An Evaluation of Local Thermal Analysis of Polymers on the Sub-Micrometer Scale Using Heated Scanning Probe Microscopy Cantilevers

Fischinger, Thomas; Laher, Martin; Hild, Sabine

doi:10.1021/jp4092859

Cited by 6 publications

(5 citation statements)

References 40 publications

(63 reference statements)

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“…Wollaston probes use bridged metal wires (often Pt-based) attached to a prestructured cantilever basis. ,, Although tip radii of down to 20 nm ,, have been reported using very special treatments, typical apex radii are in the range of some hundreds of nanometers to a few micrometers, ,, which are strongly limiting achievable resolution and positioning accuracy. The second approach uses U-shaped cantilevers, consisting of highly doped Si side-wall elements and low-doped tip areas in between. , Although tip radii below 100 nm can be achieved, , the “active areas” are fully connected with the entire cantilever, representing a huge heat sink. By that, low temperatures are more complicated to access when operated in SThM mode. ,, A combination of both approaches led to the introduction of surface-modified cantilevers: lithography-based methods are used to selectively fabricate metal structures across the tip, which can be understood as structured, conductive atomic force microscopy (C-AFM) tips.…”

Section: Introductionmentioning

confidence: 99%

“…The second approach uses U-shaped cantilevers, consisting of highly doped Si side-wall elements and low-doped tip areas in between. 1,15 Although tip radii below 100 nm can be achieved, 16,17 the "active areas" are fully connected with the entire cantilever, representing a huge heat sink. By that, low temperatures are more complicated to access when operated in SThM mode.…”

Section: Introductionmentioning

confidence: 99%

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Three-Dimensional Nanothermistors for Thermal Probing

Sattelkow¹,

Fröch

Winkler³

et al. 2019

ACS Appl. Mater. Interfaces

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Accessing the thermal properties of materials or even full devices is a highly relevant topic in research and development. Along with the ongoing trend toward smaller feature sizes, the demands on appropriate instrumentation to access surface temperatures with high thermal and lateral resolution also increase. Scanning thermal microscopy is one of the most powerful technologies to fulfill this task down to the sub-100 nm regime, which, however, strongly depends on the nanoprobe design. In this study, we introduce a three-dimensional (3D) nanoprobe concept, which acts as a nanothermistor to access surface temperatures. Fabrication of nanobridges is done via 3D nanoprinting using focused electron beams, which allows direct-write fabrication on prestructured, selfsensing cantilever. As individual branch dimensions are in the sub-100 nm regime, mechanical stability is first studied by a combined approach of finite-element simulation and scanning electron microscopy-assisted in situ atomic force microscopy (AFM) measurements. After deriving the design rules for mechanically stable 3D nanobridges with vertical stiffness up to 50 N m −1 , a material tuning approach is introduced to increase mechanical wear resistance at the tip apex for high-quality AFM imaging at high scan speeds. Finally, we demonstrate the electrical response in dependence of temperature and find a negative temperature coefficient of −(0.75 ± 0.2) 10 −3 K −1 and sensing rates of 30 ± 1 ms K −1 at noise levels of ±0.5 K, which underlines the potential of our concept.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Three-Dimensional Nanothermistors for Thermal Probing

Sattelkow¹,

Fröch

Winkler³

et al. 2019

ACS Appl. Mater. Interfaces

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“…A heated AFM cantilever overcomes this barrier but a delicate calibration is needed. 30 Another challenge is to probe the T g of partly (thin films) or entirely (dots) spatially confined materials. Ellison et al have succeeded, for the first time, to measure the T g distribution in nanoscopically confined structures through fluorescence of a pyrene-labeled polystyrene film.…”

mentioning

confidence: 99%

“…However, these tools often require macroscopic heating/cooling of the whole specimen. A heated AFM cantilever overcomes this barrier but a delicate calibration is needed …”

mentioning

confidence: 99%

Nanoscale Sensing Vitrification of 3D Confined Glassy Polymers Through Refractory Thermoplasmonics

