Recent Patents On Engineering

Recent Patents on Engineering (2008), 2, 157-164
157
1872-2121/08 $100.00+.00 © 2008 Bentham Science Publishers Ltd.
Doped-TiO
: A Review
Adriana Zaleska*
Department of Chemical Technology, Gdansk University of Technology, 80-952-Gdansk, Poland
Received: May 28, 2008; Accepted: June 16, 2008; Revised: June 17, 2008
Abstract:
Titanium dioxide represents an effective photocatalyst for water and air purification and for self-
cleaning surfaces. Additionally, it can be used as antibacterial agent because of strong oxidation
activity and superhydrophilicity. TiO2 shows relatively high reactivity and chemical stability under
ultraviolet light (<387nm), whose energy exceeds the band gap of 3.3 eV in the anatase crystalline
phase. The development of photocatalysts exhibiting high reactivity under visible light (
> 400 nm) should allow the main part of the solar spectrum, even under poor illumination of
interior lighting, to be used. Visible light-activated TiO
could be prepared by metal-ion implantation, reducing of TiO
, non-metal doping or sensitizing of TiO
with dyes. This paper reviews preparation methods of doped-TiO

2
with metallic and nonmetallic species, including various types of dopants and doping methods
currently available. The mechanism of heterogeneous photocatalysis in the presence of TiO
is also discussed.
Keywords:
Doped-TiO
, metal-doping, monmetal-doping, TiO
preparation methods, heterogeneous photocatalysis.
1. INTRODUCTION
Strong oxidation and reduction power of photoexcited titanium dioxide (TiO
) was realized from the discovery of Honda-Fujishima effect. In 1972, Fujishima
et al
. [1] reported photoinduced decomposition of water on TiO
electrodes. Since Frank and Bard [2] first examined the possibilities of using TiO
to decompose cyanide in water, there has been an increasing interest in environmental

applications. Photocatalytic reactions at the surface of titanium dioxide have been attracting much
attention in view of their practical applications to environmental cleaning such as self cleaning of
tiles, glasses, and windows. Titanium dioxide represents an effective photocatalyst for water and
air purification and for self-cleaning surfaces. Additionally, it can be used as antibacterial agent
because of strong oxidation activity and superhydrophilicity [3]. TiO
shows relatively high reactivity and chemical stability under ultraviolet light (
<387nm), whose energy exceeds the band gap of 3.3 eV in the anatase crystalline phase. The
development of photocatalysts exhibiting high reactivity under visible light (
> 400 nm) should allow the main part of the solar spectrum, even under poor illumination of
interior lighting, to be used. Several approaches for TiO
modification have been proposed: metal-ion implanted TiO
(using transition metals: Cu, Co, Ni, Cr, Mn, Mo, Nb, V, Fe, Ru, Au, Ag, Pt) [4-6], reduced TiO
photocatalysts [7-8], non-metal doped-TiO
(N, S, C, B, P, I, F) [9-11], composites of TiO
with semiconductor having lower band gap energy (e.g. Cd-S particles [12], sensitizing of TiO
with dyes (e.g. thionine) [13] and TiO
doped with upconversion luminescence agent [14,15]. In this paper, the recent patents pertaining
to the preparation methods of doped-TiO
with metallic and nonmetallic species, including various types of dopants and doping methods
currently available are presented. The
*Address correspondence to this author at the Department of Chemical Technology, Gdansk

University of Technology, 80-952-Gdansk, Poland; Tel: (++48-58)-347-2437; Fax: (++48-58)-347-
2065; E-mail: azal@chem.pg.gda.pl
mechanism of heterogeneous photocatalysis in the presence of TiO

2
is also discussed.
1.1. Mechanism of Photoactivity of Pure TiO
and TiO
Doped with Metal and Nonmetal Species
The photocatalytic mechanism is initiated by the absorption of the photon
hv
with energy equal to or greater than the band gap of TiO
(~3.3 eV for the anatase phase) producing an electron-hole pair on the surface of TiO
nanoparticle as schematized in Fig. (
). An electron is promoted to the conduction band (CB) while a positive hole is formed in the
valence band (VB). Excited-state electrons and holes can recombine and dissipate the input energy
as heat, get trapped in metastable surface states, or react with electron donors and electron
acceptors adsorbed on the semiconductor surface or within the surrounding electrical double
layer of the charged particles. After reaction with water, these holes can produce hydroxyl radicals
with high redox oxidizing potential. Depending upon the exact conditions, the holes, OH radicals, O
2-
,H
2
and O
itself can play important roles in the photocatalytic reaction mechanism [16-17].
Fig. (1).
Mechanism of TiO
photocatalysis:
hv
: pure TiO
hv
: metal-doped TiO
and
hv
: nonmetal-doped TiO
.
158
Recent Patents on Engineering
2008
, Vol. 2, No. 3 Adriana Zaleska
The visible light photoactivity of metal-doped TiO
can be explained by a new energy level produced in the band gap of TiO
by the dispersion of metal nanoparticles in the TiO

