Applications of Metal-Organic Coordination Polymers As Precursors For Preparation of Nano-Materials

Coordination Chemistry Reviews 256 (2012) 2921–2943
Contents lists available at SciVerse ScienceDirect
Coordination Chemistry Reviews

journal homepage: www.elsevier.com/locate/ccr
Review
Applications of metal–organic coordination polymers as precursors

for preparation of nano-materials
Mohammad Yaser Masoomi, Ali Morsali ∗
Department of Chemistry, Faculty of Sciences, Tarbiat Modares University, P.O. Box 14155-4838, Tehran, Islamic Republic of Iran
Contents
1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2922
2. Nano metals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2923
3. Nano metal oxides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2923
3.1. Main group metal oxides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2924
3.2. Transition metal oxides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2931
3.3. Rare earth metal oxides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2933
4. Nano metal sulfides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2935
5. Other nano-materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2940
6. Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2940
Acknowledgment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2940
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2940
a r t i c l e i n f o a b s t r a c t
Article history: In this review we present methods for preparation of nano inorganic materials in which metal–organic
Received 12 December 2011 coordination polymers are used as precursors. Here we summarize the effects of various factors such
Accepted 25 May 2012 as structure, temperature, morphology and size of precursor on the morphology and size of the nano-
Available online 2 June 2012
materials produced. A review of the literature concludes that coordination polymers are suitable
precursors for production of nanoscale materials with optimized morphologies and properties.
Keywords:
© 2012 Elsevier B.V. All rights reserved.
Metal–organic coordination framework
Coordination polymer
Precursor
Nano-materials
Abbreviations: 2,3-pydcH2 , pyridine-2,3-dicarboxylic acid; 2,6-pydcH2 , 2,6-pyridinedicarboxylic acid; 2,4,6-tcp− , 2,4,6-trichlorophenoxide; 2,4-dnp− , 2,4-
dinitrophenoxide; 2,6-NDC, 2,6-naphthalene dicarboxylate; 2-Hpyc, 2-pyridinecarboxilic acid; 3-bpdb, 1,4-bis(3-pyridyl)-2,3-diaza-1,3-butadiene; 3-bpdh, 2,5-
bis(3-pyridyl)-3,4-diaza-2,4-hexadiene; 3-Hpyc, 3-pyridinecarboxylic acid; 3-np− , 3-nitrophenoxide; 4,4 -bipy, 4,4 -bipyridine; 4-bpdb, 1,4-bis(4-pyridyl)-2,3-
diaza-1,3-butadiene; 4-Hpyc, 4-pyridinecarboxylic acid; 9-HAc, 9-anthracene carboxylic acid; AmTAZ, 3-amino-1,2,4-triazole; ba− , benzylacetylacetonate; BDC,
1,4-benzenedicarboxylate; BF-TEM, bright field transmission electron microscopy; bpa, trans-1,2-bis(4-pyridyl)ethane; bpacbH, 3,5-bis[(4-pyridylamino)carbonyl]benzoic
acid; bpcdp, 2,6-bis(4-pyridinecarboxamide)pyridine; bpe, 1,2-bis(4-pyridyl)ethylene; bpfb, N,N -bis(4-pyridylformamide)-1,4-benzene; bpp, 1,3-di(4-pyridyl) propane;
BTC, 1,3,5-benzenetricarboxylate; DdDTP, O,O -didodecyldithiophosphates; DMF, N,N -dimethylformamide; DPOAc− , diphenylacetate; FCA, 3-ferrocenyl-2-crotonic acid; FE-
SEM, field emission scanning electron microscope; Fum, fumarate; GB, 2-guanidinobenzimidazole; H2 ABDC, 2-aminoterephthalic acid; H2 ADC, acetylenedicarboxylic acid;
H2 Mal, maleic acid; H2 PDC, 2,3-pyrazinedicarboxylic acid; H2 sal, salicylic acid; H2 SB, 4-[(4-hydroxyphenyl)sulfonyl]-1-benzenol; H3 Sglu, N-(2-hydroxybenzyl)-l-glutamic
acid; H3 Sser, N-(2-hydroxybenzyl)-l-serine; H4 BTEC, 1,2,4,5-benzenetetracarboxylic acid; hfacac− , hexafluoroacetylacetonate; HMPAcO, monophenyl acetic acid; Hpic, picol-
inic acid; NTA, nitrilotriacetic acid; OAc− , acetate; ODTP, O,O -dioctyldithiophosphates; pyr, pyrazine; SAED, selected area electron diffraction; tda, S(CH2 COO)2 2− ; TFPB− ,
4,4,4-trifluoro-1-phenyl-1,3-butandionate; THDA, 2,5-thiophenedicarboxylic acid; ths, thiosemicarbazide; TPOAc− , triphenylacetate; tsc, thiosemicarbazide; tu, thiourea;
H2 L1, 2,6-bis[(4-carboxyanilino)carbonyl]pyridine; H2 L2, 4-[(1H-imidazol-4-yl)methylamino]benzoic acid; H2 L3, N,N -phenylenebis(salicylideneimine)dicarboxylic acid;
HL4, 1H-1,2,4-triazole-3-carboxylic acid; w value, water/surfactant molar ratio.
∗ Corresponding author. Tel.: +98 2182884416; fax: +98 88009730.
E-mail address: morsali a@modares.ac.ir (A. Morsali).
0010-8545/$ – see front matter © 2012 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.ccr.2012.05.032
2922 M.Y. Masoomi, A. Morsali / Coordination Chemistry Reviews 256 (2012) 2921–2943
Fig. 1. (A) High magnification FE-SEM image of as-synthesized Cu superstructures by thermolysis of the Cu-BTC MOF in the OCTF at 500 ◦ C for 10 h and (B) a photograph of
one kind of corals. (C and D) TEM images of the formed Cu nanoparticles on the surface of as-synthesized Cu superstructures [102].
Reproduced with permission of Elsevier.
1. Introduction materials find very diverse potential applications including cataly-

sis [40], magnetism [41], optics [42–45], sensors [46,47], biosensing
Metal–organic coordination polymers (MOCPs) contain metal [48–51], medical diagnostics [52,53], energy storage and batteries
ions linked by coordinated ligands into an infinite array [1–6]. [54,55], data storage [56,57] and others [58].
This is a general term that incorporates a variety of architec- MOCPs can be used as templates in order to obtain the desired
tures ranging from simple one-dimensional chains with small nano-materials. By choosing appropriate MOCP precursors with
ligands to large mesoporous frameworks like metal–organic special morphologies and under suitable experimental conditions,
frameworks (MOFs) [7,8]. Generally, the formation process pro- obtaining the desired morphologies will become possible. Nano
ceeds automatically and, therefore is called a self-assembly MOCP precursors may also be used to obtain nano-materials with
process [9–11]. better and more useful properties [59–61]. Depending on the con-
The chemical and physical properties of solid materials strongly ditions, MOCPs precursor may lead to the preparation of metals,
depend on the size and shape of the microscopic of which the metal oxides, metal sulfides or other nano sized materials. With this
compounds are made [12–14]. This is especially true for materi- method, nano-materials can be obtained in different morphologies
als with morphological features smaller than a micron in at least from different MOCPs precursors.
one dimension, commonly called nano-scale materials, or simply There are many methods for the preparation of nano-
nano-materials. Not only composition of nano-materials, but also materials including hydrothermal or solvothermal methods
their structure, morphology, phase, shape, size, distribution, and [62–64], microwave-solvothermal synthesis [65,66], microwave
spatial arrangement are affected by their physical and chemical synthesis [67,68], magnetic-field-assisted hydrothermal [69],
properties [15–21]. In such materials the ratio of surface area to vol- sol–gel process [70,71], electrochemically induced sol–gel [72],
ume is vastly increased when compared to compounds with larger microemulsion [73] and reverse micelle/microemulsion [74,75],
grain sizes and quantum mechanical effects such as the “quantum homogeneous precipitation method [76], cluster growth method
size effect” begin to play a significant role. These effects only play [77], chemical vapor deposition [78], vapor–liquid–solid process
a minor role when going from macro to micro dimensions, but [79,80], soft chemical method [81], electrophoretic deposition
become increasingly important when reaching the nanometer size [82], electrochemical fabrication [83], chemical reduction method
range. Controlling the growth of materials at the submicrometer [84,85], electrolysis of metal salts [86], rapid expansion of super-
scale is of central importance in the emerging field of nanotech- critical solvents [87,88], photoreduction of metal ions [89,90],
nology [22–27]. If exact control of size and shape of a compound is microwave plasma synthesis [91], sonochemical method [92,93]
possible, their chemical and physical properties can be altered as and mechanochemical process [94].
desired [28,29]. In this review we introduce most of the studies dealing
In the past decades, synthesis, characterization and investiga- with application of MOCPs as precursors for the synthesis of
tion of properties as well as applications of nanostructure materials nano-materials. We have tried to be comprehensive but there cer-
have been the subject of extensive research [30–36]. This trend has tainly must have been studies which were not included in this
found an even greater pace in the past few years [37–39]. These work.
M.Y. Masoomi, A. Morsali / Coordination Chemistry Reviews 256 (2012) 2921–2943 2923
2. Nano metals
Metal nanoparticles are important for technological applica-

