Solubility of bis-(2,2,6,6-tetramethyl-3,5-heptanedionato)copper(II) in mixed supercritical CO2 and H2 systems for application in supercritical fluid deposition of Cu

Momose, Takeshi; Kondo, Aiko; Kamiya, Tatsuya; Yamada, Hideo; Ohara, Junji; Kitamura, Y.; Uchida, Hirohisa; Shimogaki, Yukihiro; Sugiyama, Masakazu

doi:10.1016/j.supflu.2015.04.002

Cited by 7 publications

(9 citation statements)

References 65 publications

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“…The solubility of Cu(tmhd) 2 in a pure supercritical CO 2 system and binary mixtures of SC CO 2 and H 2 was measured by Momose and co-workers. 20 The solubility of Ni(hfac) 21 Antioxidants, such as sodium L-ascorbate and sodium erythorbate monohydrate, have found extensive application in the food industry in recent years, since they can be added to food for preservation in the place of conventional preservatives. Owing to the limited thermal stability of antioxidants, the supercritical fluid technique is a treatment safe enough for those compounds.…”

Section: System Investigatedmentioning

confidence: 99%

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Solubility of Solids in Sub- and Supercritical Fluids: A Review 2010–2017

2017

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A review of the solubility data for solids in sub- and supercritical fluids published in the literature between 2010 and 2017 is presented, including the pressure and temperature ranges and correlation methods. Compounds are categorized into the following groups: pharmaceutical, biological, aromatic, nonaromatic, organometallic, and polymer. The most commonly used solvent is supercritical CO2; some data have also been published for other solvents, such as argon, propane, and fluorinated hydrocarbons.

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Section: System Investigatedmentioning

confidence: 99%

“…The solubility of Cu(tmhd) 2 in a pure supercritical CO 2 system and binary mixtures of SC CO 2 and H 2 was measured by Momose and co-workers …”

Section: System Investigatedmentioning

confidence: 99%

Solubility of Solids in Sub- and Supercritical Fluids: A Review 2010–2017

2017

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“…Deposition procedures were as follows: (a) we enclosed samples and Cu precursor in the reactor. We utilized bis-(2,2,6,6-tetramethyl-3,5-heptanedionato)copper(II) [38] as precursor. The amount of precursor was 10 mg (0.002 mol/L).…”

Section: Experimental Design and Fabricationmentioning

confidence: 99%

Drop-In Test Structure to Evaluate Residual Stress in Conformally Grown Films

Usami

Ota

Higo

et al. 2021

IEEE Trans. Semicond. Manufact.

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We propose and demonstrate a drop-in test structure to visualize and measure the residual stress in the conformally deposited film. For reliable device process of microsystems (such as 3-D MEMS), the residual stress must be controlled through quantitative evaluation at each deposition step. A small drop-in test structure placed near the main sample is suitable for monitoring film characteristics. We developed a free-standing rotating beam stress sensor as the drop-in test structure to visualize and measure the residual stress in conformally deposited films with no additional processes. The dimensions of the developed drop-in test structure chips were 5 mm × 10 mm. For a demonstration, Cu supercritical fluid deposition (SCFD) was performed over the test structure chips under a couple of conditions. The residual stresses in SCFD Cu films were successfully extracted by equation-based analysis.

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“…Cleaning details will be explained in each following section. A chip and a copper precursor powder, bis(2,2,6,6tetramethyl-3.5-heptanedionate), (6) were placed in the precursor crucible in the chamber and firmly clamped with a torque wrench. The weight of Cu in the precursor, w Cu , was varied, where 10 mg of precursor was equivalent to 0.002 mol/L.…”

Section: Scfd Processmentioning

confidence: 99%

“…(5) Carbon dioxide is used as a reaction medium in this study. Carbon dioxide is in the gas phase at room temperature and is solid at low temperature; in the supercritical phase appearing above its critical temperature and pressure, high density, high solubility, (6) and low viscosity can be simultaneously obtained. Most importantly, since there is no surface tension in supercritical fluid, materials can be transported deep into HARNS.…”

Section: Introductionmentioning

confidence: 99%

Influence of Pretreatment on Adhesion Quality of Supercritical-fluid-deposited Cu Film on Si

Usami¹,

Ota²,

Momose³

et al. 2019

Sensors and Materials

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In this paper, we report on the impact of sample preparation methods on the adhesion reproducibility of thin films, considering future applications of supercritical fluid deposition (SCFD) to MEMS/NEMS with high-aspect-ratio micro-and nanostructures (HARMS/ HARNS). Our experiments revealed the importance of careful cleaning before SCFD. The Cu on the samples treated with appropriate cleaning and drying sequences could stick to the sample enduring the adhesive pull-out test. By using a silicon substrate, we confirmed that sample surface contaminations were reduced by cleaning, as observed by a decrease in the carbon peak in field emission Auger electron spectroscopy (FE-AES). At the same time, a subtle roughness increase (of 0.2 nm RMS) after a series of cleaning steps was confirmed by scanning probe microscopy (SPM/AFM) measurement. On the basis of the acquired knowledge, Cu SCFD on Si surfaces was studied. A relatively low temperature (130-150 °C) deposition condition was obtained, with which the produced Cu films exhibited high adhesion on all samples. The deposition of 100-nm-thick Cu was successfully demonstrated on the sidewalls of a Si trench with 450 nm width and 22.5 μm depth (aspect ratio of 50).

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Solubility of bis-(2,2,6,6-tetramethyl-3,5-heptanedionato)copper(II) in mixed supercritical CO2 and H2 systems for application in supercritical fluid deposition of Cu

Cited by 7 publications

References 65 publications

Solubility of Solids in Sub- and Supercritical Fluids: A Review 2010–2017

Solubility of Solids in Sub- and Supercritical Fluids: A Review 2010–2017

Drop-In Test Structure to Evaluate Residual Stress in Conformally Grown Films

Influence of Pretreatment on Adhesion Quality of Supercritical-fluid-deposited Cu Film on Si

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