Wide-angle X-ray Diffractometry Research Articles

Effect of organoclay on the physical properties of colorless and transparent copoly(amide imide) nanocomposites.

Copoly(amic acid) was prepared using the diamine monomer N,N'-[2,2'-bis(trifluoromethyl)-4,4'-biphenylene]bis(4-aminobenzamide) (TFAB) and the anhydride monomers 4,4'-(hexafluoro-isopropylidene)diphthalic anhydride (6FDA) and 4,4'-biphthalic anhydride (BPA). Thereafter, a colorless and transparent copoly(amide imide) (Co-CPAI) film was synthesized through various heat treatments. Co-CPAI hybrid films with a TFAB : 6FDA : BPA molar ratio of 1 : 0.5 : 0.5 were subsequently fabricated using organically modified hectorite (STN) with various contents ranging from 0 to 7 wt% via the solution intercalation method. Finally, the thermomechanical properties, clay dispersion, and optical transmittance of the hybrid films were investigated. The results of wide-angle X-ray diffractometry and transmission electron microscopy demonstrated good dispersion at low clay loadings; however, clay agglomeration was observed above a certain critical STN content. At the critical STN content of 3 wt%, the clay was evenly distributed in the matrix with a nanoscale thickness of approximately 10 nm. Hybrid films containing 3 wt% STN showed excellent thermomechanical properties. Beyond this critical clay content, the physical properties of the films decreased because of the agglomeration of excess clay. Regardless of the clay content, however, the optical properties of the hybrid films remained constant, and their yellow indices, which ranged from 2 to 4, indicated excellent colorless transparency.

Eco-Friendly Cellulose-Based Nonionic Antimicrobial Polymers with Excellent Biocompatibility, Nonleachability, and Polymer Miscibility.

This study aims to prepare natural biomass-based nonionic antimicrobial polymers with excellent biocompatibility, nonleachability, antimicrobial activity, and polymer miscibility. Two new cellulose-based nonionic antimicrobial polymers (MIPA and MICA) containing many terminal indole groups were synthesized using a sustainable one-pot method. The structures and properties of the nonionic antimicrobial polymers were characterized using nuclear magnetic resonance hydrogen spectroscopy (1H NMR), infrared spectroscopy (FTIR), wide-angle X-ray diffractometry (XRD), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), scanning electron microscopy (SEM), gel chromatography (GPC), and other analytical techniques. The results showed that microcrystalline cellulose (MCC) molecules combined with indole derivatives through an esterification reaction to produce MICA and MIPA. The crystallinity of the prepared MICA and MIPA molecules decreased after MCC modification; their morphological structure changed from short fibrous to granular and showed better thermal stability and solubility. The paper diffusion method showed that both nonionic polymers had good bactericidal effects against the two common pathogenic bacteria Escherichia coli (E. coli, inhibition zone diameters >22 mm) and Staphylococcus aureus (S. aureus, inhibition zone diameters >38 mm). Moreover, MICA and MIPA showed good miscibility with biodegradable poly(vinyl alcohol) (PVA), and the miscible cellulose-based composite films (PVA-MICA and PVA-MIPA) showed good phase compatibility, light transmission, thermal stability (maximum thermal decomposition temperature >300 °C), biocompatibility, biological cell activity (no cytotoxicity), nonleachability, antimicrobial activity, and mechanical properties (maximum fracture elongation at >390%).

Monitoring crystallite fusion of nanocellulose during colloid condensation

The crystallinity of cellulose decreases when bundled microfibrils are dispersed in water as cellulose nanofibers (CNFs) or physically separated into finer nanoscale fibrils or single microfibrils. The crystallinity of these CNFs is recovered when they become densely assembled through the dehydration of the dispersion. In this process, multiple CNFs are assumed to partially fuse, leading to the enlargement of crystallite widths. The mechanism of this CNF fusion is, however, not well understood. In this study, the recovery process of the crystallinity of CNFs was monitored by sampling wet CNF gels during condensation from a dilute dispersion to a dense aggregate, followed by wide-angle X-ray diffractometry (WAXD) and solid-state 13C nuclear magnetic resonance (NMR) spectroscopy analyses after supercritical drying. In the WAXD analysis, a two-step enlargement in the (2 0 0) crystal size was observed: the first step was a rapid increase in the range of solid content up to 1%, followed by a gradual increase in the range of 1–85%. The crystallinity index estimated by NMR hardly changed in the range of 0.5–30% but gradually increased in the range of 30–85%. A portion of the CNF samples, without drying, were also subjected to small-angle X-ray scattering and viscoelasticity analyses, indicating that the inter-CNF contact points in water significantly increased until reaching a solid content of 1%, and then at solid contents higher than 1%, the contact areas of each point gradually expanded. Finally, a mechanism of CNF fusion was proposed based on these results.

