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FIGURE 1. Schematic illustrations of two types of polymer-layered silicate morphologies: (left) intercalated and (right)
exfoliated (after Sinha-Ray and Okamoto32 ).
general family are also used, such as hectorite, These clay platelets are stacked on each other
saporite, mica, talc, vermiculite.147,148 The MMT and held together through van der Waal forces
crystal structure is made up of a layer of alu- and are separated from each other by 1 nm gaps
minum hydroxide octahedral sheet sandwiched be- (galleries).146 These galleries are usually occupied
tween two layers of silicon oxide tetrahedral sheets by cations, normally alkali and alkaline-earth cations
(Fig. 2).149 The nominal composition of MMT is such as Na+ and K+ , which counterbalance the neg-
Na1/3 (Al5/3 Mg1/3 )Si4 O10 (OH)2 .150 The layer thick- ative charges generated from isomorphic substitu-
ness of each platelet is on the order of 1 nm, and tion within the layers (for montmorillonite, Al3+
the lateral dimension is approximately 200 nm.150 replaced by Mg2+ ).146 It is well established that the
FIGURE 2. Structure of 2:1 layered silicate showing two tetrahedral sheets of silicon oxide fused to an octahedral sheet
of aluminum hydroxide (after Sinha-Ray and Okamoto32 ).
literature reports on the preparation and character- a higher d-spacing. The same authors also presented
ization of PET/clay nanocomposites,130−136 but no HDPE-based nanocomposites prepared by dissolv-
reports give a detailed description of the prepara- ing HDPE in a mixture of xylene and benzonitrile
tive method. For example, one report presents the with dispersed organically modified layered sili-
preparation of a PET nanocomposite by in situ poly- cates (OMLS).80a Syndiotactic polystyrene (s-PS) or-
merization of a dispersion of organoclay in water. ganically modified clay nanocomposites have also
However, characterization of the resulting compos- been prepared by the solution intercalation tech-
ite was not reported.130 In this report, the authors nique by mixing pure s-PS and organophilic clay
claim that water serves as a dispersing aid for the with adsorbed cetyl pyridinium chloride.195 The
intercalation of monomers into the galleries of the WAXD analyses and TEM observations showed a
organoclay. nearly exfoliated structure of these nanocomposites.
Sur et al.196 applied this solvent-based technique
to the preparation of polysulfone (PSF)-organoclay
INTERCALATION OF POLYMER
nanocomposites. PSF/organoclay nanocomposites
FROM SOLUTION
were obtained by mixing the desired amount of
Aranda and Ruiz-Hitzky101 reported the first the organoclay with PSF in DMAC at 80◦ C for
preparation of polyethylene oxide (PEO)/MMT 24 h. WAXD and TEM analyses indicated exfoliation
nanocomposites by this method. They conducted of the organoclay in the nanocomposites. Polylac-
a series of experiments to intercalate PEO tide (PLA) or poly(ε-caprolactone)-based nanocom-
(Mw = 105 g/mol) into Na+ -MMT using differ- posites have also been produced197,198a using this
ent polar solvents including water, methanol, ace- technique, but neither intercalation nor exfolia-
tonitrile, and mixtures (1:1). The nature of the tion was obtained as the clay existed in the form
solvents, with polarity of the medium being a de- of tactoids, consisting of several stacked silicate
termining factor, is critical in facilitating the in- monolayers.
sertion of polymers between the silicate layers in In another report,119 polyimide/MMT nanocom-
this method.154,189 The high polarity of water causes posites were prepared using solutions of poly(amic
swelling of Na+ -MMT. Methanol is not suitable as acid) precursors and dodecyl-MMT using N-methyl-
a solvent for high-molecular weight (HMW) PEO, 2-pyrrolidone as a solvent. FTIR, TEM, and WAXD
whereas water/methanol mixtures appear to be use- showed exfoliated nanocomposite structures at low
ful for intercalation, although cracking of the re- MMT content (<2 wt%) and partially exfoliated
sulting materials is frequently observed. Wu and structures at high-MMT content. Polyimide hybrids
Lerner190 reported the intercalation of PEO into Na+ - in thin-film form display a 10-fold decrease in per-
MMT and Na+ -hectorite using this method in ace- meability toward water vapor at 2 wt% clay loading
tonitrile. Diffusion of one or two polymer chains in compared to the neat polyimide film.