2
matrix. As shown in Fig. (
) electron can be excited from the defect state to the TiO
conduction band by photon with energy equals
hv
. Additional benefit of transition metal doping is the improved trapping of electrons to inhibit
electron-hole recombination during irradiation. Decrease of charge carriers recombination results
in enhanced photo-activity. There are three different main opinions regarding modification
mechanism of TiO
doped with nonmetals. (1) Band gap narrowing; (2) Impurity energy levels; and (3) Oxygen
vacancies. 1.
Band gap narrowing: Asashi,
et al.
[18] found N 2p state hybrids with O 2p states in anatase TiO
doped with nitrogen because their energies are very close, and thus the band gap of N-TiO
is narrowed and able to absorb visible light. 2.
Impurity energy level: Irie,
et al.
[19] stated that TiO

2
oxygen sites substituted by nitrogen atom form isolated impurity energy levels above the valence
band. Irradiation with UV light excites electrons in both the VB and the impurity energy levels, but
illumination with visible light only excites electrons in the impurity energy level. 3.
Oxygen vacancies: Ihara,
et al.
[20] concluded that oxygen-deficient sites formed in the grain boundaries are important to
emerge vis-activity and nitrogen doped in part of oxygen-deficient sites are important as a blocker
for reoxidation. The modification mechanism of anatase doped with nonmetals was also analyzed
by Zhao
et al.
[21]. They investigated N-TiO
and concluded that TiO
doped with substitutional nitrogen has shallow acceptor states above the valence state. In
contrast, TiO
doped with interstitial nitrogen has isolated impurity states in the middle of the band gap. These
impurity energy levels are mainly hybridized by N 2p states and O 2p states.
1.2. Doping Moieties and Preparation Methods
To enhance the photocatalytic effect in the visible light region, many producing methods were
proposed to dope (or incorporate) trace impurity in TiO
including: ion-assisted sputtering, plasma, ion-implantation, chemical vapor deposition (CVD) and
sol-gel. A comprehensive list of doped TiO
and methods of its preparation are shown in Table

1
[22-33]. In 2000, Anpo presented second generation titanium oxide photocatalysts - visible light
response TiO
obtained by an advanced high-voltage metal ion-implantation method [34]. The electronic