Enabling Efficient Design of Biological Formulations Through Advanced Characterization.

The present review summarizes the use of differential scanning calorimetry (DSC) and scattering techniques in the context of protein formulation design and characterization. The scattering techniques include wide angle X-ray diffractometry (XRD), small-angle neutron scattering (SANS) and small-angle X-ray scattering (SAXS). While DSC is valuable for understanding thermal behavior of the excipients, XRD provides critical information about physical state of solutes during freezing, annealing and in the final lyophile. However, as these techniques lack the sensitivity to detect biomolecule-related transitions, complementary characterization techniques such as small-angle scattering can provide valuable insights.

Synergistic improvement of CO2/CH4 separation performance of phenolphthalein-based polyimide membranes by thermal decomposition and thermal-oxidative crosslinking

Thermal oxidative crosslinking results in the generation of oxygen bridges among polymer chains and helps regulate the membrane microstructure. Simultaneously, any strategy to increase the crosslinking sites of polyimide (PI) can improve the crosslinking efficiency and allow precise control of the pore structure of membranes. Phenolphthalein-based PIs are potentially suitable precursors for thermal oxidative crosslinking of membranes, since thermal treatment will result in the degradation of lactone ring leading to the generation of a pair of phenyl crosslinking sites. In this work, three phenolphthalein-based diamines with different structures were designed and synthesized. The three diamines were subsequently reacted with 3,3′,4,4′-benzophenone tetracarboxylic dianhydride (BTDA) to prepare phenolphthalein-based PIs. The original membranes were post-treated by thermal oxidation crosslinking at 400 °C and 425 °C, respectively; the lactone ring underwent decomposition, and the imide ring opened at the same time, resulting in the generation of multiple crosslinking sites and correspondingly improving the crosslinking efficiency. The effect of the side groups (−CH3, –CF3 or unsubstituted) of phenolphthalein-based diamine and thermal treatment temperatures on the gas separation performance of phenolphthalein-based PI membranes were investigated. Wide-angle X-ray diffractometry (WAXD) and wide-angle X-ray scattering (WAXS) analysis demonstrated that the π-π stacking distance were improved. BTDA-FPP-425 had a CO2/CH4 selectivity of 37.68. This thermal degradation along with thermal oxidative crosslinking strategy provides a promising approach for fabrication of CO2/CH4 separation membrane.

Stereocomplex crystallization of chiral hydroxyalkanoic acid-based biodegradable alternating copolyesters with two types of chiral centers and opposite monomer configurational combinations of L-D and D-L (S-R and R–S)

Stereocomplex (SC) crystallization of chiral copolyesters was normally reported for those having the two types of chiral centers and identical monomer configurational combinations (MCCs) of L-L and D-D (or S–S and R-R). Herein, we report for the first time the SC crystallization of chiral hydroxyalkanoic acid-based biodegradable alternating copolyesters with the two types of chiral centers and the opposite MCCs of L-D and D-L (or S-R and R–S). Poly(l-lactic acid-alt-d-2-hydroxybutanoic acid) [P(LLA-alt-D-2HB)] with MCC of L-D and poly(d-lactic acid-alt-l-2-hydroxybutanoic acid) [P(DLA-alt-L-2HB)] with MCC of D-L were synthesized and their SC crystallization was confirmed by wide-angle X-ray diffractometry. The crystallizability was not enhanced by SC crystallization in enantiomeric polymer blending compared to homocrystallization in unblended specimens. The melting temperature was not elevated by SC crystallization as in the normal case of SC crystallization reported previously for chiral homopolyesters and copolyesters. However, the fact that only SC crystallization occurred without homo-crystallization in the enantiomeric blend indicates that interaction between the enantiomeric polymer chains were stronger than that between the identical polymer chains. It is expected that the newly proposed novel combinations of chiral hydroxyalkanoic acid-based alternating copolyesters with the two types of chiral centers and the opposite MCCs of L-D and D-L (S-R and R–S) can facilitate the preparation of biodegradable materials having a variety of physical properties and biodegradability.