between the silicate layers was observed and the Zhong and Wang198b studied the exfoliation of
intersheet spacing increased from 0.98 to 1.36 and silicate nanoclays in organic solvents such as xylene
1.71 nm, respectively. In another study, Choi et al.191 and toluene. In particular, they exposed the solu-
prepared PEO/MMT nanocomposites by a solvent- tions of clay loadings from 1 to 10 wt% to ultrasound
casting method using chloroform as a cosolvent. for several hours. When the clay particles were ex-
Intercalated structure was observed for the result- foliated, the solutions became transparent and ex-
ing nanocomposites as confirmed by WAXD analy- tremely viscous. The exfoliation was confirmed by
ses and TEM observations. Other authors192,193 have X-ray diffraction measurements, where a peak asso-
also used the same method and same solvent for the ciated with diffraction from the silicate layers dis-
preparation of PEO/clay nanocomposites. appeared. Furthermore, they observed that solvents
Jeon et al.80a applied this technique to the such as tetrahydrofuran (THF) did not lead to ex-
preparation of nanocomposites of nitrile-based foliation as evidenced by a low-viscosity turbid so-
copolymer and polyethylene-based polymer with lution. Hence, the importance of the compatibility
organically modified MMT. A partially exfoliated between the dispersing medium and the modified
structure was obtained as revealed by the TEM clay for exfoliation was established. Although they
analysis, where both stacked intercalated and ex- carried out an extensive study of the rheology of
foliated silicate layers coexist. This observation was the exfoliated clay solutions, they did not consider
confirmed by the WAXD analysis, which reveals a how this information would be used in generating
broad diffraction peak that has been shifted toward thermoplastic composites.
In another study, Avella et al.198c investigated the According to the authors, polymers containing po-
crystallization behavior and properties of exfoliated lar groups capable of associative interactions, such
isotactic polypropylene (iPP)/organoclay nanocom- as Lewis-acid/base interactions or hydrogen bond-
posites prepared by a solution technique. From the ing, lead to intercalation. The greater the polarizabil-
XRD results, it was shown that the nanocomposite ity or hydrophilicity of the polymer, the shorter the
filled with 1 wt% of organoclay possesses exfoliated functional groups in the OMLS should be in order
structure, whereas the sample with 3 wt% contains to minimize unfavorable interactions between the
both exfoliated and intercalated structures. Above aliphatic chains and the polymer.200
3 wt%, clay aggregates were observed. Young’s Vaia et al.199 were the first to apply the melt inter-
moduli increased with increasing clay content and calation technique in the preparation of polystyrene
reached the maximum at 3 wt% filler content. Above (PS)/OMLS based nanocomposites. The resulting
3 wt%, tensile moduli actually decreased due to hybrid shows a WAXD pattern corresponding to
the agglomeration and collapse of the clay layers. that of the intercalated structure. These authors
Regarding the crystallization behavior, the authors also carried out the same experiment under the
observed spherulites with positive birefringence in same experimental conditions using nonmodified
the optical microscope images for the crystallized Na+ -MMT, but WAXD patterns did not show any
iPP filled with 1% of organoclay. Also, the nucle- intercalation of PS into the silicate galleries, em-
ation density increased with increasing nanopar- phasizing the importance of polymer/OMLS inter-
ticle content, indicating that the nanoparticles be- actions. Vaia et al.202 and Shen et al.203 also ap-
have as nucleating agents. While a lot of interest- plied the same technique to the preparation of
ing observations were presented, this study was PEO/Na+ -MMT and PEO/OMLS nanocomposites,
only able to achieve exfoliated and stable structures respectively.
