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A brief review on α-zirconium phosphate intercalation compounds and nano-

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 SCIENCE CHINA
Technological Sciences
• Review • March 2016 Vol.59 No.3: 436–441
doi: 10.1007/s11431-015-5794-3

A brief review on -zirconium phosphate intercalation

compounds and nano-composites
TANG Mei, YANG TaiSheng & ZHANG Yue*
School of Materials Science & Engineering, Beihang University, Beijing 100191, China

Received January 5, 2015; accepted March 1, 2015; published online March 13, 2015

The layer structured zirconium phosphate (ZrP) can be intercalated with atoms, molecules, small organic groups and even
polymers. The structures and properties of the ZrP intercalation compounds can be deliberately tuned, leading to promising
potential applications in many fields. This article provides a brief review on the experimental results of the ZrP intercalation
compounds, with the focus on the polymer/-zirconium phosphate-ZrP) nano-composites. The computer simulations of the
ZrP intercalation compounds at the atomic level play a significant role in designing and understanding the properties of ZrP,
and in the promotion of the applications of compounds.

-zirconium phosphate, intercalations, nano-composites

Citation: Tang M, Yang T S, Zhang Y. A brief review on -zirconium phosphate intercalation compounds and nano-composites. Sci China Tech Sci, 2016, 59:
436441, doi: 10.1007/s11431-015-5794-3

1 Introduction provides a brief review on the α-ZrP intercalation com-

Due to the unique electronic and mechanical properties as
intercalated by atoms, molecules, small organic groups and
even polymers to change their properties significantly, layer
structured materials are hot research topics [1–6]. Great
progress has been achieved in the intercalation of the layer
structured zirconium phosphate (ZrP) with organic groups
and long chain polymers, and researches on the ZrP inter-
calation compounds are growing rapidly in recent years as
they have been used widely in many fields, such as photo-
chemistry [7], molecular and chiral recognition [8], bio-
technologies [9] and catalysis [10,11]. The base structure of
α-ZrP does not change appreciably under mild conditions
(ion exchange, intercalation, topotactic exchange, infinite
swelling, etc.). α-ZrP is insoluble and very stable toward
thermal treatment and wild chemical environment, such as
strong acids/bases and redox agents [12]. The present work
*Corresponding author (email: zhangy@buaa.edu.cn)
pounds.
The crystalline structure of -Zr(HPO4)2·H2O (-ZrP)
was firstly synthesized by SOL-GEL method and character-
ized by Clearfield and Stynes in 1964 [13]. SOL-GEL
method was also adopted by Sun and Xu to produce low
crystallinity -ZrP [14] and -ZrP nanoplatelets [15], re-
spectively. -ZrP can also be synthesized by using the hy-
drothermal method [16–18] and the direct precipitation re-
action method (DPRM) [19–22]. The largest size and the
highest sheet orderliness of -ZrP can be achieved by using
DPRM, while the sample prepared by SOL-GEL method
has the smallest size and the lowest sheet orderliness [23].
Figure 1 is a schematic representation of the arrangement
of three layers of -ZrP. The crystal structure is monoclinic
in space group of P21/n with a=0.9060 nm, b=0.5297 nm,
c=1.5414 nm and =101.71° [24]. In each layer, a plane of
Zr atoms is sandwiched between two layers of tetrahedral
phosphate groups and Zr atoms locate alternatively above
and below the mean plane. Each Zr atom is octahedrally