tions in various domains of science and industry, especially in
catalysis due to their high activity. The controlled and repro-
ducible synthesis of defined and stable metal nanoparticles with
a small size distribution is very important for a range of applica-
tions [95–98]. As such, metal nanoparticles of small size (<5 nm)
are only kinetically stable and will combine to thermodynamically
favor larger metal particles via agglomeration. This tendency for
aggregation is due to the high surface energy and the large surface
area of metal nanoparticle [99].
In general, Cu nano- and microstructures can be synthesized
in solution or solid state with the presence of chemical reduc-
ing agent [24,45,100,101]. In one of the reported applications
of MOCPs as precursors, calcination of [Cu3 (BTC)2 ] MOF in a
one-end closed horizontal tube furnace (OCTF) has led to the
formation of coralloid microstructures with surface interspersed
comprised of Cu nanoparticle clusters (Fig. 1) [102]. The forma-
tion process of Cu nano- and microstructures from thermolysis
of [Cu3 (BTC)2 ] MOF precursor includes decomposition, reduc-
tion, nucleation, and growth. As a result the decomposed Cu
forms symmetrical coralloid super-structures in the reductive
environment (Fig. 1).
Due to its unique properties, silver has been extensively used in a
variety of applications such as catalysis, electronics, photonics, pho-
tography and antibacterial functions [103–106]. For example, silver
has the highest electrical conductivity, thermal conductivity and
reflectivity of all metals [107]. Furthermore, silver nanoparticles
exhibit remarkable size effects in biological and medicine-related
properties [108].
Use of silver MOCPs or silver nano-MOCPs for preparation of
silver nano structures is not widely investigated. There are several
other methods that can be applied to synthesize silver nanoparti-
cles with well-defined shapes [73,86–91,94,109].
As an example for the application of MOCPs for synthesis
of nano metallic silver, calcination of nanorods of 1D-MOCP
precursor, [Ag2 (␮5 -TPOAc)2 ]n , lead to the fabrication of silver
nano-fibers (Fig. 2) [110]. Probably the 1D crystal structure of
[Ag2 (␮5 -TPOAc)2 ]n as precursor influences the production of
MOCP nanorods. During the calcination process, rod-shaped MOCP,
[Ag2 (␮5 -TPOAc)2 ]n , leads to production of Ag with a fibrous mor-
phology.
From direct calcination of nano-MOCPs, [Ag(␮4 -DPOAc)]n Fig. 2. (A) A fragment of 1D pencil shaped of [Ag2 (␮5 -TPOAc)2 ]n (Ag = violet, O = red,
[111], [Ag(␮3 -HMal)]n [112], [Ag2 (␮2 -4-pyc)2 ]n [113] and [Ag(␮- C = gray, H = white). (B) SEM image of compound [Ag2 (␮5 -TPOAc)2 ]n nanorods
obtained from sonochemical method. (C) SEM image of silver nanofibers, fabricated
bpfb)(NO3 )]n [114], agglomerated metallic silver with spongy
from calcination process of compound [Ag2 (␮5 -TPOAc)2 ]n nanorods at 500 ◦ C [110].
nanostructure have been obtained. In the last case, [Ag(␮-
Reproduced by permission of The Royal Society of Chemistry.
bpfb)(NO3 )]n , Ag2 O concomitant with Ag is present in the final
product. Besides, the thermal decomposition of the precursors in
the presence of oleic acid as surfactant can produce Ag monodis-
perse nanoparticles (Fig. 3). nanoparticles which is itself controlled by the pore size of the
In another case, 3D-MOCP [Ag2 (␮8 -SB)]n , was used to prepare silica matrix used. The temperature of calcination can also have
Ag nanoparticles in two ways, one was from calcination of its nano- an effect on the size of particles. These effects lead to the forma-
powders and another by the hydrothermal method. The former tion of particles of 3.0, 4.9 and 6.9 nm. The blocking temperatures
produces smaller particles than the latter [115]. as well as the energy barriers decrease with a reduction in the size
MOCPs may also be used in the synthesis of certain alloys, which of the nanoparticles obtained [118].
is a rare phenomenon [116]. GeFe1.4 alloy nanoparticles have been
obtained using nano MOCP, Ge–ox–Fe (ox = oxalate) as precursor,
in a reaction including solid phase reduction under H2 above 800 ◦ C 3. Nano metal oxides
accompanied by decomposition. The converted GeFe1.4 nanoparti-
cles exhibited unique ferromagnetic behavior [117]. Metal oxides display appealing electronic, optical, thermo
In another case, NiFe nanoparticles were obtained by thermol- electronic, photoelectronic and bactericidal properties [119–122].
ysis of the cyano-bridged Ni2+ /[Fe(CN)6 ]3− MOCP nanoparticles It is obvious that depending on its metal ions, various prop-
anchored within a hybrid mesostructured silica either under argon erties are observed. MOCPs can be used as templates or
or under a hydrogen atmosphere (Fig. 4) [118]. The size of these precursors to generate metal oxides with a wide range of
nanoparticles may be controlled by the size of cyano-bridged MOCP shapes.
Fig. 3. SEM images of silver spongy nano structures and nanoparticles of Ag prepared by calcination of compounds: (A, a) [Ag(␮4 -DPOAc)]n , (B, b) [Ag(␮3 -HMal)]n , (C, c)
[Ag2 (␮2 -4-pyc)2 ]n and (D, d) [Ag(␮-bpfb)(NO3 )]n . Capital letters represent nanostructures and small letters represent nanoparticles prepared in the presence of oleic acid as
surfactant [111–114].
Reproduced with permission of Elsevier and reproduced with permission of Springer-Verlag GmbH.
3.1. Main group metal oxides Indium(III) oxide (In2 O3 ) is an important n-type semiconduc-
tor that is widely used for gas sensor [124,125], photocatalysis,
Al2 O3 nanostructures were obtained in different morpholo- photovoltaic and optoelectronic devices [126,127]. It has been
gies, including cubic and coral structures, from calcination of developed in many different morphologies through several meth-
[Al8 (OH)15 (H2 O)3 (BTC)3 ]n (MIL-110) under different conditions ods [128–130].
[123]. In2 O3 nanoparticles were obtained by direct thermal decompo-
sition of compounds [In2 (OH)2 (BTEC)]n ·2nH2 O (MIL-60) [131] and
[In2 (OH)3 (BDC)1.5 ]n [132], in which there is no particle aggrega-
tion and the nanoparticles are clearly distinct. Also from calcination
of a series of In(III) coordination polymer particles (CPP), CPP-3,
CPP-5 [133], CPP-6, CPP-7 and CPP-8 [134], different morphologies
of In2 O3 have been achieved. Porous MOCPs, CPP-3 and CPP-
5 are comprised of BDC ligands and form [In(OH)(BDC)]n that
have the same components but different morphologies, while
CPP-6, CPP-7 and CPP-8 were prepared by the solvothermal
Fig. 4. Schematic representation of the two-step approach for the synthesis of NiFe
bimetallic nanoparticles in the mesostructured silica matrix [118]. reaction of In(NO3 )3 ·xH2 O and L1 ligands in which com-
Reproduced by permission of The Royal Society of Chemistry. pound morphologies change by simply adding acetonitrile under
Fig. 5. SEM images of (A-top) hexagonal rod-shaped precursor CPP-3, (B-top) hexagonal disk-shaped precursor CPP-5, (C-top) elongated hexagon-shaped precursor CPP-6,
(D-top) ellipsoid-shaped precursor CPP-7 and (E-top) rod-shaped precursor CPP-8. SEM (middle) and TEM (bottom) images of (A) non-hollow hexagonal rod-shaped In2 O3 , (B)
non-hollow hexagonal disk-shaped In2 O3 , (C) hollow elongated hexagon-shaped In2 O3 , (D) hollow ellipsoid-shaped In2 O3 , and (E) hollow rod-shaped In2 O3 after calcination.
Insets are high magnification SEM images and SAED patterns of the resulting In2 O3 [135].
otherwise identical reaction conditions (Fig. 5). In all these thermolysis at 600 ◦ C, thermal decomposition in oleic acid at 285 ◦ C,
cases the initial morphology of MOCP precursors was maintained and sol–gel method in polyvinyl alcohol at 400 ◦ C of MOCP [Tl(2,4,6-
[135]. These morphologies include, non-hollow micro hexago- tcp)]n , respectively [139].
nal rod-shaped, non-hollow hexagonal disk-shaped, hollow micro Another metal–oxide that can be obtained from thermolysis of
elongated hexagonal-shaped, hollow micro ellipsoid and rod- MOCPs is lead oxide which is fascinating because of its numerous
shaped that are all polycrystalline In2 O3 , consisting of numerous compositions and phases, such as PbO, Pb2 O, Pb2 O3 , and Pb3 O4 . PbO
In2 O3 nanocrystallites with an average size of ∼20–40 nm (Fig. 5). powders remain widely used because they are cheap and reliable
Different physical properties such as thermal stability in CPP-3 and materials for battery applications [140]. Some other methods have
CPP-6 compounds may be caused by the different compositions also been used for preparation of PbO [141–144].
and porosities of the two CPPs. CPP-3 is considered to be a perma- The following compounds are used for preparation of PbO
nently porous material with a total pore volume of 0.6101 cm3 g−1 , nanoparticles in various morphologies (e.g. aggregation of
however CPP-6 is a non-porous material with a total pore vol- nanoparticles, block nano-structures and nano-powder) via ther-
ume of 0.0113 cm3 g−1 . This difference in composition and porosity mal decomposition; [Pb(␮-4-pyc)(␮-N3 )(␮-H2 O)]n [145], [Pb(␮6 -
may affect the production of different morphologies of non-hollow Fum)]n [146], [Pb(␮-NO2 )(␮-pyc)(H2 O)]n [147], [Pb2 (␮3 -ba)2 (␮2 -
and hollow that is influenced by the decomposition mechanism of ba)2 ]n [148], {[Pb(bpacb)(OAc)]·DMF}n [149], [Pb(␮-4,4 -bipy)
MOCP precursors.
Calcination of compounds [Tl(3-np)]n and [Tl(2,4-dnp)]n pro-
duces the micro flower-like and nano crystalline powder Tl2 O3
with average size of 95 and 85 nm, respectively [136]. Moreover
from calcination of MOCPs [Tl2 (␮3 -9-Ac)(␮4 -9-Ac)(H2 O)]n [137]
and [Tl4 (␮3 -4-HBN)4 ] [138] a nano-structural surface of Tl2 O3 has
been obtained. Also nanostructures of Tl2 O3 in three different mor-
phologies with flower-like nanostructures, nano- and micro-rods,
were generated by calcination using three different methods, direct
Fig. 6. Growth illustration of Pt/ZnO nanoparticles produced by direct calcination Fig. 7. TEM images of C/ZnO produced by calcination of MOF-5 at 480 ◦ C [230].
of MOF-5 soaked in platinum tetrachloride [229]. Reproduced with permission of American Chemical Society.
Fig. 8. (A) Illustrations of the framework of [Zn(4,4 -bipy)Cl2 ]n and the formation
process to ZnO nanorods. (B) Illustrations of the framework of [Zn(ox)(4,4 -bipy)]n
and the formation process to ZnO radial nano-needles [231].
Reproduced with permission of IOP Publishing Ltd.
(␮-OAc)(hfacac)]n [150], [Pb2 (HBTC)2 (H2 O)4 ]·H2 O [151], [Pb2 (␮-3-
bpdh)(␮-NO3 )3 (NO3 )]n [152], [Pb2 (␮-bpe)3 (␮-NO3 )2 (NO3 )2 ]n and
{[Pb(␮-bpe)(␮-NO3 )2 (NO3 )(H2 O)]·(Hbpe)0.5 (bpe)}n [153], [Pb(␮-
TFPB)2 ]n [154], [Pb2 (2-pyc)2 (I)2 ] [155], [Pb(3-pyc)(N3 )(H2 O)]n
Fig. 9. (A and B) FE-SEM and TEM images of ZnO nanorods produced by calcination
[156], [Pb2 (4-pyc)2 I2 (H2 O)]n and [Pb(3-pyc)I]n [157], [Pb(␮-
of [Zn(4,4 -bipy)Cl2 ]n . The upper insets are a representative nanorod and an in situ
bpp)(␮-Br)2 ]n [158], [Pb(␮-pyr)(␮-I)2 ]n [159], [Pb(3-pyc)2 ]n [160], ED pattern. TEM images of (C) intermediates collected after 6 h reaction for ZnO
[Pb(2-pyc)(N3 )(H2 O)]n [161], [Pb(DPOAc)2 ]n , [Pb(MPAcO)2 ]n [162] nanorods and (D) for ZnO radial nano-needles. (E–G) FE-SEM, magnified FE-SEM
and microparticles of [Pb(␮7 -Mal)]n [163]. In all cases the PbO that and TEM images of ZnO radial nano-needles produced by calcination of [Zn(ox)(4,4 -
is obtained from nano coordination polymers or using surfactant, bipy)]n [231].
have the best morphology or particle size. Reproduced with permission of IOP Publishing Ltd.
Aggregated nanoparticles of Bi2 O3 have been obtained from

