Geckeler K.E., Nishide H. (Eds.) Advanced Nanomaterials

6.6 Pnictide Nanotubes 235

micelles [179] , boehmite nanotubes by a hydrothermal procedure [180] , and

hydroxyapatite nanotubes by a sol – gel procedure in an AM [181] .

La

0.5

Sr

0.5

CoO

3

nanotubes have been prepared using an AM template by the

sol – gel method [182] , while ZnAl

2

O

4

spinel nanotubes have been obtained by

making use of the Kirkendall effect [183] . ZrCr

2

O

4

has also been prepared by this

method [117] . Nanotubes of SrAl

2

O

4

[184] , as well as AgIn(WO

4

)

2

[185] , are

produced under hydrothermal conditions. By controlling the pH, single - walled

aluminogermanate nanotubes have been synthesized by the reaction of tetraethy-

lorthogermanate and AlCl

3

in NaOH solution [186] . Nickel hexacyanoferrate nano-

tubes have been fabricated in an AM using the electrokinetic method [187] .

Single - crystal calcium sulfate nanotubes can be generated by the reverse micelle

method at room temperature [188] . Self - assembled supramolecular C

32

H

70

N

2

ZnSO

4

nanotubes with high thermal stability have been prepared [189] . Bismuth subcar-

bonate nanotubes are prepared by a simple reﬂ ux of bismuth citrate and urea in

ethylene glycol [190] .

6.6

Pnictide Nanotubes

Several methods to synthesize BN nanotubes including CVD and electrical dis-

charge, as well as templating have been described in the literature [4] . Thin BN

tubes of less than 200 nm diameter were ﬁ rst obtained by arc discharge with hollow

tungsten electrodes ﬁ lled with h - BN powder. Following this initial report, a variety

of methods have been employed to prepare BN nanotubes. The other methods of

synthesis of BN nanotubes include those that are far from equilibrium, such as

the electrical arc method [191, 192] , arcing between h - BN and Ta rods in a N

2

atmosphere [193] , laser ablation of h - BN [194] , and continuous laser heating of BN

[195] . The last method produces long ropes of BN nanotubes with thin walls.

Single - walled BN nanotubes are formed in some cases [191, 196] . Single - walled

nanotubes of BN have been deposited on polycrystalline W substrates by using

electron - cyclotron resonance nitrogen and electron beam boron sources [197] .

Bando and coworkers [198, 199] , have carried out extensive work on BN nano-

tubes. They prepared the nanotubes by the reaction of MgO and B in the presence

of ammonia at 1300 ° C [198] . B

2

O

2

(obtained by heating B and MgO at 1300 ° C)

was heated in the presence of NH

3

in a long BN boat, which was placed into a

graphite susceptor that was heated from the outside by an RF furnace to obtain

BN nanotubes. The BN nanotubes exhibit a 1D nanostructure and have diameters

that range from several nanometers to about 70 nm, and lengths that go up to 10

micrometers. They show the presence of mixed hexagonal and rhombohedral BN

phases. The nanotubes of diameter around 10 nm exhibit a perfectly cylindrical

structure, although edge dislocations are occasionally observed from the rhombo-

hedrally stacking, ordered nanotubes. The concentric tube structures do not

contain internal wall closures or internal cap structures. Bando and coworkers

[199] , have also prepared BN nanotubes by the reaction of MgO, FeO, and B in

the presence of NH

3

at 1400 ° C. The nanotubes are in the pure h - BN phase and

236 6 Synthesis of Inorganic Nanotubes

have diameters of ∼ 50 nm and lengths of up to several tens of micrometers. The

reaction of boric acid or B

2

O

3

with N

2

or NH

3

at high temperatures in the presence

of carbon or catalytic metal particles has also been employed in the preparation of

BN nanotubes [200] . BN nanotubes can be grown directly on substrates at 873 K

by a plasma - enhanced laser - deposition technique [201] .