properties of TiO
was modified by bombarding them with high energy metal ions. The metal ions (specifically Cr
and V ions) were injected into the deep bulk of the TiO
when high acceleration energy (150-200 keV) was applied, then calcined in oxygen at 450-475
C. Obtained photocatalysts worked effectively in decomposition of NO into N
and O
under visible light (
> 450 nm) [34]. The same method was next successfully used to dope a series of transition metals,
such as V, Cr, Ni, Mn and Fe [35]. The iron-doped-TiO
was prepared by the hydrothermal method [36]. Titanium (IV) tetra-
tert
-butoxide and FeCl
or FeCl
2
dissolved in n-octanol was heated at 230
C for 2h in the presence of water. Resulting powders were rinsed, dried and calcined at 560
C. Photocatalyst doped with FeCl
have better photoactivity for degradation of dye in aqueous solution under UV and visible light. It
was found that the amount of doped iron ions plays a significant role in affecting its photocatalytic
activity [36]. A series of vanadium-doped TiO
photocatalysts were synthesized by two modified sol-gel methods by Wu
et al
. [24]. In the first method, vanadyl acetalacetonate dissolved in n-butanol was mixed with titanium
butoxide dissolved in acetic acid. Hydrolysis was completed by the water generated via the
estrification of acetic acid and butanol, then the solution was dried at 150
C, pulverized and calcined at 400
C. In the second procedure, the solution of vanadium chloride, ethanol and titanium dioxide was
slowly dropped into cooled acidic aqueous solution (0
C). Then, the solution was dried at 110
C, pulverized and calcined. Obtained vanadium-doped TiO
shows a red-shift in the UV-vis spectra and has higher activity in photodegradation of dyes under
visible light than pure TiO
2
[24]. First non-metal doped TiO
was described in 1986 by Sato,
et al.
[37]. They obtained N-TiO
powders from a commercial titanium hydroxide by calcination. The powders showed higher
photocatalytic activity for oxidation of carbon monoxide and ethane than standard TiO
in the visible region (434 nm). But at that time, this result did not attract attention. Only in 2001,
Asashi,
et al
. reported the band-gap narrowing of titanium dioxide by nitrogen doping [18]. They prepared TiO
2-x
films by sputtering the TiO
target in a N
(40%)/Ar gas mixture and by treating anatase powder (ST01, Ishihara Sangyo Kaisha, Japan) in the
NH
(67%)/Ar atmosphere at 600
C for 3 h. Soon after, successfully prepared and exhibiting higher photoactivity under visible light -
N-doped TiO
2
was followed by other nonmetal doped titania photocatalysts such as carbon [38] sulfur [39,40],
boron [32, 41], phosphorus [33, 42], flour [43] and iodine [44]. Titanium dioxide modified with
non-metal atoms was prepared by hydrolysis of titanium precursors in the presence of dopant,
followed by calcination [29-30, 45], gas-phase thin film deposition method [46], oxidative
annealing of TiN, TiS
or TiC pow-ders [27, 28, 47] and atmospheric pressure plasma-enhanced nanoparticles synthesis
(APPENS) [48], see Table
. Concluding, the sol-gel process is one of the versatile methods to prepare nano-size materials.
This technique does not require complicated instruments and provides simple and easy means for
preparing nano-size particles. The incorporation of an active dopant in the sol during the gelation
stage allows the doping elements to have a direct interaction with support, therefore, the material
possesses catalytic or photocatalytic properties. A typical preparation procedure by the sol-gel
method of doped TiO
is shown in Fig. (
). Titanium precursor, such as titanium isoprooxide (TIP), tetrabutyl orthotitanate (TBOT), titanium
tetra-
Doped-TiO
2008
, Vol. 2, No. 3
159
chloride, is mixed with dopant precursor dissolved in alcohol, followed by hydrolysis performed at
the room or elevated temperature. The precipitate is dried usually at temperature range from 80
to 110
C, pulverized to obtain xerogel and calcinated in air at temperature from 200 to 600
C. The following section reviews some of the latest patents in titanium dioxide doping by metallic
and nonmetallic species.
2. RELATED PATENTS OF METAL-DOPED TIO
Oxonica Ltd. is a developer of innovative surface-doped particles of TiO
and ZnO [49]. This invention relates to
Table 1. Doping Moieties and Preparation Methods of Doped-Titanium Dioxide Photocatalysts
Kind of dopant Doped element Preparation method Potential application References
Ag Silver nitrate was mixed with reduction agent (sodium citrate tribasic dihydrate) and the
reaction temperature was raised to 80
C with continuous stirring. Then TIP and HNO
were added and the reaction was maintained at 50
C for 24 h. The prepared sol was dried at 105
C for 24 h and calcined at 300

°
C. Degradation of nitrophenol in aqueous phase [22] Fe The reactive magnetron sputtering

method: 99.99% titanium target and 99.9% iron pieces were placed in the reaction chamber and
mixture of argon and oxygen was introduced into the chamber during discharging. Wastewater
decoloring [23] V Sol-gel method: Solution 1 (vanadyl acetylacetonate dissolved in n-butanol) was
mixed with solution 2 (acetic acid in titanium butoxide) and hydrolyzed (24 h) by the water
generated via the estrification of acetic and butanol. The suspension as dried at 150
C, pulverized and calcined at 400
C for 0, 5 h. Wastewater decoloring [24] Au Titanium (IV) butoxide dissolved in absolute ethanol
was added to solution containing tetrachloroauric acid (HAuCl
·4H
O), acetic acid and ethanol. The resulting suspension was aged (2 days), dried under vacuum,
grinding and calcinated at 650
C. Wastewater decoloring [25]
M e t a l d o p a n t s
Pt Photoreduction process: TiO
was suspended in a mixture of hexachloroplatinic acid in methanol. The suspension was irradiated
with a 125 W mercury lamp (60 min.). Pt-TiO
was separated by filtration, washed with distilled water and dried at 100
C for 24 h. Wastewater decoloring [26] Titanium nitride (TiN) oxidation : Heating of TiN at 450-550
°
C for 2h in air (heating and cooling temperature rate: 2
C/min). Photooxidation of aromatic compounds (e.g. toluene) [27] N Treating anatase TiO
powder ST01 in the NH
(67%)/Ar atmosphere at 600
C for 3 h. Photooxidation of acetaldehyde in gas phase [18] S Oxidation annealing of titanium