the calcination of MOCP, {[Bi(␮-4,4 -bipy)Br4 ]·(4,4 -Hbipy)}n [164] and nanonails [208], nanohelix [209], hierarchical nanostructures
under an air atmosphere. [210,211] and colloidal or arrayed nanocrystals [212–214], have
ZnO is a polar inorganic and an important semiconductor been fabricated. The photoluminescence (PL) spectroscopy studies
material with a wide direct energy band gap of 3.37 eV [165] of ZnO show that they are sensitive to the particle size, temperature,
and large excitonic binding energy of 60 meV [166–168]. It has preparation method, etc. [23,130,166,215–217].
attracted intensive study due to its wide potential applications Thermal decomposition of several different MOCPs, such as
in optics [169], optoelectronics [170], photoelectric devices [171], ([Zn(␮-4,4 -bipy)(␮-3-bpdh)(H2 O)2 ](ClO4 )2 ·(4,4 -bipy)0.5 )n [218],
electronic devices [172], surface acoustic wave devices [173,174], ([Zn(␮-4,4 -bipy)(␮-3-bpdb)(H2 O)2 ](ClO4 )2 ·4,4 -bipy·3-bpdb·
field-emission devices [175,176], sensors [177,178], ultraviolet H2 O)n [219], [Zn(4-bpdb)(NO2 )2 ]n and ([Zn(3-bpdb)(NO2 )]·
lasers [179], solar cells [180,181], nanoresonators and cantilevers 0.5H2 O)n [220], [Zn(3-bpdh)(NO2 )2 ]n [221], {[Zn(GB)2 ]·(␮-
[182,183], varistors [184], catalysis [185], adsorption [186], actu- bpe)3 }n (ClO4 )2n ·nH2 O [222], [Zn(␮-3-bpdh)2 (N3 )2 ]n [223], [Zn(␮-
ators, energy, biomedical sciences and spintronics [187–189]. 3-bpdh)(H2 O)4 ](NO3 )2 ·2(3-bpdh) and [Zn(␮-3-bpdh)(H2 O)4 ]
Various synthetic methods have been developed to synthesize zinc (ClO4 )2 ·2(3-bpdh) [224], {[Zn(␮-3-bpdb)(3-bpdb)2 (H2 O)2 ](ClO4 )2 ·
oxide nanostructures [81,82,190–192], some of which are environ- 3-bpdb}n [225], {[Zn(bpcdp)2 (DMF)4 ](ClO4 )2 ·(H2 O)2 }n [226],
mentally friendly [193]. {[Zn(3-bpdb)(NO2 )]·0.5H2 O}n , [Zn(4-bpdb)(NO2 )2 ]n [227] and
ZnO nanostructures with a broad range of features, including Zn(ABDC)(ADC) [228] under various conditions has led to the
nanowires [194], nanobelts [130,195], nanorods [81,196], nanor- formation of ZnO nanostructures with different sizes and mor-
ings [197], nanotubes [198], nanotetrapods [199,200], nanoflowers phologies. In the preparation process, the effects of temperature,
[201], nanodisks [202], cones [203], towers [204], hollow spheres adding surfactant and size of MOCP precursor have been inves-
[185,205], nanosprings and nanospirals [206,207], nanobridges tigated. For example the last compound, Zn(ABDC)(ADC) shows
Fig. 10. (A) The typical 3D pillared framework and (B) SEM image of complex
[Zn(L2)]n [233].
Fig. 12. (A) Proposed mechanism for the synthesis of micrometer-sized hexago-
remarkably strong and stable visible light emission centered at
nal ZnO rings by a combination of template-directed coordination polymer growth
600 nm. and thermal decomposition of compound Zn(L3)(BDC). (B and C) Low- and high-
Nanocrystalline ZnO nanoparticles have also been obtained magnification SEM images of hexagonal-ring ZnO [234,235].
from calcination of MOF-5, [Zn4 O(BDC)]3 , at 600 ◦ C, but it is Reproduced with permission of Wiley-VCH Verlag GmbH & Co. KGaA.
interesting that upon calcination of MOF-5 soaked in platinum
tetrachloride DMF solution, platinum-supporting zinc oxide
(Pt/ZnO) nanoparticles have been generated (Fig. 6) [229]. The
resultant Pt/ZnO samples with average diameters of 30 nm
Fig. 11. SEM images of ZnO obtained by calcination of [Zn(L2)]n at 500 ◦ C for 10 h (A), 15 h (B), 600 ◦ C for 10 h (C), 15 h (D), 700 ◦ C for 10 h (E), 15 h (F) [233].
Fig. 15. (A) The reaction process from [Mn(SO4 )(4,4 -bipy)(H2 O)2 ]n to the ␥-MnO2
crystal lattice. (B) FE-SEM image of ␥-MnO2 nanowires produced by oxidation reac-
tion on [Mn(SO4 )(4,4 -bipy)(H2 O)2 ]n [247].
Reproduced with permission of Wiley-VCH Verlag GmbH & Co. KGaA.
display higher catalytic activity for CO oxidation than conventional

