Morphology and properties of foamed high crystallinity<scp>PEEK</scp>prepared by high temperature thermally induced phase separation

Rusakov, Dmitrii; Menner, Angelika; Spieckermann, Florian; Wilhelm, Harald; Bismarck, Alexander

doi:10.1002/app.51423

Cited by 14 publications

(5 citation statements)

References 49 publications

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“…These axialite PEEK morphologies have not been observed in other PEEK aerogel systems. Only globular morphologies [32][33][34] or open cellular structures [44,54,56] have been reported previously. To further investigate the hierarchical morphology of PEEK aerogels, X-ray scattering experiments were performed.…”

Section: Morphology Of Peek Aerogelsmentioning

confidence: 99%

“…Solid-liquid phase separation can lead to crystalline textures, such as spherulites [50][51][52][53] and axialites [28,52,53]. Porous PEEK systems have been prepared using solvents including 4-phenylphenol [54], diphenyl sulfone [55,56], and benzophenone [57]. Interestingly, TIPS of PEEK in diphenyl sulfone has been shown to yield fibrillar foams [56] or powders [55], depending on the preparation.…”

Section: Introductionmentioning

confidence: 99%

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High Modulus, Strut-like poly(ether ether ketone) Aerogels Produced from a Benign Solvent

Spiering,

Godshall,

Moore

2024

Gels

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Poly(ether ether ketone) (PEEK) was found to form gels in the benign solvent 1,3-diphenylacetone (DPA). Gelation of PEEK in DPA was found to form an interconnected, strut-like morphology composed of polymer axialites. To our knowledge, this is the first report of a strut-like morphology for PEEK aerogels. PEEK/DPA gels were prepared by first dissolving PEEK in DPA at 320 °C. Upon cooling to 50 °C, PEEK crystallizes and forms a gel in DPA. The PEEK/DPA phase diagram indicated that phase separation occurs by solid–liquid phase separation, implying that DPA is a good solvent for PEEK. The Flory–Huggins interaction parameter, calculated as χ12 = 0.093 for the PEEK/DPA system, confirmed that DPA is a good solvent for PEEK. PEEK aerogels were prepared by solvent exchanging DPA to water then freeze-drying. PEEK aerogels were found to have densities between 0.09 and 0.25 g/cm3, porosities between 80 and 93%, and surface areas between 200 and 225 m2/g, depending on the initial gel concentration. Using nitrogen adsorption analyses, PEEK aerogels were found to be mesoporous adsorbents, with mesopore sizes of about 8 nm, which formed between stacks of platelike crystalline lamellae. Scanning electron microscopy and X-ray scattering were utilized to elucidate the hierarchical structure of the PEEK aerogels. Morphological analysis found that the PEEK/DPA gels were composed of a highly nucleated network of PEEK axialites (i.e., aggregates of stacked crystalline lamellae). The highly connected axialite network imparted robust mechanical properties on PEEK aerogels, which were found to densify less upon freeze-drying than globular PEEK aerogel counterparts gelled from dichloroacetic acid (DCA) or 4-chlorphenol (4CP). PEEK aerogels formed from DPA were also found to have a modulus–density scaling that was far more efficient in supporting loads than the poorly connected aerogels formed from PEEK/DCA or PEEK/4CP solutions. The strut-like morphology in these new PEEK aerogels also significantly improved the modulus to a degree that is comparable to high-performance crosslinked aerogels based on polyimide and polyurea of comparable densities.

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Section: Morphology Of Peek Aerogelsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

High Modulus, Strut-like poly(ether ether ketone) Aerogels Produced from a Benign Solvent

Spiering,

Godshall,

Moore

2024

Gels

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“…Due to the high melting temperature of PEKK (T m = 300 °C to 360 °C, depending on T/I), high boiling point solvents must be used in order to break down the semi-crystalline structure of PEKK during dissolution. To date, solvents reported for PEKK include: dichloroacetic acid (DCA), 14 4-phenylphenol, [15][16][17] and 9-fluorenone. 17 These solvents require dissolution temperatures ranging from 180 °C for DCA to over 230 °C for 4-phenylphenol and 9-fluorenone.…”

Section: Introductionmentioning

confidence: 99%

Blocky bromination of poly(ether ketone ketone) as a means to preserve crystallizability and rapid crystallization kinetics

Pomatto,

Crater,

Godshall

et al. 2024

Polym. Chem.

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“…We recently demonstrated a high‐temperature TIPS process to produce porous PEEK using a high boiling aprotic solvent. [ 21,22 ] Here, we will show that this approach can be translated to PEKK in high boiling point aprotic solvent solutions; 4‐phenylphenol and 9‐fluorenone were identified as suitable solvents for the high‐temperature TIPS process. In this study, we report the preparation of high‐porosity PEKK foams with controllable porosity and morphology.…”

Section: Introductionmentioning

confidence: 99%

High Porosity Poly(ether ketone ketone): Influence of Solvents on Foam Properties

Rusakov

Menner

Bismarck

2023

Macro Materials & Eng

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Poly(ether ketone ketone) (PEKK) is a semicrystalline high‐performance polymer with exceptional mechanical properties, high continuous operation temperature, and is insoluble in most common solvents. Porous PEKK, desired for biomedical applications, is produced by a high‐temperature thermally induced phase separation process using PEKK solutions in two high boiling aprotic solvents, 4‐phenylphenol and 9‐fluorenone, with concentrations up to 20 wt.%. It is demonstrated that the solvent choice has a pronounced influence on the phase separation behavior, which determines the foam morphology, physical and mechanical properties of PEKK foams. Porous PEKK with porosities ranging from 70% to 90%, specific surface areas up to 194 m2 g−1 and elastic moduli ranging from 35 to 100 MPa are produced.

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Morphology and properties of foamed high crystallinityPEEKprepared by high temperature thermally induced phase separation

Cited by 14 publications

References 49 publications

High Modulus, Strut-like poly(ether ether ketone) Aerogels Produced from a Benign Solvent

High Modulus, Strut-like poly(ether ether ketone) Aerogels Produced from a Benign Solvent

Blocky bromination of poly(ether ketone ketone) as a means to preserve crystallizability and rapid crystallization kinetics

High Porosity Poly(ether ketone ketone): Influence of Solvents on Foam Properties

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