Simultaneous in situ Raman monitoring of the solid and gas phases during the formation and growth of carbon nanostructures inside a cold wall CCVD reactor

Reinhold-López, Karla; Braeuer, Andreas; Romann, Bettina; Popovska-Leipertz, Nadejda; Leipertz, Alfred

doi:10.1016/j.carbon.2014.06.064

Cited by 9 publications

(6 citation statements)

References 47 publications

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“…It is seen as a noninvasive method for controlling the fabrication and morphology of precision thin films. The most frequently used techniques include reflectance anisotropy spectroscopy (RAS), , surface photon absorption (SPA), , and ellipsometry. , Although in situ optical monitoring of nanostructure fabrication is not unseen, − their characterization is largely performed post growth and is often done at the expense of destroying the sample. Real-time in situ optical monitoring could open the door to the scalable and repeatable production of functional nanostructured systems, in particular resonant plasmonic nanostructures, whose optical properties are strongly sensitive to geometrical parameters, including refractive index, size, and shape. , Real-time monitoring can also show the interplay and development of new modes as the growth of complex nanostructures progresses, providing a better understanding of their underlying behavior, but most of all allowing one to design optical functionalities on demand in vivo.…”

Section: Introductionmentioning

confidence: 99%

In Situ Ellipsometric Monitoring of Gold Nanorod Metamaterials Growth

Morgan

Murphy

Hendren

et al. 2017

ACS Appl. Mater. Interfaces

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An in situ transmission-based system has been designed to optically monitor the ellipsometry constants of a hyperbolic plasmonic metamaterial during electrochemical growth. The metamaterial, made from an array of vertically aligned gold nanorods, has demonstrated an unprecedented ability to manipulate the polarization of light using subwavelength thickness slabs, making in situ ellipsometric data a powerful tool in the controlled design of such components. In this work, we show practical proof-of-principle of this design method and rationalize the ellipsometric output on the basis of the modal properties of the nanorod metamaterial. The real-time optical monitoring setup provides excellent control and repeatability of nanostructure growth for the design of future ultrathin optical components. The performance of the ellipsometric method was also tested as a refractive index sensor. Monitoring refractive index changes near the metamaterial’s epsilon near zero (ENZ) frequency showed a sensitivity on the order of 500°/RIU in the ellipsometric phase for a metamaterial that shows 250 nm/RIU sensitivity in its extinction.

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Section: Introductionmentioning

confidence: 99%

In Situ Ellipsometric Monitoring of Gold Nanorod Metamaterials Growth

Morgan

Murphy

Hendren

et al. 2017

ACS Appl. Mater. Interfaces

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“…[32] Amongst the latter,a lmosta ll studies deal with materials adsorbedo ns olid surfaces. [33][34][35][36][37] Other exampless howingt he utility of FT-Raman investigations are known for epoxyr esins [38,39] and diverse other resins. [40][41][42][43][44][45] Selected examples show the application of Ramant echniques for peptide [46][47][48] and flow synthesis [49] or demonstrate the scope of the Ramant echnique, especially due to the fast performance of the experimentsa nd tolerance of watera ss olvent or impurity.D uring our studies on diverse reactions on solid supports, in which we faced the ongoing challenge to provide suitable tools for fast analysis of the resulting immobilised compounds, we found that Ramanm easurements allow fast and reliable interpretation of the reactions.…”

Section: Introductionmentioning

confidence: 99%

“…Whereas IR analysis has already found its way into standard procedures for monitoring solid‐phase reactions and, in selected examples, the progress of the reaction, Raman and surface‐enhanced Raman spectroscopy has been reported only in a few applications for the identification of small compounds on solid phases, probably due to the limited availability of Raman instruments . Amongst the latter, almost all studies deal with materials adsorbed on solid surfaces . Other examples showing the utility of FT‐Raman investigations are known for epoxy resins and diverse other resins .…”

Section: Introductionmentioning

confidence: 99%

Monitoring Reactions on Solid Phases with Raman Spectroscopy

Protasova

Heißler

Jung

et al. 2017

Chemistry A European J

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The benefits of Raman spectroscopy were shown for the on-bead monitoring of diverse reactions. Raman spectroscopy was used for the development of new procedures on established linker systems, the real-time observation of several reactions on solid phases and the estimation of the reaction time for a new cleavage strategy. Selected conversions on solid phases, such as the on-bead conversion of functional groups and the attachment of novel building blocks, were demonstrated. Raman spectra were obtained after isolation and purification of the solid supports, but they were also measured directly in the reaction vessels. Even the detection of Raman-active functional groups in swollen polymer resins and in reaction mixtures was demonstrated, and allows real-time observation of the progress of diverse reactions on solid supports.

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“…Recent years have witnessed an increasingly wider range of in situ IR and Raman. [3][4][5][6][7][8] The monitoring of organic reaction progress continues to be one of the most frequently applications for both spectroscopy techniques. Each technique has its own advantages and disadvantages.…”

Section: Introductionmentioning

confidence: 99%

Monitor Polyimide Production from Diamine and Dianhydride Reactions Using a Combination of In Situ Infrared and Raman Spectroscopy

Chen

Wang²,

Bu³

2017

Appl Spectrosc

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A two-step synthesis of polyimide reaction from dianhydride and diamine was followed by both infrared (IR) and Raman spectroscopy in situ in this case study. In the first step, the two reactants form poly(amide acid), which resulted in substantial spectral changes easily detected by both spectroscopic techniques. The reaction was found to occur rapidly and reached completion within tens of minutes at room temperature. In the second step, trimethylamine (catalyst) and acetic anhydride (dehydration agent) were added to form the five-member imide ring. Interestingly, different spectral changes were observed using IR and Raman spectroscopic methods due to their different responses toward the various functional groups involved. Conclusive evidence was also obtained based on the Raman results to demonstrate a long-lived intermediate species, which was harder to observe in the IR results. This work provides a good case study of the combined use of different vibrational spectroscopy techniques to extract maximum information from a reaction system.

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Simultaneous in situ Raman monitoring of the solid and gas phases during the formation and growth of carbon nanostructures inside a cold wall CCVD reactor

Cited by 9 publications

References 47 publications

In Situ Ellipsometric Monitoring of Gold Nanorod Metamaterials Growth

In Situ Ellipsometric Monitoring of Gold Nanorod Metamaterials Growth

Monitoring Reactions on Solid Phases with Raman Spectroscopy

Monitor Polyimide Production from Diamine and Dianhydride Reactions Using a Combination of In Situ Infrared and Raman Spectroscopy

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