© Science China Press and Springer-Verlag Berlin Heidelberg 2015 tech.scichina.com link.springer.com
 Tang M, et al. Sci China Tech Sci
coordinated by six oxygen atoms from six different phos-
phate groups. Thus, three oxygen atoms of each phosphate
are bonded to three different zirconium atoms arranged at
the apices of a near equilateral triangle. The fourth oxygen
atom of phosphate protrudes into the interlayer space as
shown in Figure 1. The protruded -OH group or just its
protons can be replaced by other groups or cations via
ion-exchange or intercalation processes. In the region be-
tween two neighboring layers of -ZrP, the distance be-
tween adjacent oxygen atoms is 0.53 nm and the number of
negatively charged oxygen atoms of -P-OH groups on each
side is 4.12×1014/cm2. The corresponding ‘free area’ associ-
ated with each -P-OH group is thus 0.24 nm2. When -ZrP
is in its original form of Zr(HPO4)2, the adjacent Zr-Zr in-
terlayer distance is 0.75 nm, which seems too small to ac-
commodate large molecules. However, the layered α-ZrP
crystal is flexible, it is possible for the layers to move apart
to make organic molecules accommodate to the interlayer
region.
2 -ZrP intercalation compounds
The unique layered structure and flexibility of α-ZrP permit
ions, small organic groups and even long-chain polymers to
intercalate into the interfacial region. For small ions, inter-
calation is mainly via ion diffusion and exchanges with the
H atom of the -OH group. For example, a limited number of
cations (Li+, Na+, Ag+, Cu+ and Ca2+) can exchange with the
protons of α-ZrP at a high rate in acid solutions [25]. Large
monovalent and divalent cations (such as NH4+, Rb2+, and
Ba2+) or highly hydrated divalent and trivalent cations (such
as Mg2+, Cu2+, Cr3+ and Rh3+) [26] are also able to replace
the protons of α-ZrP, but the rates are very slow [27]. Usu-
ally, precursors with a large interlayer separation [28], such
as α-Zr(HPO4)(NaPO4)·5H2O and intercalation compounds
with ethanol or alkylamine, can be employed to facilitate
the exchange of large size or highly hydrated cations. Ex-
perimental results show that even the small ion intercalated
α-ZrP can improve their performance significantly. For
example, both Cu [29] and Fe [30] intercalated α-ZrP are
Figure 1 Schematic representation of α-ZrP layered structure. (a) Viewed
along the b axes; (b) viewed along the c axes [24].
March (2016) Vol.59 No.3 437
very efficient catalysts.
Small organic groups -R usually substitute the -OH
group in the phosphonates of α-ZrP with its layered inor-
ganic network essentially unaltered. A more detailed de-
scription about organic derivatives of -ZrP with -R pen-
dant groups is referred to refs. [31–33]. More recently, Am-
icangelo [34] synthesized some organic derivatives of -
ZrP, which have general formula of Zr(O3PR)1(O3PR′)1
with R and R′ being -C10H7, -C14H9, -OC4H9, or -OC2H5
(Figure 2). They were single-phase structures with random
mixtures of the organic moieties within the interlayer and
possess d spacings that were between those of the two par-
ent zirconium bis (phosphonates).
Recently, research interests in the α-ZrP based polymeric
nano-composites are growing, because the chemical, me-
chanical, and thermal properties of nano-composites can be
significantly improved by introducing -ZrP in the poly-
meric interface as nanofillers [21,35,36]. Accordingly, sev-
eral experimental methods have been developed to synthe-
size polymer/-ZrP inorganic nano-composites, including
exfoliation-adsorption, in-situ intercalative polyme- rization,
melt intercalation and template synthesis [37–40]. There
have been several experimental investigations on poly-
mer/-ZrP nano-composites including poly (ethylene ter-
ephthalate)(PET)/-ZrP [41], epoxy/-ZrP [42–45], poly-
acrylamide (PAM)/-ZrP [46,47], poly(vinyl alcohol)
(PVA)/-ZrP [48–53], and starch/-ZrP [54,55]. These
nano-composites will be reviewed in detail in the following
paragraphs and the combustion and mechanical properties
of some nano-composites are listed in Tables 1 and 2.
Figure 2 Idealized structural representations of the general formula
Zr(O3PR)1(O3PR′)1 . (a) R and R′=-C10H7; (b) R and R′=-OC2H5) [34].
438 Tang M, et al. Sci China Tech Sci March (2016) Vol.59 No.3

Table 1 Combustion data of the -ZrP-based compositesa)

Sample TTI THR PHRR Reference
PET 66 98 511
PET-co-DDP 70 91 400 [41]
PET-co-DDP-ZrP 73 76 270
PA6 75±1 233±12 1201±93
PA6-ZrP 88±1 217±22 880±61
PET 124±1 49±2 701±80
PET-ZrP 130±1 50±2 661±68
[36]
PP 46±1 100±1 878±9
PP-ZrP 30±1 97±2 895±5
EVA 80±1 107±4 1160±101
EVA-ZrP 55±1 98±4 1000±30
EVA 55±0 97±4 1183±136
EVA-1%ZrP 55±4 109±5 1406±107
[36]
EVA-3%ZrP 53±4 109±3 1448±148
EVA-5%ZrP 52±2 112±7 1412±135
a) TTI, time to ignition, s; EVA, ethylene-co-vinyl acetate; PET, poly(ethylene terephthalate); THR (total heat released), kw/m2; PHRR (peak heat release
rate), kw/m2. PET-co-DDP/-ZrP was synthesized by the direct condensation of terephthalic acid, ethylene glycol, 9,10-dihydro-10[2,3-di(hydroxycar-
bonyl)propyl]-10-phosphaphenanthrene-10-oxide (DDP) and nano -ZrP.

