effects related to the uptake of moisture. However, the changes in the sorption behavior of wood by treatments with DMDHEU and its derivatives are not fully understood. In the present study, wood blocks were treated with DMDHEU, ether-modified DMDHEU and diethyleneglycolated DMDHEU in order to study the factors that control the changes in moisture uptake in the hygroscopic range (0–95% RH). Dimensional changes of wood blocks during water soaking cycles suggested that the treatments caused a permanent cell wall bulking, whereas the swelling restraint by cross-linking of adjacent cell wall polymers was not permanent. However, the changes in water vapor sorption were not only a result of the cell wall bulking effect that reduced the space in the cell wall to accommodate water. The N-methylol compounds within the wood also provided additional sorption sites, but there was no correlation between absorbed water and accessible OH groups. It was speculated that the co-condensation of the N-methylol compounds with wood polymers had a significant effect on the sorption of the treated wood. At elevated RH, pure resins that were formed by self-condensation took up large quantities of moisture. However, when the N-methylol compounds were heat-cured within the hierarchical structure of wood, the moisture uptake of the treated wood at elevated RH was even lower compared to unmodified wood. Furthermore, the covalent bond formation between wood and resin prolonged the attainment of an equilibrium moisture content.

Effect of Plasma Treatment and TMCTS Vapor Annealing on the Reinforcement of Porous low-k Films

2005 ◽  
Vol 863 ◽  
Author(s):  
Kazuo Kohmura ◽  
Hirofumi Tanaka ◽  
Shunsuke Oike ◽  
Masami Murakami ◽  
Tetsuo Ono ◽  
...  
Keyword(s):  
Mechanical Strength ◽  
Plasma Treatment ◽  
Polymer Network ◽  
Porous Silica ◽  
Argon Plasma ◽  
Silica Films ◽  
Oh Groups ◽  
Vapor Annealing ◽  
Silica Wall ◽  
Low K

AbstractA novel process of TMCTS vapor annealing combined with a plasma treatment has been developed for improving the mechanical strength of porous silica films having ultralow dielectric constant. When porous silica films annealed under 1,3,5,7-tetramethylcyclotetrasiloxane (TMCTS) vapor were treated with argon plasma and then re-treated with TMCTS vapor, the mechanical strength (i.e., elastic modulus, hardness) of the films increased significantly. Results of Fourier transform infrared spectroscopy (FT-IR) suggested an accelerative effect resulted from the plasma treatment on the conversion of Si-CH3 and Si-H groups to Si-OH groups. The latter group appears to react faster with TMCTS from the second annealing to form cross-linked polymer network on the porous silica wall surfaces. The resulting cross-linked network is thought to keep the low permittivity and enhance the mechanical strength of the low-k films.

scholarly journals Chemical modification and characterization of boehmite particles

2008 ◽  
Vol 2 (1) ◽  
pp. 27-32
Author(s):  
Witold Brostow ◽  
◽  
Tea Datashvili ◽  
Keyword(s):  
Fourier Transform ◽  
Water Adsorption ◽  
Surface Characteristics ◽  
Surface Hydrophobicity ◽  
Hydroxyl Groups ◽  
Commercial Alumina ◽  
Inorganic Hybrid ◽  
Oh Groups ◽  
Powder Surface

Polymerizable organic silane molecules 3-(trimethoxysilyl)propylmethacrylate (3MPS) and vinyltri(2-methoxyethoxy)silane (VTMES) have been introduced onto surfaces of high purity Boehmite (a commercial alumina) via hydroxyl groups on the oxides in order to obtain organic-inorganic hybrid “macromonomers”. Changes of surface characteristics have been determined using thermogravimetric analysis (TGA) and Fourier-transform infrared spectroscopy (FTIR). The influence of the type of silane used and modification conditions have been determined. Preheating was applied to some Boehmite samples; it leads to lower concentrations of –OH groups on the powder surface and the adsorption yields lower than in samples without preheating. Modification leads to surface hydrophobicity and thus reduces significantly water adsorption; in TGA we see desorption of water below 423 K only in un-modified Boehmite.

Moisture uptake and dielectric property of methylsilsesquioxane/high-temperature porogen hybrids and porous low-k films

2011 ◽  
Vol 26 (23) ◽  
pp. 2987-2995 ◽  
Author(s):  
Mu-Lung Che ◽  
Jun-Yuan Teng ◽  
Po-Cheng Lai ◽  
Jihperng Leu
Keyword(s):  
High Temperature ◽  
Dielectric Property ◽  
Moisture Uptake ◽  
Image Position ◽  
Low K

Abstract

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