disulfide (TiS
) at 300-600
C. Wastewater decoloring [28] N, S Hydrolysis of Ti(SO
in NH
aqueous solution. Precipitate was centrifuged, washed with distilled water and alcohol. Obtained
gels were dried under vacuum at 80 for 10 h and were ground to obtain xerogel. The xerogel was
calcinated at 400-800
C in air for 3 h. Photooxidation of volatile compounds in gas phase (e.g. acetone and formaldehyde
[29] Sol-gel method: TBOT was hydrolyzed in the presence of ethanol, water and nitric
acid; precipitated titanium hydroxide was dried at 110
°
C and calcinated in air at 150-200
C. Degradation of NOx; Wastewater decoloring [30] C Acid-catalyzed sol-gel process. Alkoxidide

precursor was dissolved in corresponding alcohol, mixed with hydrochloric acid aqueous solution.
Obtained gel was aged for several days and calcinated in air (3 h at 65
C and 3 h at 250
C) and grounded. Photooxidation of phenol compounds in aqueous phase [31] B Anatase TiO
powder (ST01) was grinding with boric acid triethyl ester and calcinated in air at 450
C. Photooxidation of phenol compounds in aqueous phase [32]
N o n m e t a l d o p a n t s
P Sol-gel method: TIP was hydrolyzed in the presence of isopropanol and water, After hydrolysis
phosphoric acid was added. Dispersion was stirred for 2h, centrifuged at 3500 rpm and dried at
100
C. Obtained powder was calcinated at 300
C. Photooxidation of phenol compounds in aqueous phase [33]

160
2008
metal-doped nanoparticles, which find utility as stabilizing ingredients within cosmetics to prevent
degradation from sun light, for use in agriculture, horticulture and veterinary medicine, as coatings
for plastics and for environmental protection. A particles of TiO
or ZnO were doped with one or more other elements such as concentration of dopant in the
surface of the particle is greater than that at the core of the particles. Suitable dopants for the
oxide particles include manganese (especially in form of Mn
3+
), vanadium, chro-mium, cerium, selenium, iron, nickel, copper, tin, aluminum, lead, silver,
zirconium, zinc and cobalt. The surface-doped particles of the present invention can be obtained
by combining particles of a host lattice (TiO
) with a second component in the form of a salt in solution in water, and then baking it, typically
at a temperature of at least 300
C and then calcining it at a higher temperature, for example at least 500 or 600
C. Patent application, published in 2006, is related to a method for preparing TiO
/SiO
aerogel micro-ball doped with iron [50]. Iron-doped TiO
2
could be obtained by mixing TiOSO
and FeCl
with deionized water and adjusting pH value to 7-8. Obtained precipitate is washed and mixed
with nitric acid solution at 50-90
C. Subsequently, silica sol is prepared by mixing of silicasol with nitric acid and anhydrate ethyl
alcohol. Then, titanium sol is mixed with SiO
alcohol sol at 1:3-8 volume ratio. TiO
/SiO
composite sol is added into oil phase to obtain micro ball, washed with acetone and dries.
Obtained micro-balls have diameter from 10 to 200
m. Described method represents a low-cost and simple process for doped-nanoparticles