only up to 1 wt% clay content. Also, it would be Liu et al.204a first applied melt intercalation tech-
useful to conduct rheological experiments to deter- nique in the preparation of a commercially available
mine the nanocomposites’ behavior of the exfoli- nylon-6 with octadecylammonium-MMT nanocom-
ated and nonexfoliated structures. This study, along posites, using a twin-screw extruder. WAXD pat-
with other studies using solvent-based technique, terns and TEM observations indicate exfoliated
requires a suitable polymer/solvent pair, which can nanocomposite structures with MMT less than
be expensive and environmentally unfriendly due 5 wt%. At a loading of 4.2 wt% MMT, the yield
to the use of organic solvents. strength increased from 68.2 to 91.3 MPa, the ten-
sile modulus increased from 3.0 to 4.1 GPa, and the
heat distortion temperature increased from 62◦ C to
112◦ C.
MELT INTERCALATION
Fornes et al.204b investigated the effect of organ-
This method was first demonstrated by Vaia oclay structure on nylon-6 nanocomposite morphol-
et al.199 in 1993, which stimulated the revival of in- ogy and properties. To study this effect, a series of or-
terest in PLS nanocomposites. In recent years, this ganic amine salts were ion exchanged with sodium
method has become mainstream for the fabrication montmorillonite (Na+ -MMT) to form organoclays
of PLS nanocomposites179,180 because it is simple, varying in amine structure or exchange level relative
economical, and environmentally friendly. to the starting clay. Each organoclay was melt-mixed
Vaia and Giannelis200,201 applied a mean-field sta- with a high-molecular grade of N6 (Capron B135WP,
tistical lattice model to study the thermodynamic is- with Mn = 29,300) using a twin-screw extruder.
sue associated with nanocomposite formation. They Figure 7 summarizes the structure and correspond-
reported that calculations based on this mean-field ing nomenclature of various amine compounds used
theory agree well with the experimental results. for the modification of Na+ -MMT using the ion-
Details regarding this model and explanation are exchange method. Figure 8 summarizes WAXD pat-
presented in Vaia and Giannelis.200 The authors terns and TEM observations for one representative
claimed that from their theoretical model, entropic nanocomposite. From the WAXD analysis, the au-
and energetic factors primarily determine the out- thors observed that the galleries of the organoclays
come of nanocomposite formation via polymer melt expand in a systematic manner to accommodate the
intercalation. General guidelines may be established molecular size and the amount of amine surfactant
for selecting potentially compatible polymer/OMLS exchanged for the Na+ -MMT. They also identified
systems based on the Vaia and Giannelis study.200 three distinct surfactant structural effects that led to
FIGURE 7. (a) Molecular structure and nomenclature of amine salts used to organically modify Na+−MMT by ion
exchange. The symbols M: methyl, T: tallow, HT: hydrogenated tallow, HE: 2-hydroxy-ethyl, R: rapeseed, C: coco, and H:
hydrogen designate the substitutents on the nitrogen. (b) Organoclays used to evaluate the effect of structural variations
of the amine cations on nanocomposite morphology and properties (after Fornes et al.204b ).
greater extents of exfoliation, higher stiffness, and in- of the cyclic oligomers converted the matrix into a
creased yield strengths for the nanocomposites: de- linear polymer without disruption of the nanocom-
creasing the number of long alkyl tails from two to posite structure. TEM imaging revealed that partial
one tallow, use of methyl rather than hydroxy-ethyl exfoliation was obtained, although no indication of
groups, and finally, use of an equivalent amount layer correlation was observed in the WAXD.