Pt/ZnO catalyst. In another experiment, calcination of MOF-5
at 480 ◦ C resulted in sphere-shaped 10 nm ZnO nanoparticles
which were covered by amorphous carbon, C/ZnO (Fig. 7). How-
Fig. 13. (A) SEM image of MOCP Zn(ABDC)(THDA) precursor. (B) SEM image of ZnO
nanostructures produced by calcination of the Zn(ABDC)(THDA) as precursor at
ever, mesoporous carbon with a large surface area of 1844 m2 /g
550 ◦ C in air atmosphere for 75 min [228]. may also be generated by the removal of ZnO from the C/ZnO
Reproduced by permission of The Royal Society of Chemistry. nanoparticles [230].
A nanorod morphology of ZnO has been obtained by calcina-
tion of [Zn(3-bpdh)(NO2 )2 ]n [220], [Zn(␮-3-bpdh)(NO2 )2 ]n [224],
[Zn(4,4 -bipy)Cl2 ]n (Fig. 9A and B) [231] and [ZnF(AmTAZ)]·solvents
[232]. Moreover, from calcination of 2D-MOCP, [Zn(ox)(4,4 -
bipy)]n , ZnO radial nano-needles are formed (Fig. 9E–G) [231].
Comparison of these different morphologies obtained by differ-
ent MOCPs reveals that the different frameworks of MOCPs could
influence the final morphology of ZnO nanostructures. This may
be derived by various intermediates in the formation process,
and the intermediates then mature to different morphologies
in the final product (Fig. 8). TEM image of intermediates of
compounds [Zn(ox)(4,4 -bipy)]n and [Zn(4,4 -bipy)Cl2 ]n shows dif-
ferent morphologies, the intermediates of ZnO nanorods were
some rod-shaped nanoparticles (Fig. 9C), while those of ZnO radial
nanoneedles were spherically aggregated nanoparticles (Fig. 9D),
that finally led to the different morphology of nanorods and
radial nano-needles (Fig. 9). The photoluminescence properties of
[Zn(ox)(4,4 -bipy)]n and [Zn(4,4 -bipy)Cl2 ]n have been investigated
and has shown that the method of preparation plays a key role in
the optical properties of the ZnO nanostructures [231].
Thermal decomposition of 3D-MOCP [Zn(L2)]n (Fig. 10) at dif-
ferent temperatures shows that an increase in the thermolysis
temperature influences morphology and changes it from nanopar-
ticles into nanorods (Fig. 11) [233]. Observations suggest that at
500 ◦ C, ZnO particles are spherical and similar to that of the pre-
cursor, while the sizes of ZnO particles are smaller than those of
the precursor. A mechanism for the production of final nanorods
was proposed on the basis of the structural changes of the MOCP
precursor in the calcination process which can be attributed to the
Fig. 14. (A) ORTEP diagram of one-dimensional zigzag chain of
loss of L22− ligands [233].
[Cd(BDC)2 (H2 O)3 ]n ·4H2 O. (B) TEM image of CdO nanowires produced by calcination
of [Cd(BDC)2 (H2 O)3 ]n ·4H2 O [239]. Hexagonal-ring MOCP Zn(L3)(BDC) can be used as a template
Reproduced with permission of Elsevier. for the preparation of ZnO micro hexagonal-rings. The overall size
of the hexagonal-ring ZnO was reduced to approximately 1.16 ␮m
Fig. 16. (A) SEM image of an individual Fe2 O3 crystal obtained by calcination of K4 [Fe(CN)6 ]. (B) An enlarged image of the surface of the Fe2 O3 crystal. (C) TEM image of an
individual Fe2 O3 crystal prepared by calcination of K4 [Fe(CN)6 ]. Inset is the SAED pattern of it. (D) An enlarged TEM image of the Fe2 O3 crystal [259].
Fig. 17. (A) The selective preparation of hematite (␣-Fe2 O3 ) and magnetite (Fe3 O4 ) nanorods from coordination polymer nanorods (Fe-MIL-88B), (B) SEM image of the
resulting hematite nanorods with an average width of 70 ± 8 nm produced by calcination of Fe-MIL-88B at 380 ◦ C in air atmosphere and (C) SEM image of the resulting
magnetite nanorods with an average width of 70 ± 12 nm produced by calcination of the organic residue-containing hematite after the second thermal treatment up to 700 ◦ C
under a nitrogen atmosphere [260].
Fig. 18. (A) Growth illustration of agglomerated Co3 O4 nanoparticles, (B) SEM images of the Co3 O4 prepared by calcination of [Co3 (2,6-NDC)3 (DMF)4 ]n and (C) enlarged
region in (B) [272].
compared to hexagonal-ring CPP of the precursor (ca. 2.34 ␮m) In another case, the thermal decomposition of 2D-MOCP,
(Fig. 12) [234]. The ZnO maintains the original morphology of the Zn(tda)(H2 O), led to the production of ZnO with a porous and
precursor during the solid-state transformation. Also after calcina- sponge-like structure with an extensive connection of thick flakes
tion, Zn(ABDC)(THDA) is transformed into ZnO which is a porous containing large pores of average diameter of ∼10 ␮m. The fine
hexagonal nanostructure in which the original morphology of the structure of a single flake consists of countless ZnO crystals of aver-
precursor is maintained (Fig. 13) [228]. age size of ∼10 nm [236].
Fig. 19. SEM images of (A) the precursor Ni3 (BTC)2 ·12H2 O, (B) the synthesized porous NiO prepared by calcination of [Ni3 (BTC)2 ·12H2 O] at 400 ◦ C for 24 h and (C and D)
HRTEM images of the NiO at different magnification. The inset of (D) contains the selected area diffraction pattern [282].
3.2. Transition metal oxides
Manganese is a transition metal whose oxides are important for