Structure and Properties of PVDF/PA6 Blends Compatibilized by Ionic Liquid-Grafted PA6.

Compatibilization of immiscible blends is critically important for developing high-performance polymer materials. In this work, an ionic liquid, 1-vinyl-3-butyl imidazole chloride, grafted polyamide 6 (PA6-g-IL(Cl)) with a quasi-block structure was used as a compatibilizer for an immiscible poly(vinylidene fluoride) (PVDF)/PA6 blend. The effects of two PA6-g-IL(Cl)s (E-2%-50K and E-8%-50K) on the morphology, crystallization behavior, mechanical properties, and surface resistance of the PVDF/PA6 blend were investigated systematically. It was found that the two types of PA6-g-IL(Cl)s had a favorable compatibilization effect on the PVDF/PA6 blend. Specifically, the morphology of the PVDF/PA6 = 60/40 blend transformed from a typical sea-island into a bicontinuous structure after incorporating E-8%-50K with a high degree of grafting (DG). In addition, the tensile strength of the PVDF/PA6/E-8%-50K blend reached 66 MPa, which is higher than that of PVDF, PA6 and the PVDF/PA6 blend. Moreover, the PVDF/PA6/E-8%-50K blend exhibited surface conductivity due to the conductive path offered by the bicontinuous structure and conductive ions offered by grafted IL(Cl). Differential scanning calorimetry (DSC) and wide-angle X-ray diffractometry (WAXD) results revealed that PA6-g-IL(Cl) exhibits different effects on the crystallization behavior of PVDF and PA6. The compatibilization mechanism was concluded to be based on the fact that the nongrafted PA6 blocks entangled with the PA6 chains, while the ionic liquid-grafted PA6 blocks interacted with the PVDF chains. This work offers a new strategy for the compatibilization of immiscible polymer blends.

Zinc and Silver Salts-Containing Lamellar Titanium Phosphate: A Multifunctional Filler

Zinc and silver compounds have been studied because they have ultraviolet light barrier properties and bactericidal action, respectively. Materials with multifunctional characteristics have been sought to produce polymeric nanocomposites. In this work, the chemical modification of titanium phosphate (TiP) was carried out through a route with successive intercalations. TiP was synthesized and consecutively pre-expanded with ethylamine and pyromellitic acid. Then it was modified with zinc acetate and silver nitrate. The final product was characterized by Fourier transform infrared spectroscopy, differential scanning calorimetry, wide-angle X-ray diffractometry, field emission scanning electron microscopy coupled with energy dispersive X-ray spectroscopy and thermogravimetry. Infrared revealed dislocation and appearance of bands according to the intercalating agent. Inorganic salts interfered in the crystallization and melting processes of pyromellitic acid. Vanishing of the TiP hkl plane and variation and appearance of new crystallographic planes at low diffraction angles induced intercalation. SEM showed agglomerated structures. New thermal degradation events at higher temperatures endorsed the formation of zinc and silver carboxylate salts. We concluded that a new miscellaneous and multifunctional matter was achieved.

Analysis of the Poly(Butylene Succinate-Co-Lactate)/ Montmorillonite-Kaolinite Nanocomposite in the Formation of Microcapsules

A nanocomposite system comprised by a biodegradable polymer, poly(butylene succinate-co-lactate) (PBSL), and a Brazilian nanoclay (VMF1) containing montmorillonite (MMT) and kaolinite (K) is used to prepare microcapsules by solvent diffusion method. The nanocomposite PBSL/MMT-K and the microcapsules were characterized by wide angle X-ray diffractometry (XRD), scanning electron microscopy (SEM), stereomicroscopy, and Fourier transform infrared spectroscopy (FTIR). The overall results show that PBSL/MMT-K presents intercalated nanostructure of montmorillonite and kaolinite, both PBSL and PBSL/MMT-K proved to be very effective as matrix for production of uniform spherical microcapsules, as surveyed by scanning electron microscopy and stereomicroscopy. The spherical microcapsules repared from PBSL/MMT-K nanocomposite presented diameters smaller than 50Ž¼m, and can probably be used as delivery systems.

Critical assessment of structural changes in some copolyamide‐clay hybrid materials in correlation with the filler characteristics

AbstractA series of three copolyamide‐clay hybrid nanocomposites were prepared using three different smectite clays (bentonite, montmorillonite K10, and Nanomer I.30P) by a solventless melt mixing process. The influence of the nature of clays on the structural changes was critically assessed by comparison with the neat copolyamide. Nanocomposite samples were analyzed by scanning electron microscopy (SEM), wide angle X‐ray diffractometry (WAXD), UV–vis spectrometry and differential scanning calorimetry (DSC). The testing yielded in direct and indirect evidences of structural changes induced by the presence of clays in correlation with their characteristics, as nature of the clay, particle size, granulometric distribution, and particle dispersion into the matrix.