of surfactant on the clay as opposed to an excess Lee and Huang et al. prepared poly(etherimide)
amount. (PEI)/MMT nanocomposites by melt-blending
Gilman et al.205 reported the preparation of hexadecylamine-modified MMT and PEI at 350◦ C to
polyamide-6 (PA6) and PS-based nanocomposites obtain thermoplastic poly(etherimide) (PEI)-based
of MMT modified with trialkylimidazolium cations. nanocomposites.206,207a The dispersion of the MMT
WAXD analyses and TEM observations showed an layers within the PEI matrix was verified using
exfoliated structure for a PA6-based nanocomposite, WAXD and TEM. From WAXD patterns, it was
whereas for a PS/MMT system, mixed intercalated assumed that exfoliation was achieved because of
and exfoliated structures were obtained. the lack of diffraction peaks. However, TEM ob-
In another study, Huang et al.137 reported the servations revealed stacked silicate layers heteroge-
synthesis of a partially exfoliated bisphenol polycar- neously dispersed in the polymer matrix.
bonate nanocomposite prepared by using carbonate Finally, in a different study, Liu and coworkers
cyclic oligomers and dimethylditallowammonium- investigated the effects of clay concentration and
exchanged MMT. WAXD patterns indicated that ex- processing-induced clay dispersion on the struc-
foliation of this OMLS occurred after mixing with ture and properties of PA6/clay nanocomposites.207b
the cyclic oligomers in a Brabender mixer for 1 h The PA6/clay nanocomposites were prepared via
at 180◦ C. Subsequent ring-opening polymerization a melt-compounding method using a Brabender
the influence of varying the processing temperature compared to other supercritical fluids.208 High vis-
and screw speed on the enhancement of mechanical cosity is usually a major problem in the process-
properties of polypropylene nanocomposites. Using ing of high-molecular weight polymers or complex
XRD, SEM, TEM, and a dynamometer as character- mixtures of particle-filled polymers. To overcome
ization methods, the authors observed the best re- this problem, sc-CO2 can be used as a plasticiz-
sults at high-screw speed (350 rpm) and low-barrel ing agent to lower the viscosity of various poly-
profile temperature (170◦ C–180◦ C). At these process- mer melts.209−211 Under ambient conditions, CO2 is
ing conditions, maximum shear stress exerted on the a gas that makes its removal from the polymeric
polymer was achieved, which helped shearing and product easy. At near critical conditions, as Berens
breaking the clay platelets apart more effectively. and Huvard212 point out, CO2 behaves like a po-
Clay types can also have critical effects on the mor- lar, highly volatile organic solvent, which swells
phology and physical properties of the nanocom- and plasticizes polymers when it interacts with
posites. Thus, depending on the polymer matrix, the them. Montmorillonite is a typical swellable mineral
right clay surface modifier must be selected in order because it contains alkali metal ions between the
to achieve the best delamination and dispersion. Lei silicate sheets, and, therefore, it can be swollen in
et al. studied the effect of clay types on the process- polar solvents such as water and sc-CO2 .150 In po-
ing and properties of polypropylene nanocompos- lar solvents, the basal distance of the silicate sheets
ites and showed that the surface treatment of clay expands and finally the silicate sheets come to ex-
can improve the clay dispersion in the PP matrix.207f foliate into individual sheets. These concepts can be
The clays included in the study were Cloisite 15A, utilized in the fabrication of PLS nanocomposites as
Cloisite 20A, Nanocor I30E, and Nanocor I31PS. a few authors have reported.213,214 However, the ex-
Cloisite 15A and 20A were modified by long-alkyl tent of success is questionable and further research is
chains with quaternary ammonium groups, whereas needed because most authors did not investigate or
I30E and I31PS were modified by long-alkyl chains report quantitatively the improvements in the mate-
with amine groups. It was found that nanocompos- rials’ properties.