their applications in battery technologies and catalysis due to its
ability to completely oxidize various volatile organic substances
or hydrocarbons [18,166,240,241]. Besides using MOCPs as precur-
sor for preparation of manganese oxides, some other preparation
methods have been used [242–246].
Through oxidation reaction on MOCP precursor, [Mn(SO4 )(4,4 -
bipy)(H2 O)2 ]n , nanowires of ␥-MnO2 have been achieved whose
product consists of nanowires with average diameters of 20–40 nm
and lengths ranging from 3 to 6 ␮m (Fig. 15) [247]. In the
process of oxidation, the different coordination abilities of the
ligands in the polymer will probably lead to a faster oxida-
tion along one direction, which results in an oriented growth
of metal oxide nanowires. Carrying out the same process on
another polymer such as [Mn(N3 )2 (4,4 -bipy)]n [248] has led to
no nanowires which can indicate the importance of crystal struc-
ture of the coordination polymer on the morphology of the final
Fig. 20. Formation process of TPBA cubes and their thermal conversion to material.
nanoporous Ti–Fe-based oxides [283].
Iron(III) oxides, as important metal oxides, contain several poly-
morphs including ␣-Fe2 O3 , ␤-Fe2 O3 , ␥-Fe2 O3 , ␧-Fe2 O3 [249]. Fe2 O3
has potential applications in pigments, catalysis, magnetic stor-
The MOCPs, {[Cd(bpa)(4,4 -bipy)2 (H2 O)2 ](ClO4 )2 }n [237] and age, batteries, and biomedical applications such as drug delivery
[Cd3 (3-pyc)4 (N3 )2 (H2 O)]n [238] are used for preparation of CdO [249–254]. In addition to the method that we describe here, other
nanoparticles. In both cases, using oleic acid as a surfactant is preparation methods have been developed to synthesize iron(III)
not beneficial and leads to the production of larger particle size. oxides [254–257].
Increasing the temperature of calcination can also have a similar From calcination of Prussian blue Fe4 [Fe(CN)6 ]3 [258] and its
effect, but using nano-MOCP of these compounds as precursor leads analogs K4 [Fe(CN)6 ] [259] cubic ␤-Fe2 O3 and spinel ␥-Fe2 O3 poly-
to a decrease in particle size. Another example is the production morphs have been achieved at temperatures of 350 and 450 ◦ C,
of CdO from calcination of 1D-MOCP, [Cd(BDC)2 (H2 O)3 ]n ·4H2 O, respectively. The former is in the form of crystalline nano-powder
which has a nanowire morphology (Fig. 14) [239]. Probably the latter has an elongated cubic shape that is made up of an aggre-
during thermal decomposition, 1D infinite zigzag chains in gation of nanocrystals (Fig. 16). Calcination of Fe4 [Fe(CN)6 ]3 at a
the precursor influence the final 1D metal oxide nano-sized minimum decomposition temperature of 250 ◦ C, yields sponge-like
structure. agglomerates between 30 and 120 nm, comprised of ultra-small
Fig. 21. (A) Structural schematic diagram on formation process of the Eu(BTC)·6H2 O nanorods. (B and C) FE-SEM images of Eu(BTC)·6H2 O. (D and E) FE-SEM images of the
Eu2 O3 [289].
Reproduced with permission of American Chemical Society.
Fig. 22. (A) Schematic representation of the preparation of the silica@Ln2 O3 core/shell and hollow Ln2 O3 microspheres (Ln = Gd3+ , Eu3+ , Y3+ ) from silica@coordination polymer
core/shell microspheres. TEM images of (B) silica@coordination polymer core/shell microspheres with an average diameter of (1.31 ± 0.02 ␮m), (C) silica@Gd2 O3 core/shell
microspheres and (D) hollow Gd2 O3 microspheres with an average layer thickness of (40 nm ± 8 nm), (E) TEM and SEM (inset) images of hollow Eu2 O3 microspheres with an
average layer thickness of (48 nm ± 11 nm) and (F) TEM and SEM (inset) images of hollow Y2 O3 microspheres with an average layer thickness of (31 nm ± 6 nm) [290].
amorphous Fe2 O3 nanoparticles with a size of 1–4 nm and large 250 nm have been obtained consisting of small nanoparticles with
surface area of 400–200 m2 /g depending on the Prussian blue par- the size of about 25 nm (Fig. 18) [272]. The electrochemical prop-
ticle size [258]. Also by controlling the calcination conditions of erties of the Co3 O4 have also been examined.
Fe-MIL-88B nanorods, hematite (␣-Fe2 O3 ) and magnetite (Fe3 O4 ) Thermal treatment of Co(NTA)H nanowires provided porous
nanorods have been selectively prepared while maintaining the Co3 O4 nanowires. The electrochemistry test results show that
original morphology of the precursor (Fig. 17) [260]. the porous Co3 O4 nanowires exhibit a high reversible capacity of
Co3 O4 as a p-type semi-conductor has been studied due to 810 mAh g−1 and stable cyclic retention at 30th [273].
its wide applications in magnetic materials [261,262], catalysts Nano-structured NiO is another p-type semiconductor which
[263], sensors [264] and electrochemistry [265,266]. Several other has important applications including preparation of cathode mate-
methods can be used for preparation of nano sized cobalt oxides rials of alkaline batteries [274], electrochemical capacitors [275],
[267–270]. smart windows [276] and active layer for gas sensors [277,278].
From thermal decomposition of Co-BDC coordination polymer, In addition to the production of NiO from MOCP precursors, some
3D superstructures of Co3 O4 have been produced, assembled from other preparation methods for synthesis of NiO nano structures
hundreds of microscale 2D-sheets, densely composed of many have been developed [269,279–281]. Nano-strand mesoporous
uniform nanoparticles with an estimated mean size of ca. 30 nm NiO was obtained through calcination of coordination polymer
[271]. The BET surface area of Co3 O4 nano/micro superstructure is [Ni3 (BTC)2 ·12H2 O], in which NiO arrays keep the morphology of the
21.5 cm2 g−1 , the pore volume is 0.16 cm3 g−1 and the average pore precursor [Ni3 (BTC)2 ·12H2 O] (Fig. 19) [282]. The electrochemical
size is 28.8 nm. Such hierarchical porosity of Co3 O4 nano/micro properties of the NiO have also been examined.
superstructures can facilitate electrolyte impregnating into parti- By direct calcination of [Cu3 (BTC)2 ] or by in situ thermal calci-
cles and ensure that there are enough electrolyte ions to rapidly nation of the coralloid Cu 3D superstructures in air (Section 2) the
contact the much larger surfaces of the electroactive Co3 O4 mate- morphology remained unchanged and CuO coralloid microstruc-
rials [271]. tures were obtained [102].
Also upon heating of MOF [Co3 (2,6-NDC)3 (DMF)4 ]n , by con- In one case calcination of titanium containing Prussian blue
verting cobalt oxide subunits in a cobalt-MOF via pyrolysis, analog (TPBA), K0.25 Ti[Fe0.875 (CN)6 ]·6H2 O, led to the production of
agglomerated Co3 O4 nanoparticles with the diameter of around microstructural nanoporous cubes of mixed titanium-iron-based
Fig. 23. (A) La–asparagine coordination compound hollow sphere obtained with reactant quantity (asparagine:La3+ ) = 6 mmol:0.125 mmol after reaction at 160 ◦ C for 12 h.
(B and C) SEM images of corresponding La2 O3 hollow spheres after calcination. (D) TEM image of La2 O3 hollow spheres. (E) SEM images of Ce–asparagine coordination
compound microspheres. (F) CeO2 core–shell spheres obtained by calcination of Ce–asparagine coordination compound spheres [291].
oxides, TiO2 –Fe2 O3 . The initial morphology of the precursor cubes amounts of coordination polymer precursors and silica cores, the
was retained even after calcination (Fig. 20) [283]. thicknesses of the shells within the silica@coordination polymer
core/shell structures can be controlled [290].
3.3. Rare earth metal oxides After calcination of La–asparagine coordination compound