B

2

O

3

- coated multi - walled carbon nanotubes, on reaction with NH

3

at high tem-

peratures, yield BN nanotubes [202] . Bando and coworkers have reviewed various

aspects of BN nanotubes and cite methods involving arc - discharge, laser ablation,

and the plasma jet method (Fig. 6.19 ) [203] . Straight BN nanotubes have been

grown by heating a mixture of Mg(BO

2

)

2

· H

2

O, NH

4

Cl, NaN

3

, and Mg powder in

an autoclave at 600 ° C for 20 – 60 h. These BN nanotubes had diameters mainly in

the range of 30 – 300 nm and lengths of up to ∼ 5 μ m, and a majority of them had

at least one closed end [204] . Multi - walled BN nanotubes have been obtained by a

reduction – nitridation route wherein the reaction of boron triﬂ uoride etherate and

sodium azide was carried out in the presence of Fe – Ni powder in a sealed autoclave

at 600 ° C for 12 h. The BN nanotubes so obtained have an average outer diameter

of 60 nm, an inner diameter of 30 nm, and lengths up to 300 nm [205] . By anneal-

ing an Fe ﬁ lm evaporated on boron pellets at 1000 ° C in N

2

gives rise to BN nano-

tubes [206] . Microwave plasma - enhanced CVD has been employed to obtain BN

nanotube arrays [207] . In this method, AM are used (for conﬁ nement) along with

borane and ammonia or nitrogen. BN nanotubes that are 1 mm long are obtained

by an optimized ball - milling and annealing method [208] . The annealing tempera-

Figure 6.19 a,b) HRTEM images of two

zig - zag BN MWNTs. A different stacking

order is apparent in the marked areas in

(a) and (b), as highlighted in the insets.

Hexagonal - (a) and rhombohedral - type

(b) stacking (in 12.5 ° fringe inclinations with

respect to the tube axis) are veriﬁ ed by the

corresponding computer - simulated HRTEM

images (c and d, respectively) for BN MWNTs

having the axes strictly parallel to the [10 – 10]

orientations ( “ zig - zag ” NTs). Note a

characteristically open tip - end of a BNNT in

(b). This feature is frequently seen in BNNTs

obtained from high - temperature chemical

syntheses. Reproduced with permission from

6.6 Pnictide Nanotubes 237

ture of 1100 ° C is crucial for the growth of the long BN nanotubes because at this

temperature there is a fast nitrogen dissolution rate in Fe and the B/N ratio in Fe

is 1.

By combining polymer thermolysis and the use of templates, ordered arrays of

BN nanotubes have been obtained [209] . In this method, liquid borazine in AM is

thermolyzed at high temperatures in a nitrogen atmosphere. Double - walled BN

nanotubes are obtained by the reaction of a ﬂ owing stream of borazine and

ammonia with a nickelocene catalyst vapor in the hot zone of a furnace maintained

at 1200 ° C [210] . The mechanism of growth of single - walled BN nanotubes by laser

vaporization has been examined in detail [211] . It appears that the root - growth

model that involves a droplet of B is applicable for this growth. It may be noted

that laser vaporization is a unique route for the synthesis of single - walled BN

nanotubes.

Single - walled BCN nanotubes are obtained by bias - assisted hot - ﬁ lament CVD

[212] . In this method, a Fe – Mo catalyst supported on MgO powder is used for the

decomposition of a mixture of CH

4

, B

2

H

6

, and ethylenediamine. The as - grown

SWNTs have clean and smooth surfaces with diameters in the range of 0.8 – 2.5 nm

and lengths up to micrometers. Homogeneous BC

4

N nanotube brushes have been

obtained recently by the reaction of amorphous carbon nanotubes with boric acid

and urea (Fig. 6.20 ) [213] . The BCN nanotubes have open ends with a diameter of

170 nm, a length of 15 mm, and thickness of around 50 nm. The SAED pattern

shows faint rings and a few spots. The X - ray diffraction (XRD) pattern of the BCN

nanotube brushes shows broad reﬂ ections with d - spacings of 3.43 Å and 2.13 Å ,

which correspond to the (002) and (100) planes, respectively, similar to the pattern

reported for BC

3

N. The broad reﬂ ections in the XRD pattern and the diffuse rings

in the electron diffraction pattern suggest the turbo static nature of the

nanotubes.