Table 2 Tensile strength and elongation at break of the -ZrP-based composites

Sample Tensile strength (MPa) Elongation at break (%) Reference

PA6  189±92
PA6-ZrP  7±2
[36]
PET  3.0±0.4
PET-ZrP  2.6±0.3
PVA ~24 ~340
PVA-(3M)ZrP ~35 ~370
[50]
PVA-(6M)ZrP 41.2 488.4
PVA-(12M)ZrP ~28 ~390
PVA 25 345
[51]
PVA-0.8wt% ZrP 32.3 404.23

2.1 PET/-ZrP nano-composites
PET is a semicrystalline polymer with excellent chemical
resistance, thermal stability, high strength and spinnability.
However, its flammability and severe dripping during
combustion greatly limit its applications. Considering the
thermal and chemical stability of -ZrP [56], the PET/-
ZrP nano-composite may improve the fire retardant perfor-
mance. A novel fire retardant nano-composite of PET/-
ZrP by in-situ polymerisation was obtained by Wang [41]. In
the nano-composites, the -ZrP nanofiller was well dis-
persed and the interlayer separation increased from 0.77 nm
to 1.13 nm by incorporation of the modifier molecules at
first and ultimately to 2.38 nm. The similar PET/-ZrP
nano-composites can also be prepared by a melt extrusion
method [19].
2.2 Epoxy/-ZrP nano-composites
Epoxy has been widely used as protective coatings and its
mechanical properties are essential for its applications. The
exfoliated α-ZrP nanofiller can greatly improve the modulus
and strength of the epoxy matrix without compromising its
ductility [43]. The intercalation is hydrogen-bonded to the
host and exhibits a bilayer structure into the interlayer
spacing. The tensile modulus of the nano-composites is in-
creased by 50% of the reference epoxy. In another work,
epoxy/-ZrP nano-composites show a large interlayer
spacing. A simple geometric model was developed to de-
scribe the relationship between interlayer spacing and filler
loading level [57]. The model prediction was in good
agreement with the TEM result that the interlayer spacing
was 2 vol% of ZrP layers in epoxy matrix.
2.3 PAM/-ZrP nano-composites
PAM is a water-soluble polymer with wide applications in
many fields such as infiltrative film, biosensor, anlistatig
coating, nonlinear optical devices and the flocculation of
municipal and industrial waste. In a recent work by Zhang
[46], a PAM/-ZrP polymer nano-composite was synthe-
sized by exfoliation-adsorption and in-situ intercalative
polymerization. The results indicated that the interactions
between PAM and -ZrP include electrostatic adsorption
 Tang M, et al. Sci China Tech Sci
and some weak interactions such as hydrogen bonding or
protonation, as shown in Figure 3. Thermal stability of the
nano-composites was improved due to the retardant effect
of the exfoliated or intercalated α-ZrP nanometer lamellae
[46].
2.4 PVA/-ZrP nano-composites
PVA is a cheap polymer and has outstanding properties
including high chemical resistance, good mechanical be-
haviors and excellent film-forming ability. It is widely used
in home textiles, coating materials and industrial materials.
The water soluble property of PVA makes it to be easily
combined with the exfoliated -ZrP colloidal dispersion.
The PVA/-ZrP nano-composite was firstly synthesized by
Yang and Liu [48]. The nano-composite showed a good
miscibility resulting from hydrogen bonding, and the ther-
mal stability and mechanical properties were also improved.
In the following research [49], the effects of aspect ratio,
surface area and dispersion of -ZrP on the properties of the
nano-composites were examined. Higher aspect ratio led to
significant improvements in modulus, tensile strength,
elongation at break and heat distortion temperature. But
high aspect ratio could result in poor dispersion of -ZrP
and cause deterioration of the film properties. Work of Lu
showed that the dispersion state and the chemical effect of
the -ZrP particles played important roles in the thermal
stability and flammability performance of the materials
[51,52].
2.5 Starch/-ZrP nano-composites
Starch is cheap, easy-to-get and completely biodegradable
polymer, which makes it one of the most promising raw
materials to be applied in various fields such as agriculture,
medicine and packaging. However, its mechanical and wa-
ter resistance properties are poor. In Wu’s work [54], a se-
ries of thermoplastic nano-composite films were synthe-
sized from glycerol-plasticized pea starch and -ZrP. The
presence of -ZrP decreased the moisture uptake of the
nano-composite films, resulting from the hydrogen bonding
formed between -ZrP and starch molecules. Composite
Figure 3 Schematic of the arrangement of PAM chains between the
interlayers of -ZrP [46].
March (2016) Vol.59 No.3 439
films of potato starch and -ZrP were also prepared by us-
ing glycerol as plasticizer agent and gels of -ZrP in water
as a source of high aspect ratio filler particles [55]. In this
work, the presence of the filler improves the thermal re-
sistance of the starch at both low and high temperatures.
3 Perspectives
Although the properties of the mentioned polymers can be
improved significantly by compositing with -ZrP, their
atomic level structures and mechanisms of the function of
-ZrP in polymer/-ZrP nano-composites are open yet.
Much work should be carried out on this area in the future
to guide the design of polymer/-ZrP nano-composites.
Besides experiments, computational simulation is another
choice. Until now, only one computational work on amor-
phous phase formation of the exfoliated ZrP was illustrated
[57]. Further work, by using both molecular dynamics sim-
ulations and Monte Carlo methods at the atomic level and
first-principles calculations at the electronic level, is neces-
sary in order to understand the mechanisms and improve the
applications of polymer/-ZrP nano-composites.
This work was supported by the National Natural Science Foundation of
China (Grant No. 51272009).
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