Synthesis, barrier performance, and molecular simulation of a high-barrier polyimide that contains amide groups

4-Amino-N′-(4-aminobenzoyl)benzohydrazide (AAPDA), a diamine monomer that contains two amide groups, was synthesised by amidation and reduction, after which it was polymerised with pyromellitic dianhydride (PMDA) to prepare AAPPI, a novel polyimide. AAPPI exhibited excellent barrier performance, with oxygen- and water-vapor-transmission rates (OTR and WVTR, respectively) of only 1.7 cm3 m−2 d−1 and 1.0 g m−2 d−1, respectively. This polyimide (PI) also exhibits outstanding thermal properties, with a glass transition temperature (Tg) of 423 °C, a 5% weight-loss temperature (Td5%) of 509 °C, and a coefficient of thermal expansion (CTE) of 2.58 ppm K−1 under nitrogen. The barrier performance of AAPPI was also compared to that of DABPI, a structurally similar PI. Molecular simulations, wide-angle x-ray diffractometry (WAXD), and positron annihilation lifetime spectroscopy (PALS) revealed that AAPPI forms many more interchain hydrogen bonds than DABPI due to its additional amide groups. Consequently, AAPPI has very tightly packed polymer chains, a high degree of crystallinity, a small free volume, and poor chain mobility. These factors generally inhibit the permeation of small molecules, which explains why AAPPI has better barrier properties than DABPI. This novel PI has broad applications for the packaging of flexible electronics.

Effect of thermal annealing on crystal evolution and multiple melting behaviors of molded poly(L-lactic acid) and poly(butylene succinate) blends upon heating investigated by TMDSC

The influence of post-process annealing treatment on the structural and thermal behaviors of poly(L-lactic acid)/poly(butylene succinate) (PLLA/PBS) blend was investigated by temperature modulated differential scanning calorimetry (TMDSC) and wide-angle X-ray diffractometry. It is shown that the low-order α′-structure of PLLA was formed in the as-molded samples and the molded products annealed at the temperatures below the melting of PBS, whereas the high-order α-crystal was developed when the high temperature of annealing (152 °C) was applied. With the addition of poly(ethylene glycol) plasticizer to the blends, the formation of high-order α-structure was prohibited. During the DSC heating scan, the α′- to α-crystalline phase transformation did not occur. The evidence of multiple melting behaviors observed by TMDSC was ascribed to the simultaneous melting, recrystallization, and remelting of the PLLA and PBS crystals in the blends.

Cellulose isolated from Delonixregia pods: Characterisation and application in the encapsulation of vitamin A

Native cellulose (NC) was extracted from agricultural waste (flamboyant fruit pods) using acidified sodium sulphite treatment followed by mercerization with sodium hydroxide. Carboxyl methyl cellulose (CMC) and cellulose acetate (CA) derivatives were obtained via etherification and acetylation of NC respectively under acidic conditions. Chemical composition, structural crystallinity, morphology, thermal studies, degree of substitution and acetylation of modified cellulose were reported. Wide angle X-ray diffractometry showed remarkable reduction in structural crystallinity and increased amorphous character upon modificationof NC.Scanning Electron Microscopy (SEM) displayed irregular spherical morphology and rough spongy-like mass for native and modified cellulose respectively confirming the surface disruption upon acetylation and carboxylmethylation. Proximate analysis revealed a reduction in the ash and fat contents of modified cellulose. Thermal analysis showed improved stability upon chemical modification of the NC. CMC significantly enhanced the stability of vegetable oil-water emulsion and ensured successful encapsulation of vitamin A in oil phase.