et al. 2021

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Advances in plasmonics have been fundamentally rooted in minimizing ohmic losses in metallic nanostructures. However, the losses at resonance can play a positive role; for instance, in optical heating, there are two sides to every story. Under laser illumination, plasmonic nanostructures serve not only as near-field enhancers but heat generators. The emerging field of thermoplasmonics opens up unprecedented possibilities to probe temperature-dependent phase transitions locally. In this paper, we develop a new approach behind plasmon-assisted optical heating for spectroscopically recognizing the glass transition temperature (T g) of spatially confined poly(methyl methacrylate) (PMMA) polymers deposited on a square-shaped titanium nitride (TiN) pad. A local photoheating is controlled through Raman thermometry of a c-Si (100) substrate that functions as a temperature-sensing Raman reporter. The reliability of temperature measurements is corroborated by using both the anti-Stokes/Stokes ratio and the Raman peak shift. We show that optical heating can be adjusted by extruding a c-Si substrate, for example, the temperature increase is achieved by making c-Si pillars beneath the TiN pads longer. This peculiarity gives the possibility to probe the T g in a broad temperature range for the diversity of glassy polymers. We believe that the developed method will pave the way for 2D mapping structural glass transitions of heterogeneous glassy polymers, polymeric blends, and eventually, 3D confined polymers.

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“…Localised quantitative thermal analysis, often referred to as local thermal analysis (LTA), is also possible using a variation this technique. These techniques use silicon probes with highly doped conductive legs and a low doped resistive area close to the tip that afford spatial resolution in the nm range, as shown in figure 32(a) (Fischinger et al 2014). Applying a voltage across the cantilever legs induces an electric current, which gives rise to resistive heating in the tip region due to Joule heating.…”

Section: Afm-thermal Analysismentioning

confidence: 99%

Hyphenated analytical techniques for materials characterisation

Armstrong¹,

Kailas²

2017

Eur. J. Phys.

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This topical review will provide a survey of the current state of the art in ‘hyphenated’ techniques for characterisation of bulk materials, surface, and interfaces, whereby two or more analytical methods investigating different properties are applied simultaneously to the same sample to better characterise the sample than can be achieved by conducting separate analyses in series using different instruments. It is intended for final year undergraduates and recent graduates, who may have some background knowledge of standard analytical techniques, but are not familiar with ‘hyphenated’ techniques or hybrid instrumentation. The review will begin by defining ‘complementary’, ‘hybrid’ and ‘hyphenated’ techniques, as there is not a broad consensus among analytical scientists as to what each term means. The motivating factors driving increased development of hyphenated analytical methods will also be discussed. This introduction will conclude with a brief discussion of gas chromatography-mass spectroscopy and energy dispersive x-ray analysis in electron microscopy as two examples, in the context that combining complementary techniques for chemical analysis were among the earliest examples of hyphenated characterisation methods. The emphasis of the main review will be on techniques which are sufficiently well-established that the instrumentation is commercially available, to examine physical properties including physical, mechanical, electrical and thermal, in addition to variations in composition, rather than methods solely to identify and quantify chemical species. Therefore, the proposed topical review will address three broad categories of techniques that the reader may expect to encounter in a well-equipped materials characterisation laboratory: microscopy based techniques, scanning probe-based techniques, and thermal analysis based techniques. Examples drawn from recent literature, and a concluding case study, will be used to explain the practical issues that arise in combining different techniques. We will consider how the complementary and varied information obtained by combining these techniques may be interpreted together to better understand the sample in greater detail than that was possible before, and also how combining different techniques can simplify sample preparation and ensure reliable comparisons are made between multiple analyses on the same samples—a topic of particular importance as nanoscale technologies become more prevalent in applied and industrial research and development (R&D). The review will conclude with a brief outline of the emerging state of the art in the research laboratory, and a suggested approach to using hyphenated techniques, whether in the teaching, quality control or R&D laboratory.

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An Evaluation of Local Thermal Analysis of Polymers on the Sub-Micrometer Scale Using Heated Scanning Probe Microscopy Cantilevers

Cited by 6 publications

References 40 publications

Three-Dimensional Nanothermistors for Thermal Probing

Three-Dimensional Nanothermistors for Thermal Probing

Nanoscale Sensing Vitrification of 3D Confined Glassy Polymers Through Refractory Thermoplasmonics

Hyphenated analytical techniques for materials characterisation

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