Polymer characterization using thermomechanical analysis

Henderson, J. B.; Emmerich, Wolfgang

doi:10.1007/bf01912213

Cited by 11 publications

(5 citation statements)

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“…The glass transition temperature (T g ), 5% weight loss temperature (T d5 ), and char yield which is defined as the mass percentage of the residue when heated to 550 °C were found to be >250 °C, 355 °C, and 21%, respectively. The remarkably high T g , compared to normal linear polystyrene, [19] supports the idea that a densely cross-linked network structure was successfully formed in the organic-inorganic hybrid polymer film by the heat treatment, which resulted in the high heat resistance.…”

Section: Thermal Treatment Of Poly(tmsst-co-bast-co-hfast) For Cross-linking Formationsupporting

confidence: 54%

One‐Step Synthesis of Alkaline‐Soluble Polystyrene Containing Trimethoxysilyl‐ and Boronic Acid‐Moieties as Inorganic, Reactive Pendant Groups for Photosensitive Materials

Doi

Sugiura

Shimokawa

2021

Macro Chemistry & Physics

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It is of great interest in simple preparation of organic–inorganic hybrid thermoset soluble in alkaline developer, intended for photosensitive materials used in the field of semiconductor packaging based on sophisticated molecular design from the viewpoint of performance improvement and cost reduction. Here successful one‐step synthesis of alkaline‐soluble polystyrene with three kinds of pendant groups along the chain; trimethoxysilyl (TMS), boronic acid (BA), and hexafluoroisopropylalcohol (HFA) groups is shown. Solvent composition‐based equilibrium control of reactions involving the inorganic pendant groups (TMS and BA) as well as the hydrogen bonding ability and sterically bulky structure of the HFA group are effective in suppressing cross‐linking reactions during polymerization. The latter is confirmed through DFT calculation and terpolymerization experiments where the effect of the HFA group is compared to other ten kinds of p‐substituted functional groups. The obtained terpolymer is soluble in alkaline developer and forms an insoluble membrane with high heat‐resistance after heat treatment. Furthermore, its photosensitive polymer composition with photochemical acid generator exhibits negative‐type photosensitivity. The organic–inorganic hybrid thermosetting polystyrene is a promising material for semiconductor package applications.

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Section: Thermal Treatment Of Poly(tmsst-co-bast-co-hfast) For Cross-linking Formationsupporting

confidence: 54%

One‐Step Synthesis of Alkaline‐Soluble Polystyrene Containing Trimethoxysilyl‐ and Boronic Acid‐Moieties as Inorganic, Reactive Pendant Groups for Photosensitive Materials

Doi

Sugiura

Shimokawa

2021

Macro Chemistry & Physics

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“…Glass transitions can induce an increase in the expansion coefficient (Henderson and Emmerich 1991), a reduction of sample volume or increase of penetration (Keinath and Boyer 1981), and sample softening (Ng and Williams 1981) around the transition temperature. TMA is more sensitive to physicochemical transitions than DSC (O'Neal et al 1995) and thus could be used to detect WaMB transitions in mineral soil material, where DSC is not sensitive enough.…”

Section: Introductionmentioning

confidence: 99%

Potential of AFM–nanothermal analysis to study the microscale thermal characteristics in soils and natural organic matter (NOM)

Schaumann

Mouvenchery

2011

J Soils Sediments

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Purpose This exploratory study evaluates the potential of nanothermal analysis (nTA) coupled with atomic force microscopy (AFM) of soil samples for understanding physicochemical processes in soil and for linking the nanospatial and microspatial distribution of thermal characteristics with the macroscopic properties of soil samples. Materials and methods Soil and reference samples were investigated by differential scanning calorimetry and AFMnTA. nTA was conducted on 16 points of each AFM image in two subsequent heating cycles (55-120°C and 55-300°C, respectively). Thermograms were subdivided into characteristic types and their spatial distribution was compared between sample replicates and materials. Results and discussion Thermogram types consisted of partly structured expansion and compression phases, suggesting material-specific thermal profiles. The distribution of thermogram types reflected sample-dependent nanoscale and microscale heterogeneity. Indications for water molecule bridge transitions were found by nTA in peat and soil. Organic materials generally revealed strong expansion and irreversible compression phases, latter probably due to the collapse of pore and aggregate structures. In contrast to charcoal and manure, peat shows strong expansion below 120°C and compression only above 120°C. Conclusions All investigated samples are heterogeneous on the nanoscale and microscale with respect to thermal behaviour. AFM-nTA allows distinguishing numerous different materials on nanometre and micrometre scales in soil samples. The material-dependent characteristics will help in understanding and learning more about the nanoscale distribution of different materials and properties. Related to the macroscopic thermal behaviour, this will allow studying links between the properties of biogeochemical interfaces and the processes governed by them.

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“…The printed pieces were analysed using DSC methods, in order to receive information on the influence of the hybrid heating on the printed material and on the surface characteristics. Thermal analysis is used as a tool to study the degradation, melting or crystallization of a polymer [14][15][16][17]. The results can offer relevant information regarding their evolution in specific conditions.…”

Section: Deposited Layer -Materials Characteristicsmentioning

confidence: 99%

Resistive-IR Hybrid Heating in FDM Printing

Ciornei¹,

Savu²,

Sîrbu³

et al. 2021

KEM

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FDM printing is based on resistance to heat of the polymer filament, which starts in a viscous state and is extruded from nozzle to the printing area. The printing area is hot around 70°C for a better adherence of the deposited polymer and for slow cooling of it. The later deposited layers will experience faster cooling and the characteristics of the polymer will suffer light changes. The paper aims to present the results of a preliminary research regarding the double source successive heating and double source hybrid heating of the extruded polymer in FDM process. There were used two distinct heat sources, the resistive source mounted in the extrusion nozzle and IR lamp heat source placed in the printing chamber. The first heating, which acts during the extrusion process, is a hybrid heating and it is developed inside the extrusion nozzle (hot-end); it is given by the resistive heat source by the IR lamp. After the extrusion, during the deposition process and after the deposition process, the heating of the polymer continues due to the IR lamp. The difference between the printing with IR heating and without IR heating was monitored. A decreasing of about 5-8% of the material stiffness was noticed when the IR lamp was introduced. The material became more viscous and the bonding of the successive layers was improved. DSC analysis has been performed in both cases: with and without IR heat source. The evolution of the elastic modulus proved a decreasing of the plasticity during the simple printing process. The decreasing was less (at least by about 25%) when used IR heat source. The elongation viscosity was analysed and its values were decreasing while the temperature was increasing that took place. The decreasing was produced by the reduction of the elasticity, when the chain branches were decreasing their length. The decreasing is more pronounced while the increasing of the temperature. A low difference (of about 2-5%) was observed to the mechanical characteristics after tensile tests.

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Polymer characterization using thermomechanical analysis

Cited by 11 publications

References 1 publication

One‐Step Synthesis of Alkaline‐Soluble Polystyrene Containing Trimethoxysilyl‐ and Boronic Acid‐Moieties as Inorganic, Reactive Pendant Groups for Photosensitive Materials

One‐Step Synthesis of Alkaline‐Soluble Polystyrene Containing Trimethoxysilyl‐ and Boronic Acid‐Moieties as Inorganic, Reactive Pendant Groups for Photosensitive Materials

Potential of AFM–nanothermal analysis to study the microscale thermal characteristics in soils and natural organic matter (NOM)

Resistive-IR Hybrid Heating in FDM Printing

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