Temperature and time-dependent self-assembly and gelation behavior of chitin in aqueous KOH/urea solution

Chitin is the most abundant natural glycosaminoglycan that is derived from marine crustaceans and has enormous potential in biomedical applications because of its high similarity in chemical structure to the component of extracellular matrix. However, the key challenge remains the discovery of appropriate solvents for dissolving chitin and the limited understanding of the solution properties of chitin solutions, which hampers its development and applications. An aqueous KOH/urea solution was demonstrated to be a high-efficiency, energy-saving, and “green” solvent for chitin dissolution. Herein, we report the self-assembly and gelation behavior of chitin in aqueous KOH/urea solution using atomic force microscopy, fluorescence microscopy, rheology, wide-angle X-ray diffractometry, and differential scanning calorimetry. The molecular conformation, aggregate structure, and macroscopic solution properties of chitin in aqueous KOH/urea solution are affected by the temperature, chitin concentration, molecular weight, and aging time of the chitin solution. Understanding the self-assembly and gelation behavior of chitin solutions will enable accurate manipulation of the properties of chitin-based materials in potential applications such as structural materials, biomedicine, textile, and so on.

Enhancement in Flux and Antifouling Properties of Polyvinylidene Fluoride/Polycarbonate Blend Membranes for Water Environmental Improvement.

In this work, to overcome the fouling phenomenon of hydrophobic polymer membranes, polyvinylidene fluoride (PVDF) was blended with hydrophilic polycarbonate (PC) to prepare ultrafiltration membranes via the nonsolvent-induced phase separation method. The effects of PC content on membrane morphology, pore size distribution, and surface porosity were characterized and investigated by FE-SEM and image analyzer software. Solubility parameters calculated by molecular dynamics (MD) simulation showed that PVDF and PC are compatible and the results were confirmed by differential scanning calorimetry and wide angle X-ray diffractometry. The long-term chemical stability against NaOH and mechanical property before and after the abrasion test of the prepared membranes were also characterized by dynamic thermomechanical analysis. It was found that the hydrophilicity, water flux, abrasion resistance, and antifouling properties as the performance criteria of polymeric membranes were improved because of the presence of PC, and the separation efficiency of PVDF/PC membranes is much higher than that of the pristine PVDF membrane. The exemplary water filtration performances of these polymer membranes are harnessed here in this work to purify raw water polluted by natural organic matters, addressing the key environmental issue of water contamination.

Preparation, crystallization and degradation properties of poly(butylene succinate-co-neopentyl glycol succinate) copolymer/graphite oxide composites

In this study, graphene oxide (GO) was prepared by the modified Hummers’ method and poly(butylene succinate-co-neopentylglycol succinate)/graphene oxide (GO–PBNPGS) nanocomposites were synthesized via in situ polymerization with a series of GO contents (from 0.01 to 0.10 mass%). The GO was characterized by Fourier transform infrared spectrum, atomic force microscopy and wide-angle X-ray diffractometry. The non-isothermal crystallization kinetics and crystalline morphology of the neat PBNPGS and its nanocomposites were analyzed by differential scanning calorimetry and polarized optical microscopy (POM), respectively. The results showed that GO was prepared successfully and dispersed in PBNPGS uniformly during the experimental process. The non-isothermal crystallization kinetics was characterized using Avrami equation modified by Jeziorny. The experimental results indicated that the non-isothermal crystallization behavior of the GO–PBNPGS was influenced by the GO content and cooling rate, the crystallization rate first increased and then decreased with an increase in GO content. Therefore, it was expected that the GO could accelerate the crystallization process. POM observations indicated that GO served as an effective nucleating agent for the crystallization of GO–PBNPGS when 0.10 mass% GO was added, and 0.05 mass% GO in PBNPGS had the largest spherulites and the lowest nucleation ability. In addition, the experimental data also showed that the biodegradation rate increased with the increasing of GO content, with a significant rate of degradation occurring in the composite sample with 0.10 mass% GO content.

Effect of modified microcrystalline cellulose on poly(3-hydroxybutyrate) molecular dynamics by proton relaxometry

Hybrid films of poly(3-hydroxybutyrate) (PHB) and modified cellulose by solution casting method were prepared, aiming to study the influence of modified cellulose (0.25%, 0.5% and 0.75% w/w) on the structural organization and thermal properties of PHB matrix. The modified cellulose showed good dispersion in polymer matrix, due to the high compatibility between phases explained by similarity of polymer and filler structures. The composites were studied by wide-angle X-ray diffractometry, differential scanning calorimetry, thermogravimetric analysis, and time-domain nuclear magnetic resonance (NMR) spectroscopy. The conjugation of results coming from those techniques allowed to determine the cellulose concentration that had the highest influence on crystalline planes and degree of crystallinity of PHB, that is, the influence in the composite structure. The molecular dynamics obtained by NMR showed a reciprocal influence between polymer matrix and cellulose particles, enhancing the interactions present in the agglomerated particles.