at 720 ◦ C, La2 O3 micro hollow spheres are obtained with wall
Rare earth oxides and mixed oxides have wide applications due thickness of ca. 100 nm (Fig. 23A–D) [291]. Also by calcina-
to their luminescent, catalytic, electric, and magnetic properties tion of Ce–asparagine coordination compound, CeO2 core–shell
[284–288]. microspheres were obtained that are assembled by CeO2
From thermal decomposition of Eu(BTC)·6H2 O nanorods, Eu2 O3 nanoparticles (Fig. 23F) [291]. The core–shell CeO2 microspheres
nanorods were obtained with the same morphology as their pre- consisting of nanoparticles may offer a potential candidate
cursor with diameters of 80–100 nm and lengths of 1–2 ␮m (Fig. 21) material for CeO2 -based solar cells. Moreover after calcination
[289]. A balance between the inner force of molecular stacking and of lanthanide–asparagine coordination compounds (lanthanide
the external force of solubility seem to be responsible for forma- ions = Pr-, Nd-, Sm-, Eu), Pr6 O11 , Nd2 O3 , Sm2 O3 , Eu2 O3 micro-
tion of MOCP nanorods. In fact, 1D ribbon-like crystalline structures spheres have been obtained. Mixed lanthanide coordination
of Eu(BTC)·6H2 O influence the production of 1D nanostructures compound microspheres were used to produce La–Ce oxide, Eu3+ ,
(Fig. 27A). After calcination, the surface of Eu2 O3 nanorods becomes Tb3+ doped La2 O3 as well as transition metal doped lanthanide
rough due to release of the CO2 gas generated in the process oxides (Co3+ , Ni2+ doped CeO2 ) microspheres [291]. In all the above
of decarboxylation (Fig. 27E). Luminescence spectra of the Eu2 O3 cases the final products have the same morphology as the precur-
nanorods show the strongest emission peak at 610 nm [289]. sors.
Hollow Gd2 O3 , Eu2 O3 and Y2 O3 microspheres were obtained By thermal decomposition of monolithic macroporous foams of
by using an etching process from silica@Gd2 O3 , Eu2 O3 and lanthanide–organic coordination polymers (lanthanide ions = La-,
Y2 O3 core/shell microspheres, respectively, which are them- Ce-, Pr-, Nd-, Sm-, Eu and ligand = L-asparagine) as precursors, hier-
selves prepared by calcination of silica@coordination polymer archically meso-macroporous or macroporous monolithic foams
core/shell precursors (Fig. 22) [290]. Silica@coordination poly- of lanthanide oxides (La2 O3 , CeO2 , Pr6 O11 , Nd2 O3 , Sm2 O3 and
mer core/shell microspheres precursors have been prepared by Eu2 O3 ) were obtained [292]. For La2 O3 , CeO2 and Pr6 O11 foams,
a mixture of Ln(NO3 )3 (Ln = Gd3+ , Eu3+ , Y3+ ) and isophthalic acid the macropore walls are composed of crystal flakes, aggrega-
using a solvothermal method. Through manipulation of the relative tion of nano-crystals and meshwork of crystal Pr6 O11 nanorods
Fig. 24. Representative TEM and HRTEM images of (A and B) La2 O3 foam, (C and D) CeO2 foam and (E and F) Pr6 O11 foam [292].
respectively (Fig. 24), whereas in the case of Sm2 O3 and Eu2 O3 MOF [Gd(H2 O)3 Co(2,3-pydc)3 ] at 400, 700 and 800 ◦ C which leads
foams, irregular macropores with different sizes are observed. to the production of GdCoO3 mixed-metal oxides with particle
Mixed-lanthanide oxides and lanthanide transition metal oxides sizes of 3 ± 2, 12 ± 3, and 200 ± 20 nm, respectively (Fig. 25) [310].
can be obtained by using doped lanthanide coordination polymer Studies indicate that the photocatalytic decomposition of organic
foams [292]. dyes, phenol, and substituted phenols as model pollutant with 3 nm
Binary, ternary and quaternary metal oxide nanoparticles GdCoO3 is more efficient than the Degussa P-25 catalyst.
[41,293–297] offer a wide variety of important physical properties, In another example, Perovskite-type oxide, LaFeO3 , is synthe-
including magnetism [298], catalysis [299,300], superconductiv- sized by thermolysis of MOCP, La[Fe(CN)6 ]·nH2 O, in which LaFeO3
ity [301], ferroelectricity [302], nonlinear optical behavior [303], has high porosity with highly ordered submicrometer-sized pores
photocatalysts [304,305], ionic conductivity [306], and also appli- with diameters of 100–200 nm [311]. Similar to the cases that were
cations as in electrode materials, sensors [307,308] and fuel cells mentioned before, during thermal decomposition, the crystal shape
[309]. However, it is likely that control of the stoichiometry and size of precursor was maintained, even though the decomposition tem-
of the mixed-metal oxides could cause significant problems for the perature was 1000 ◦ C.
successful synthesis of such nanostructures. Calcination of CoFe Prussian blue analog–silica nanocomposites
As seen above, using MOCPs precursor is a simple way to synthe- at 700 ◦ C tends to give a homogeneous nanocomposite contain-
size mixed-metal oxides. Another typical example of application ing isolated nanoparticles of a mixed-metal oxide CoFe2 O4 with an
of MOCPs for preparing mixed-metal oxides is the calcination of average diameter of 3.8 nm [312].
Fig. 25. TEM images of GdCoO3 formed by calcination of [Gd(H2 O)3 Co(2,3-pydc)3 ] at three different temperatures: (A) 400, inset shows SAED pattern, (B) 700, and (C) 800 ◦ C
[310].
4. Nano metal sulfides final products. In another case a PbS nanoparticle/layered polymer
composite was generated by exposing the poly(lead methacry-
Sulfides are a large class of solid compounds, which are late) layers – which contain 2D layered [Pb(C4 H5 O2 )2 ·H2 O] (lead
not as widely studied as oxides [313]. Metal sulfides with methacrylate) networks – to H2 S gas at room temperature. The
novel micro and nano structures exhibit higher performance average size of PbS nanoparticles is about 6 nm (Fig. 27) [322].
compared with ordinary derivatives. Therefore, many different Different morphologies of Bi2 S3 were obtained using
approaches have been developed for the synthesis of metal three different MOCPs, Bi(S2 COEt)3 , Bi(S2 COiPr)3 and
sulfides [314–319]. Bi(S2 CN(CH2 )4 )2 Cl·CHCl3 as precursors. Short nanorods, nano-
By thermal decomposition of nano 2D-MOCP precursors, fibers and nanorods of Bi2 S3 were obtained from solution decom-
[Pb(2-pyc)(NCS)]n and [Pb(3-pyc)(NCS)]n at 400 ◦ C, nanorods and position method using the above MOCPs, respectively (Fig. 28A–C)
nano-plates of PbS were obtained (Fig. 26) [320]. The sizes and [323]. Also Bi2 S3 thin films with needle-shaped nanorods, micro-
shapes of the nanostructures are related to the structure of the sized particles and again nanorods morphology were obtained from
coordination polymers and different frameworks leading to dif- chemical vapor deposition (CVD), using Bi(S2 COEt)3 , Bi(S2 COiPr)3
ferent morphologies of PbS. Application of the same procedure on and Bi(S2 CN(CH2 )4 )2 Cl·CHCl3 as precursors (Fig. 28D–F) [323].
the precursor [Pb(L4)(␮1,1 -NCS)(H2 O)]n has led to the formation In other cases, different types of Bi2 S3 nanorods were produced
mixture of PbS and Pb2 (SO4 )O nanoparticle [321]. This reveals that from MOCP precursors, [Bi6 (2,6-pydc)8 (2,6-pydcH)2 (tu)8 ] and
the composition or crystal packing of MOCP may lead to different {[Bi2 (2,6-pydc)3 (tsc)(H2 O)2 ]·3H2 O}n using different reaction
Fig. 26. A fragment of the two-dimensional polymer (A) in compound [Pb(2-pyc)(NCS)]n and (B) in compound [Pb(3-pyc)(NCS)]n . SEM images of (C) PbS nanorods produced
by calcination of [Pb(2-pyc)(NCS)]n and (D) PbS nanoplate produced by calcination of [Pb(3-pyc)(NCS)]n [320].
methods, which include solution decomposition, hydrothermal

