Non-destructive DRIFT spectroscopy measurement of the degree of curing of industrial epoxy/silica composite buildup layers

Granado, Lérys; Maurin, D.; Kempa, Stefan; Gregoriades, Laurence J.; Brüning, Frank; Fréty, Nicole; Anglaret, Éric; Bantigniès, Jean-Louis

doi:10.1016/j.polymertesting.2018.07.007

Cited by 8 publications

(7 citation statements)

References 28 publications

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“…The partial degrees of curing achieved during this precuring stage (i.e., degrees of precuring, α) were controlled by DRIFT, with the methodology previously reported. 40 The glassy and rubbery states of the ABF layers were identified in an enhanced temperature−time transformation diagram which was published elsewhere. 42 The ultimate glass transition temperature, T g , of the fully cured ABF was as high as 155 °C (DSC).…”

Section: ■ Materials and Methodsmentioning

confidence: 99%

“…The precuring of the epoxy matrix was performed at 180 °C for 5–90 min. The partial degrees of curing achieved during this precuring stage (i.e., degrees of precuring, α) were controlled by DRIFT, with the methodology previously reported . The glassy and rubbery states of the ABF layers were identified in an enhanced temperature–time transformation diagram which was published elsewhere .…”

Section: Methodsmentioning

confidence: 99%

“…Diffusereflectance infrared Fourier transform (DRIFT) absorption spectroscopy has been proven to be a reliable and accurate technique to measure the degree of curing on industrial panels, in agreement with calorimetric results. 40 Furthermore, a deep knowledge of curing behavior and kinetics was provided for the control of the curing process. 41,42 With these methods at hand, the present investigation aims to establish the relationships between the precuring step, the desmear performances, and polymer−copper adhesion, which currently remain to be poorly known.…”

Section: ■ Introductionmentioning

confidence: 99%

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Improvements of the Epoxy–Copper Adhesion for Microelectronic Applications

Granado

Kempa

Gregoriades

et al. 2019

ACS Appl. Electron. Mater.

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Upcoming electronic devices are required to be further miniaturized. The microelectronics industry and packaging technology focus efforts on optimizing adhesion between plated copper and printed circuit board (PCB) substrate (here epoxy/glass buildup composite), while keeping smooth surfaces for high-frequency application. We propose herein to review and deepen the basic understanding of the sequential buildup process employed worldwide for the past several decades for multilayered PCB manufacturing. This multiscale and interdisciplinary study aims to establish the relationships between degrees of precuring (α), oxidative etching (permanganate desmear wet treatment), and copper adhesion. The epoxy curing states on industrial coupons were evaluated by diffuse-reflectance infrared Fourier transform spectroscopy. Then, atomic force microscopy (AFM) described the desmear performances through topography evolution with α between the different sequence steps. Finally, polymer−copper adhesions were investigated by using peel strength tests, AFM, and X-ray photoemission spectroscopy. We remark that high adhesion strengths were obtained for very smooth surfaces. This study outlines the contribution of the polymer network viscoelasticity (relaxation dynamic) on the polymer−copper adhesion. We observed that faster polymer relaxation rates tended to increase polymer−copper adhesions.

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Section: ■ Materials and Methodsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Section: ■ Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Improvements of the Epoxy–Copper Adhesion for Microelectronic Applications

Granado

Kempa

Gregoriades

et al. 2019

ACS Appl. Electron. Mater.

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“…Three different areas of the samples were probed to check the reproducibility (deviations < 5%). Note that this NIR method was proven to remain quantitative, even considering the diffuse-reflection of the IR beam caused by the multiple matrix–filler interfaces …”

Section: Experimental Sectionmentioning

confidence: 99%

“…Note that this NIR method was proven to remain quantitative, even considering the diffuse-reflection of the IR beam caused by the multiple matrix−filler interfaces. 28 Considering system (C), after mixing the epoxy and m-XDA at RT during 5 min, 500 μL was placed into a glass cuvette. The cure monitoring was performed at 60.0 ± 0.1 °C for 1 h on an ABB MB3600 NIR spectrometer, using a deuterated triglycine sulfate (DTGS) detector with a resolution of 4 cm −1 and 32 scans/spectrum (acquired every 2 min).…”

Section: ■ Experimental Sectionmentioning

confidence: 99%

In Situ Vibrational Probes of Epoxy Gelation

et al. 2019

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This paper presents an efficient way to measure the curing kinetics and gel point, α gel , in epoxy resins from one single experiment. The epoxy curing reaction is herein monitored using in situ and time-resolved near-infrared absorption spectroscopy (NIR). The curing profiles over different isothermal conditions are in good agreement with DSC. Furthermore, the increase of the NIR absorption bands of aromatic rings (unreactive throughout curing) probe the cure shrinkage, as more and more aromatic rings are localized within the fixed sample volume. Therefore, the gel point is determined using the onset of the aromatic absorption increase. The results are in good agreement with the theoretical gel point, as well as DMA results. This innovative approach enables gelation measurements on epoxy neat resins and film composites with an easy-to-perform, accurate, robust, and versatile method.

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Review of curing deformation control methods for carbon fiber reinforced resin composites

Zhang

et al. 2022

Polymer Composites

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Under the influence of extrinsic curing conditions and intrinsic properties of carbon fiber reinforced resin composites, the formation of curing deformation is inevitable, which makes the shape of the manufactured components differ from the designed structure, and even exceeds the assembly tolerance, resulting in the scrap of parts. Therefore, it is very urgent and important to optimize the curing deformation of carbon fiber reinforced resin composites. In this paper, the mechanism of stress and curing deformation is reviewed firstly, and then the factors affecting the curing deformation are summarized. In particular, from the point of view of materials in curing process, three curing deformation control strategies, including (i) reinforcement structure optimization, (ii) resin modification and process optimization, (iii) die surface compensation and tool‐part contact optimization, were proposed. And with the development of curing deformation simulation technology, the (iv) inverse design strategy before curing and (v) hot sizing method from the view of after cured were further put forward, respectively. By analyzing the link between processing details and curing deformation, it is found that the dominant factor affecting deformation may change under different conditions, so the interaction between factors needs to be further discussed. Subsequently, the effect of these distortion control methods on curing deformation was analyzed and evaluated, and the shortcomings were pointed out. Finally, the challenges existed in curing deformation research were identified, in order to contribute to the development of curing deformation research.

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Non-destructive DRIFT spectroscopy measurement of the degree of curing of industrial epoxy/silica composite buildup layers

Cited by 8 publications

References 28 publications

Improvements of the Epoxy–Copper Adhesion for Microelectronic Applications

Improvements of the Epoxy–Copper Adhesion for Microelectronic Applications

In Situ Vibrational Probes of Epoxy Gelation

Review of curing deformation control methods for carbon fiber reinforced resin composites

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