Sustainable Plastics from Biomass: Blends of Polyesters Based on 2,5-Furandicarboxylic Acid.

Intending to expand the thermo-physical properties of bio-based polymers, furan-based thermoplastic polyesters were synthesized following the melt polycondensation method. The resulting polymers, namely, poly(ethylene 2,5-furandicarboxylate) (PEF), poly(propylene 2,5-furandicarboxylate) (PPF), poly(butylene 2,5-furandicarboxylate) (PBF) and poly(1,4-cyclohexanedimethylene 2,5-furandicarboxylate) (PCHDMF) are used in blends together with various polymers of industrial importance, including poly(ethylene terephthalate) (PET), poly(ethylene 2,6-naphthalate) (PEN), poly(L-lactic acid) (PLA) and polycarbonate (PC). The blends are studied concerning their miscibility, crystallization and solid-state characteristics by using wide-angle X-ray diffractometry (WAXD), differential scanning calorimetry (DSC) and polarized light microscopy (PLM). PEF blends show in general dual glass transitions in the DSC heating traces for the melt quenched samples. Only PPF–PEF blends show a single glass transition and a single melt phase in PLM. PPF forms immiscible blends except with PEF and PBF. PBF forms miscible blends with PCHDMF and PPF, whereas all other blends show dual glass transitions in DSC and phase separation in PLM. PCHDMF–PEF and PEN–PEF blends show two glass transition temperatures, but they shift to intermediate temperature values depending on the composition, indicating some partial miscibility of the polymer pairs.

Mechanical and thermal properties of hyperbranched poly(ε-caprolactone) modified graphene/epoxy composites

Graphene nanosheets (GNs) often results in incompatibility with the hydrophobic polymer matrix, and the tendency to form aggregates during processing. Herein, hyperbranched polycaprolactone modified GNs (PGNs) was obtained using 3,4,9,10-perylenetetracarboxylic acid anhydride (PTCDA)reacted with GNs and caprolactone. Firstly, π-π stacking interactions between GNs and perylenebisimide derivatives (PBI), and then in-situ polymerization of e-caprolactone. The structure and characteristic of PGNs were investigated by infrared spectroscopy, wide angle X-ray diffractometry, thermogravimetric analysis and ultraviolet spectrum. PGNs was added into epoxy matrix at different contents to improve the mechanical and thermal properties of epoxy. At 1.0 wt.% PGNs content, the impact strength and tensile strength of PGNs/epoxy composites were 43.41 kJ/m2 and 91.60 MPa. Compared with those of pure epoxy, these value increased by148% and 87%, respectively, as well as the Tg increased by about 20 °C.

Intercalation of α-titanium phosphate with long-chain amine aided by short-chain amine

In the textile industry, various chemicals are used to produce quality yarns. Thinking about its future use for improving the dyeability of the textile yarns, the intercalation of alpha-titanium phosphate (α-TiP) using long-chain amine was accomplished. In this work, we studied α-titanium phosphate intercalation by a long-chain amine aided by a short-chain one. The synthesis of the titanium phosphate was performed using titanium isopropoxide and orthophosphoric acid with a molar ratio of 1:8. The phosphate was organically modified using two different amines—ethylamine (E) and the oligoetheramine [O-(2aminopropyl)-O’-(2-methoxyethyl) polypropylene glycol, Jeffamine®, (J)] using the 0.5:1 amine:phosphate molar ratio. The materials were characterized by thermogravimetry, Fourier-transform infrared spectroscopy, wide-angle X-ray diffractometry, Raman spectroscopy and energy-dispersive X-ray spectroscopy. JETiP and EJTiP thermogravimetric curves evidenced higher amine incorporation into titanium phosphate. X-ray diffractogram patterns of ETiP, JETiP and EJTiP showed new diffraction peaks coexisting with pristine one. Fourier-transform infrared spectroscopy indicated that amine was incorporated into α-TiP galleries as amine salt. Evaluation of several absorption ratios showed that better efficiency of amine intercalation was found in the JETiP and EJTiP assembled system. ETiP, JETiP and EJTiP Raman spectroscopy revealed change in α-TiP spectra owing to the chemical modification and intercalation promoted by amines. According to the energy-dispersive X-ray spectroscopy, JETiP and EJTiP showed the highest level of Jeffamine® incorporation. We concluded that the use of ethylamine was indispensable in the intercalation of long-chain amine inside the α-TiP galleries.