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Summary

Abstract

Introduction

Protocol

Representative Results

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Materials

References

Engineering

Electrospray Deposition of Uniform Thickness Ge23Sb7S70 and As40S60 Chalcogenide Glass Films

Published: August 19th, 2016

DOI:

10.3791/54379

1Department of Materials Science and Engineering, Clemson University, 2Department of Materials Science and Engineering, Texas A&M University, 3Department of Electrical and Computer Engineering, Texas A&M University, 4College of Optics and Photonics, Center for Research and Education in Optics and Lasers (CREOL), University of Central Florida, 5Department of Materials Science and Engineering, Massachusetts Institute of Technology, 6Department of Mechanical Engineering, Virginia Polytechnic Institute, 7Microphotonics Center, Massachusetts Institute of Technology

A method of uniform thickness solution-derived chalcogenide glass film deposition is demonstrated using computer numerical controlled motion of a single-nozzle electrospray.

Solution-based electrospray film deposition, which is compatible with continuous, roll-to-roll processing, is applied to chalcogenide glasses. Two chalcogenide compositions are demonstrated: Ge23Sb7S70 and As40S60, which have both been studied extensively for planar mid-infrared (mid-IR) microphotonic devices. In this approach, uniform thickness films are fabricated through the use of computer numerical controlled (CNC) motion. Chalcogenide glass (ChG) is written over the substrate by a single nozzle along a serpentine path. Films were subjected to a series of heat treatments between 100 °C and 200 °C under vacuum to drive off residual solvent and densify the films. Based on transmission Fourier transform infrared (FTIR) spectroscopy and surface roughness measurements, both compositions were found to be suitable for the fabrication of planar devices operating in the mid-IR region. Residual solvent removal was found to be much quicker for the As40S60 film as compared to Ge23Sb7S70. Based on the advantages of electrospray, direct printing of a gradient refractive index (GRIN) mid-IR transparent coating is envisioned, given the difference in refractive index of the two compositions in this study.

Chalcogenide glasses (ChGs) are well-known for their broad infrared transmission and amenability to uniform thickness, blanket film deposition 1-3. On-chip waveguides, resonators, and other optical components can then be formed from this film by lithography techniques, and then subsequent polymer coating to fabricate microphotonic devices 4-5. One key application that we seek to develop is small, inexpensive, highly sensitive chemical sensing devices operating in the mid-IR, where many organic species have optical signatures 6. Microphotonic chemical sensors can be deployed in harsh environments, such as near nuclear reactors, where ex....

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Caution: Please consult Material Safety Data Sheets (MSDS) when working with these chemicals, and be aware of the other hazards such as high voltage, mechanical motion of the deposition system, and high temperatures of the hotplate and furnaces utilized.

Note: Begin this protocol with bulk chalcogenide glass, which is prepared by well-known melt-quench techniques 2.

1. Preparation of ChG Solutions

Note: Two solutions are utilized in this study, Ge

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A schematic representation of the serpentine path utilized to obtain uniform thickness films with single nozzle electrospray is shown in Figure 2. Figure 3 shows an example transmission FTIR spectrum of a partially-cured As40S60 film made with serpentine motion of the spray, as well as the spectrum of pure ethanolamine solvent. From the information that can be obtained from the FTIR spectra such as shown in Figure 3,.......

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At the beginning of a uniform thickness film deposited with serpentine motion of the spray relative to the substrate, the film thickness profile is increasing. Once the distance travelled in the y-direction exceeds the diameter of the spray (upon arrival at the substrate), the flow rate becomes approximately equivalent for every point on the substrate, and thickness uniformity is achieved. To determine the appropriate deposition parameters of a uniform thickness electrosprayed film, theoretical film thickness, T, is util.......

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Funding for this work was provided by Defense Threat Reduction Agency contracts HDTRA1-10-1-0073: HDTRA1-13-1-0001.

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Name Company Catalog Number Comments
Ethanolamine Sigma-Aldrich 411000-100ML 99.5% purity
Si wafer University Wafer 1708 Double side polished, undoped
Syringe Sigma-Aldrich 20788 Hamilton 700 series, 50 microliter volume
Syringe pump Chemyx Nanojet
CNC milling machine MIB instruments CNC 3020
Power supply Acopian P015HP4 AC-DC power supply, 15 kV, 4 mA

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