and solvothermal decomposition, under different conditions
(solvent, temperature and surfactant) (Fig. 29) [324]. The mech-
anism of formation for nanorods may be explained by extrinsic
and intrinsic factors. Formation of 1D nanostructures of Bi2 S3 in
anisotropic growth along the c axis may be caused by strong cova-
lent bonds along the c crystallographic axis and much weaker van
der Waals bonding between the chains of the layered structures
of MOCPs. This intrinsic factor combined with extrinsic factor of
capping ability of surfactants leads to formation of Bi2 S3 nanorods.
Apparently, 1-dodecanethiol (DT) and 1-octadecanethiol (OT) play
a major role in formation of nanorods due to the strong capping
ability of thiol groups associated with Bi(III). The differences in
affinity of the surfactants affect growth of Bi2 S3 nanoparticles and
produce various morphologies for the nanoparticles obtained by
various synthetic routes [324]. It is believed that rod-like Bi2 S3
nanostructures are formed through decomposition of precursors
and formation of initial Bi2 S3 nuclei. In this procedure, Ostwald-
type ripening and crystal splitting processes allow formation of
nanorods of various morphologies.
By hydrothermal reaction using MOCP precursors
{[Cu(HSglu)(H2 O)]·H2 O}n [325] and [Cu3 (HSser)3 (H2 O)2 ]·2H2 O
[326], and the sulfonating reagent, thiourea, CuS hierarchical 3D
flowerlike nanostructure and hollow nano-spheres were achieved
(Fig. 30). The effect of time and molar ratio have been monitored
that show the CuS 3D flower-like mesostructure is an assembly
of many plate-like petals (Fig. 31) and the CuS hollow spheres
were self-assembled of nanorod/plate particles with a shell of
thickness 70 ± 7 nm. The formation of hollow materials seems
to support the argument that the hollow trait in the CuS may
have resulted from the angular arrangement of Cu(II) atoms and
ligands in the crystal lattice (Fig. 32) [326]. In the former precursor
cubic phase of Cu2 S, digenite, in addition to CuS, was observed
by changing the molar ratio of precursor to thiourea, at 1:10
molar ratio. This might be due to the partial reduction of Cu2+
to Cu+ during the reaction carried out at a high concentration of
thiourea [325].
In another case, from nanowire precursors, [Cu(tu)]Cl·1/2H2 O,
Fig. 27. (A) Synthetic pathway for the preparation of PbS nanoparticles/layered
polymer composite materials and (B) TEM image of PbS nanoparticles/layered poly- porous CuS nanotubes were obtained which are composed of small
mer composite materials [322]. nanocrystals (Fig. 33) [327]. The architecture of the nanowire
Reproduced with permission of Springer-Verlag GmbH.
Fig. 28. SEM images of the Bi2 S3 nanoparticles prepared by solution decomposition method using precursors (A) Bi(S2 COEt)3 , (B) Bi(S2 COiPr)3 and
(C) Bi(S2 CN(CH2 )4 )2 Cl·CHCl3 ; SEM images of Bi2 S3 thin films generated by CVD using precursors (D) Bi(S2 COEt)3 , (E) Bi(S2 COiPr)3 , (F) Bi(S2 CN(CH2 )4 )2 Cl·CHCl3 [323].
Fig. 29. BF-TEM images of the Bi2 S3 particles obtained by decomposition of [Bi6 (2,6-pydc)8 (2,6-pydcH)2 (tu)8 ] in anisole in the presence of DT (A1–A4) and OA (B1–B4): after
4 min, 10 min, 1 h, and 16 h, respectively. The scale bar is 50 nm in all cases. (C) Fragment of the polymeric chain in {[Bi2 (2,6-pydc)3 (tsc)(H2 O)2 ]·3H2 O}n [324].
Fig. 30. (A and B) FE-SEM and TEM images of CuS produced using {[Cu(HSglu)(H2 O)]·H2 O}n as precursor and (C and D) FE-SEM and TEM images of CuS produced using
[Cu3 (HSser)3 (H2 O)2 ]·2H2 O as precursor [325,326].
Fig. 31. Probable formation mechanism for the CuS nanostructure prepared by hydrothermal reaction using MOCP, {[Cu(HSglu)(H2 O)]·H2 O}n [325].
precursors can influence the morphology of CuS nanotubes. As in