GaN nanotubes have been grown in AMs by employing MOCVD. The reac-

tants used are trimethylgallium and NH

3

[214] . The diameter of the GaN

nanotubes is approximately 200 – 250 nm and the wall thickness is about 40 – 50 nm.

Nanotubular GaN consists of numerous ﬁ ne GaN particulates with a size

range of 15 – 30 nm. XRD and TEM analyses indicate that the grains in the

GaN nanotubular material is nanocrystalline with a hexagonal structure. By

the reaction of GaCl

3

with excess NaN

3

in dry benzene, GaN nanotubes with

branched tubules have been grown in mesoporous MCM 48 [215] . These GaN

nanotubes are polycrystalline with a wurtzite structure and an outer diameter

of 50 – 150 nm. The tube wall thickness is ∼ 10 nm and the lengths go up to

several micrometers. Amorphous carbon nanotube brushes, on reaction with

GaCl

3

followed by reaction with NH

3

, give rise to GaN nanotube brushes (Fig.

6.21 ) [216] . The close packing of 1D GaN nanotube - nanobristles have diameters

from 100 to 230 nm and lengths in the 7 – 10 μ m range. The tubes are open

at one end and their surface appears to be smooth. The nanotube brushes

have a wurtzite structure. The TEM images in Figures 6.21 c – e shows a nano-

tube with an outer diameter of 200 nm and the wall thickness is in the range

of 10 – 15 nm. The HRTEM image of the nanotube wall in Figure 6.21 f shows

238 6 Synthesis of Inorganic Nanotubes

interplanar spacing of 0.244 nm, which indicates the single crystalline nature

of the GaN nanotube.

Si

3

N

4

nanotubes can be prepared by the sol – gel route in which tetraethoxysilane

(TEOS) and phenolic resin are used to prepare a carbonaceous silica xerogel, and

ferric nitrate is employed as an additive. The xero - gel is heated at 1300 ° C for 10 h

in nitrogen [217] . Molybdenum nitride nanotubes have been obtained by deposit-

ing a nitride ﬁ lm on anodic alumina and etching away the template with NaOH

[218] .

Single crystalline nanotubes of Cd

3

P

2

and Zn

3

P

2

have been obtained by a tem-

plate process in which Cd and Zn nanorods formed in - situ act as self - sacriﬁ cing

templates [219] . A mixture of reactants that contain CdS (or ZnS), P, and Mn

3

P

2

is heated to 1350 ° C in an induction furnace to obtain nanotubes. Single - crystal-

line, single - walled, SbPS

4 −

x

Se nanotubes with a tunable band - gap have been pre-

pared by taking a mixture of stoichiometric amounts of the elements Sb, P, S, for

SbPS

4

, and the corresponding amounts for SbPS

3

Se, SbPS

2

Se

2

, and SbPSSe

3

in

fused silica tubes sealed under vacuum, and heated [220] .

Figure 6.20 a) FESEM images of BCN

nanotube brushes with the average diameter

of a single tube being around 170 nm. The

inset shows a FESEM image of BCN nanotube

brushes of 40 nm diameter. b) Higher

magniﬁ cation FESEM images of BCN

nanotube brushes. TEM images of a BCN

nanotube: c) 170 nm diameter and d) 40 nm

diameter. e) Elemental mapping of the boron,

carbon, and nitrogen of BCN nanotubes

obtained from EELS. Reproduced with

6.6 Pnictide Nanotubes 239

Figure 6.21 a) Schematic showing the formation of nanotube

brushes of carbon, Ga

2

O

3

, and GaN. b) SEM image of a GaN

nanotube brush. c – e) TEM images of GaN nanotubes and

f) HRTEM image of the wall of a GaN nanotube. Reproduced

240 6 Synthesis of Inorganic Nanotubes

6.7

Nanotubes of Carbides and other Materials

SiC nanowires, SiC/SiO

2

core – shell nanocables, and SiC nanotubes have been

synthesized simultaneously by directly heating Si powder and multiwall carbon

nanotubes (MWCNTs) [221] . Single - phase TiC nanotubes are prepared by the

reaction of carbon nanotubes with Ti powder at 1300 ° C for 30 h [222] .