ites with alkyl-onium ion treated clays have higher To date, there are only a few papers that have re-
moduli and better thermal stability than the ones ported on the use of supercritical carbon dioxide as
with alkyl amine treated clays. A similar study by an alternative route for the preparation of polymer–
Dan et al. also shows the effect of clay modifiers clay nanocomposites.213,214 Zerda et al.214 used
on the morphology and properties of thermoplastic sc-CO2 for the synthesis of poly(methyl
polyurethane/clay nanocomposites.207g This is not methacrylate)-layered silicate intercalated
an exhaustive list of work that studied the effects nanocomposites. The authors presented a syn-
of processing machinery, conditions, and clay mod- thetic route to produce nanocomposites with
ifiers on the resulting nanocomposites. However, significantly high concentrations of OMLS. OMLS
it includes enough to show the importance many used in this experiment were Cloisite 15A, 20A,
processing factors have on the melt compound- and 25A from Southern Clay Products, Gonzales,
ing of nanocomposites. Therefore, when preparing Texas. At high levels of OMLS (>20 wt%), the
nanocomposites using the melt-compounding tech- viscosity was apparently high and was overcome by
nique, careful selection of mixer type, clay modifier, using sc-CO2 as a reaction medium. Homogeneous
and processing conditions must be made in order dispersion of monomer, initiation, and subsequent
to have a successful development of good quality polymerization all occur under a significantly
nanocomposites. reduced viscosity in this medium. The detailed
experiments can be found in Caskey and Lesser.215
NANOCOMPOSITE SYNTHESIS WITH THE The authors reported a homogeneous morphology,
AID OF SC-CO2 which was aided by sc-CO2 , in the intercalated
nanocomposites containing as high as 40 wt% of
Supercritical fluids have been receiving atten- OMLS. At this loading, only a 50% increase in
tion recently in various applications such as in the modulus was observed.
food and pharmaceutical industries as well as in In a different approach, Wingert et al.216 investi-
the plastics industry. Particularly, supercritical car- gated the effect of nanoclay and sc-CO2 on polymer
bon dioxide (sc-CO2 ) has been used widely in many melt rheology in an extrusion process. Polystyrene
applications because it is environmentally friendly, and organophilic montmorillonite (Cloisite 20A)
nontoxic, relatively low cost, and nonflammable were used in the fabrication of the nanocomposite.
An extrusion slit die rheometer with backpressure mers may, thus, be impracticable, especially in view
regulator was used to measure the shear viscosity of the high costs associated with solvents them-
of polystyrene/CO2 /nanoclay melts. The authors selves, their disposal and their environmental im-
observed that, without the presence of sc-CO2 , the pact. Furthermore, the extent of intercalation com-
viscosity of the nanocomposite (<5 wt% OMLS) in- pletely depends upon the nature of solvent used.
creased with nanoclay loading. With the presence For the melt intercalation technique, the drawback
of sc-CO2 , the nanocomposite melt is swollen, and is its dependence on the processing conditions, and
the nanoclay acts to reduce viscosity compared to favorable interactions between the polymer and the
the pure polystyrene/CO2 system. No satisfactory clay are required. Thus far in most studies, only ex-
explanation of why the nanoclay lubricates the flow foliated nanocomposite structures with up to 5 wt%
was given by the authors. No information regard- MMT can be achieved. In order to capitalize on the
ing nanocomposite structures nor material proper- potential offered by nanoparticles in areas such as
ties was reported. reinforcement, barrier, and electrical conductivity,
Recently, another approach to prepare polymer higher levels of fully dispersed nanoparticles must
nanocomposites using sc-CO2 in the melt intercala- be reached. The use of supercritical CO2 , if appro-
tion process was reported by Lesser and Manuel.213 priately used, may lead to higher concentrations of
Here, a study of the effect of sc-CO2 on the melt inter- exfoliated nanoclay particles.
calation process and on the final structure and mor-
phology of polymer–clay nanocomposites is pre-
sented. sc-CO2 was absorbed into the nanoclay par-
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