Fig. 33A–C, when a highly dispersed dandelion-like nanowire pre-
cursor is used, the CuS product comprises regular round porous
nanotubes. However its thorn-like counterpart forms a porous
nanotube structure, in which due to close packing architectural
structure of the nanowires, three or more of these tubes are fused
together as a single pillar (Fig. 33D–F) [327].
Cu2 S nanocrystals and mixture of copper sulfides, CuS and
Cu9 S5 in the shape of triangular nanoplates were prepared by ther-
mal decomposition of Cu(ODTP)2 and Cu(DdDTP)2 , respectively
[328]. The average particle size and side length of these nanocrys-
tals and triangular nanoplates are 9.8 ± 0.3 nm and 12.3 ± 0.6 nm,
Fig. 33. (A) Growth mechanism of the hierarchical nanotubular structures from
steps 1–3 using dandelion-like [Cu(tu)]Cl·1/2H2 O nanowires. (B) Dandelion-like
architecture of MOCP precursor. (C) CuS nanotubes prepared from dandelion-like
Fig. 32. Schematic representation of the packing structure of architecture. (D) Growth mechanism for thorn-like [Cu(tu)]Cl·1/2H2 O nanowires.
[Cu3 (HSser)3 (H2 O)2 ]·2H2 O, (B) the magnified portion of the part highlighted (E) Thorn-like architecture of MOCP precursor. (F) CuS nanotubes prepared from
in image (A); where the ligands in plane are represented as red and the ligand in a thorn-like architecture [327].
folded way is represented as blue and (C) orange and purple bonds are the bonds
connecting the trinuclear units and the ligands are omitted for clarity [326].
Fig. 34. TEM images and SAED patterns of copper sulfide nanocrystals (A) synthesized with Cu(ODTP)2 and (B) synthesized with Cu(DdDTP)2 at 140 ◦ C for 5 h [328].
Fig. 35. (A and B) TEM images of the synthesized chain-like superstructures composed of Ag2 S nanoparticles using Ag(I)-cysteine nanofibers as templates [329].
Fig. 36. A fragment of the two-dimensional polymer in (A) MOCP [Pb(␮-bpp)(␮-Br)2 ]n , (B) MOCP [Pb(␮-pyr)(␮-I)2 ]n and SEM images of (C) [Pb(␮-bpp)(␮-Br)2 ]n nanoparticles,
(D) PbBr2 nanoparticles prepared by calcination of nano-sized [Pb(␮-bpp)(␮-Br)2 ]n , (E) [Pb(␮-pyr)(␮-I)2 ]n nanoparticles and (F) PbI2 nanoparticles prepared by calcination
of nano-sized [Pb(␮-pyr)(␮-I)2 ]n [158,159].
respectively, where in the latter, six-leave flower-like clusters are Zn2 SiO4 :xTb3+ submicrometer phosphors containing different
partially observable (signed with white circles in Fig. 34B) [328]. amounts of Tb have been obtained through calcination of in situ
The effect of various reaction conditions (temperature and con- generated [Zn2−x Tbx (sal)2 ]n coordination polymer at 900 ◦ C. The
centration) on the copper sulfide nanocrystals size and shape has particle sizes range from 50 to 200 nm and the submicrometer
also been investigated. Triangular particles are generally difficult Zn2 SiO4 :Tb3+ phosphors exhibit a strong characteristic green fluo-
to obtain due to their higher energies, compared to spherical rescence of Tb3+ ions at 542 nm [337].
particles.
By exposing the Ag(I)–cysteine nanofibers to electro-radiation 6. Conclusions
in TEM, semiconductor silver sulfide nanoparticles have been
formed with the same shape as these templates [329]. The resulting Coordination polymers may be suitable precursors for the
nanoparticle superstructures appear in chains composed of indi- preparation of desirable nanoscale materials. Use of MOCPs as
vidual Ag2 S nanoparticles in the acanthite phase with diameters precursors for preparation of inorganic nano-materials such as
between 4 and 9 nm (Fig. 35). metal oxides is a method with interesting advantages. Some of
ZnS nanoparticles were prepared from three MOCP pre- these advantages are simplicity of processing and forgoing the
cursors, [Zn(␮-3-bpdh)2 (NCS)2 ]n [223], [Zn(FCA)2 ]n [330] and need for special instruments; relationship between structures of
[Zn(BDC)(4,4 -bipy)]n [331] via three preparation methods the target products and raw materials; being more appropriate for
(thermolysis, ionic liquid-assisted templating and solvothermal phase control of products; better control over process conditions,
method) and nanoparticles, spherical nanocrystals and nanorods particle size, particle crystal structure, and purity; reducing the
of ZnS were obtained, respectively. chance of interparticle collisions; simplicity, cost effectiveness and
By using MOCP precursor [Cd(BDC)(4,4 -bipy)]n , via solvother- the potential for large-scale fabrication. In addition, through pres-
mal method, CdS nanorods and spherical nanoparticles have been ence of capping ligand, the undesired aggregation of nanoproducts
obtained when sulfur sources of thiourea and Na2 S2 O3 were used, will be hindered. Another important advantage of this method is
respectively [331]. that elemental components can be controlled as desired which is
Decomposition of compounds [Cd(Hsal)2 (tu)2 ], accomplished by mixing the selected metal ions and the appropri-
[Cd(pic)2 (tu)2 ]·0.5H2 O, [Cd(pic)2 (ths)2 ]·2H2 O, [Cd(2,6-pydc)(tu)2 ] ate organic bridging ligands. Also one of the unique features of this
and [Cd(2,6-pydc)(ths)2 (H2 O)]·2H2 O under different conditions method is formation of nano-materials that could not be obtained
using different surfactants has led to the formation of CdS by other methods. For instance, Cd3 OSO4 nanostructure may only
nanostructures in various morphologies including gypsum rose, be produced via this method. However, the process entails compli-
spherical particles, ellipsoidal particles and nanorods [332]. The cated steps involving preparation of polymer-based precursors.
best rod-like CdS nanocrystals were obtained via decomposition Most likely the mechanism of final morphology formation in
in a mixture of ethylenediamine and hexadecylamine at 175 ◦ C for nano-materials depends on various intermediates controlled by
2 h [332]. inner and external forces during the formation process. Crystal
structure and the interactions in MOCP (such as covalence, coor-
5. Other nano-materials dination, hydrogen, and van der Waals forces) are inner forces
affecting intermediates and solvent–MOCP interactions, electro-
Under some conditions (e.g. different temperatures or atmo- static and dipolar fields as well as hydrophilic or hydrophobic
spheres) the thermal decomposition of metal–organic coordination interaction give rise to external forces controlling system morphol-
polymers can lead to the preparation of nano-materials such as ogy [324–326,331].
metal halides, metal hydroxides, etc. Therefore, it is concluded that size and morphologies of
Thermal decomposition of four nano MOCPs, inorganic nano-materials are dependent on several parameters:
[Pb(4-pyc)(Br)(H2 O)]n [333], [Pb(3-pyc)Br]n [334], [Pb(␮- (a) relationship between MOCP crystalline structure and mor-
HPDC)(␮-Br)(H2 O)]n [335] and [Pb2 (2-pyc)2 (Br)2 ] [155], leads phology of desired materials [135,231,247,324–326,328,331],
to the formation of PbBr(OH) nanostructures with nanoparti- (b) influence of initial morphology of the MOCP precur-
cle and nanorod morphology. However through calcination of sors [60,135,148,159,228,234,283,327,338], (c) preparation
the nanostructure compound [Pb(␮-4-pyc)(␮-NCS)(␮-H2 O)]n , method [117,247,323,329,339,340], (d) thermolysis temperature
Pb2 (SO4 )O nanoparticles are produced [145]. [238,310,311,341,342], (e) effects of surfactant [111–114,147,238]
PbBr2 and PbI2 nanoparticles were obtained by thermal decom- and (f) size of initial MOCP precursors [321].
position of nano-sized 2D-MOCPs, [Pb(␮-bpp)(␮-Br)2 ]n [158] and Finally, finding the precise and clear-cut mechanisms for
[Pb(␮-pyr)(␮-I)2 ]n [159] under an argon atmosphere. Recall that transformation of MOCPs to desired nano-materials is the main
calcination of these compounds under air leads to the formation challenge in this field. So, the future research should focus on
of PbO nano-powder. The morphology of the PbBr2 nanoparticles description and explanation of nano-material formation mecha-
(Fig. 36C) and PbO is very similar to that of compound [Pb(␮- nisms and finding rules that govern the relation between influential
bpp)(␮-Br)2 ]n (Fig. 36B). This may be due to direct removal of the factors and final morphologies. This might be accomplished
bpp ligand without altering the morphology under calcination in through purposeful utilization of various MOCPs with different
argon and air atmospheres. The same point has also been observed compositions and structural varieties–i.e. 1D, 2D, 3D as well as
in PbI2 and its precursor (Fig. 36E and F). porous and nonporous structures.
The same thing happens when nano-MOCP, {[Bi(␮-4,4 -
bipy)Br4 ]·(4,4 -Hbipy)}n [164] is calcined under an argon atmo- Acknowledgment
sphere which results in formation of BiBr3 nano-powder,
instead of Bi2 O3 nanoparticles that were obtained under an air This work was supported by Tarbiat Modares University.
atmosphere.
In another example a 3D-MOCP precursor, {[Cd3 (3- References
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Applications of Metal-Organic Coordination Polymers As Precursors For Preparation of Nano-Materials

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Coordination Chemistry Reviews 256 (2012) 2921–2943

Contents lists available at SciVerse ScienceDirect

Coordination Chemistry Reviews

Applications of metal–organic coordination polymers as precursors

1. Introduction materials ﬁnd very diverse potential applications including cataly-

Metal nanoparticles are important for technological applica-

Aggregated nanoparticles of Bi2 O3 have been obtained from

display higher catalytic activity for CO oxidation than conventional

3.2. Transition metal oxides

Manganese is a transition metal whose oxides are important for

methods, which include solution decomposition, hydrothermal

precursors can inﬂuence the morphology of CuS nanotubes. As in

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