Silicon oxycarbide ceramic nanotubes can be obtained by the pyrolysis of poly-

silicone nanotubes using a sacriﬁ cial AM as a template [223] . In a typical synthesis,

the AM templates were immersed in a mixture of low - molecular - weight silicone

starting materials, such as {CH

3

(CH = CH)SiO}

n

( n = 3 – 7), named VC4, and a

cyclic - type silicone bearing vinyl groups, and (CH

3

)

3

SiO{CH

3

(H)SiO}

m

( m = 20),

named KF - 99 and heated in an oven at two different temperatures, 50 and 200 ° C.

Large - scale aligned silicon carbonitride nanotube arrays have been synthesized by

microwave - plasma - assisted CVD using SiH

4

, CH

4

, and N

2

as precursors. The

nanotubes are 6 – 7 μ m in length and 100 – 200 nm in diameter [224] .

Transition metal halides such as NiCl

2

crystallize in the CdCl

2

structure, with

the metal halide layers held together by weak van der Waals forces. NiCl

2

has been

shown to form closed cage structures and nanotubes [225] . These were prepared

by heating NiCl

2

· 6H

2

O initially in air to remove the water of crystallization, and

heated further at 960 ° C under Ar. Zeng et al. [226] . have carried out UV -

light - induced fabrication of CdCl

2

nanotubes starting from CdSe solid nanocrys-

tals through a Kirkendall effect. In this procedure, CdCl

2

nanotubes are obtained

starting with a solution of CdSe nanocrystals in o - dichlorobenzene (which gener-

ates chlorine free radicals on photolysis).

6.8

Complex Inorganic Nanostructures Based on Nanotubes

In addition to the simple nanotube structures, more complex nanotubular

structures of various inorganic materials such as coaxial cables, heterojunc-

tions, and nanotube - nanowire or nanotube - nanoparticle composites have been

prepared and characterized by several workers. Typical examples of such nanos-

tructures are the following: Integration of ZnO nanotubes with ordered nano-

rods [227] , conversion of ZnO nanorod arrays into ZnO – ZnS nanocable and

ZnS nanotube arrays [228] , core – sheath heterostructure CdS – TiO

2

nanotube

arrays [229] , ZnS nanotube – In nanowire core – shell heterostructures [230] ,

ZnO – ZnS core – shall nanotube arrays [231] , Cu nanotube – Bi nanowire hetero-

junctions [232] , carbon nanotubes in TiO

2

nanotubes [233] , TiO

2

– Pt coaxial

nanotube arrays [234] , Sn nanowires on TiO

2

nanotubes [235] , Fe

2

O

3

– TiO

2

nanorod – nanotube arrays [236] , SiO

2

– Ta

2

O

5

core – shell nanowires and nanotubes

[237] , multi - walled BCN – carbon nanotube junctions [238] , and BN nanotubes

with periodic iron nanoparticles [239] .

References 241

6.9

Outlook

The preceding presentation should sufﬁ ce to demonstrate the great progress made

in the synthesis of inorganic nanotubes. It would appear that today we are able to

synthesize almost any inorganic material in tubular form. Not only do we have an

arsenal of inorganic nanotubes but also several strategies to synthesize them.

There are still many synthetic challenges. One of them relates to the need to syn-

thesize single - walled single - crystalline nanotubes of inorganic materials. There are

hardly one or two reports of single - walled inorganic nanotubes at present. With

the availability of inorganic nanotubes in sufﬁ cient quantities, there is much scope

to measure their properties and investigate phenomina associated with them.

This Chapter has been published previously online in

Advanced Materials 3 Aug 2009

Doi: 10.1002/adma.200803720

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