manufacturing. Another invention is related to TiO
doped with molyb-denum (Mo) [51]. TiO-Mo monocrystalline substance could be obtained by
mixing TiO
with MoO
in the specific proportion, pressure molding the mixture and calcining this in air. The above-
mentioned molded body of TiO
2
doped with Mo consists of polycrystalline substance well-regulated in crystal size. In case of the
proportion of Mo doped in single crystal is less than 2.0 mol%, the granular growth of crystal is not
caused but it is made dense and intercrystalline cracking is not caused. In case the proportion of
Mo is more than 8.0 mol%, the granular growth of crystal is irregularly caused and the
intercrystalline cracking is not caused. US6884739
is related to lanthanide-doped TiOx dielec-tric films obtained by plasma oxidation [52]. A method
of forming a dielectric film includes evaporating a Ti source at a first rate to deposit a Ti on a
substrate, evaporating a lanthanide source at a second rate to form a lanthanide doped Ti film,
and oxidize the Ti/lanthanide film to grow a dielectric film on a substrate. The Ti and the
lanthanide are evaporated using electron beam evaporation or are assisted by ion beam
bombardment of the substrate surface during deposition. The evaporation of the Ti and
lanthanide is followed by oxidation using a Kr/oxygen plasma. The next invention provides
pyrogenically prepared titanium dioxide doped by an aerosol and containing, as a doping
component, an oxide selected from the group consisting of zinc oxide, platinum oxide, magnesium
oxide and/or aluminum oxide as the doping components [53]. Invented photocatalyst has either:
a) a BET surface area of 65 m
/g to 80 m
/g and a doping component concentration of 40 ppm to 800 ppm, or b) a BET surface area of 35 m
/g to 60 m
/g and a doping component concentration of more than 1000 ppm. Process for preparation of
doped-TiO
comprising two main steps: (1) feeding an aerosol into a flame used for the preparation of
pyrogenic titanium dioxide, and (2) separating the resulting photocatalys from the gas mixture;
wherein the titanium dioxide is prepared by flame oxidation or flame hydrolysis, and wherein the
aerosol: (a) comprises a salt solution or suspension containing: a metal salt, a metalloid salt,
mixtures of a metal salt and a metalloid salt, a suspension of a metal insoluble in water, a
suspension of a metalloid compound, or a mixture of a suspension of a metal insoluble in water
and a suspension of a metalloid compound, (b) is produced by atomisation using a two-com-
ponent nozzle, an aerosol generator, or ultrasound atomi-sation, and (c) is mixed homogeneously
with a gas mixture, wherein the gas mixture further comprises air, and allowed to react in the
flame. The core element of the apparatus is the open burner of known type, as is customarily used
for the preparation of pyrogenic oxides. The burner consists of an inner nozzle, from which the
main gas stream flows into the flame tube and burns. The inner nozzle is surrounded by a further
nozzle (jacket nozzle), from which ring or secondary hydrogen flows in order to avoid caking.
Between the nozzle outlet and the flame tube there is arranged a diaphragm through which the
aerosol is fed in, the aerosol gas stream from the diaphragm being mixed homogeneously with the
gas stream of the inner nozzle and the jacket nozzle [53].
Fig. (2).
Typical procedure of doped-TiO
preparation by sol-gel method.
Doped-TiO
2
2008
, Vol. 2, No. 3
161
The titanium dioxides according to the invention may be used for the degradation of impurities in
waste water and/or waste air and/or waste gases and for the sterilization of water with UV
irradiation. In that case, the titanium dioxides may be used both suspended in the waste water
and/or waste air and fixed to a support [53]. Japanese patent application describes method for
crystal-lizing metal-doped TiO
thin film and laminate having metal-doped TiO
thin film [54]. In this method, a polymer film is subjected to a plasma treatment by applying high
frequency electric power between two electrodes in an argon gas atmosphere, thereby the metal-
doped TiO
thin film highly crystallized and with enhanced electroconductivity is obtained. Another invention
refers to metallic ion-doped nano TiO
transparent photocatalytic emulsion and preparation method thereof [55]. According to the
invention optical transparent lotion features in 0.5 to 10% TiO
mixed with V, Sn, Zn, Fe, 1 to 10% emulsifier with the rest being water. It is obtained by making of
titanic chloride water solution containing metal ions is hydrolyzed to generate TiO
, VO
3
and Sn
4+
, Zn
2+
, Fe
3+
or Ce
3+
compound oxidation deposit. This method uses cheap titanium tetrachloride and ammonium
vanadate, iron trichloride, tin tetrachloride and zinc sulfate, using low temperature complex
hydrolysis to allow higher ability to mix and expanding spectral response zone to visible light.
Photocatalytic emulsion could be used to degradation of organic pollutants utilizing sun light or
irradiation emitted by fluorescent lamps [55].
2. RELATED PATENTS OF NONMETAL-DOPED TIO
Kabushiki Kaisha Toyota Chuo Kenkyusho is a developer of a photocatalytic material, a titanium

compound Ti-O-X, exhibiting a photocatalytic action when exposed to light with a wavelength in
the region of ultraviolet and visible irradiation [56]. Anion X is an element selected from B, C, P, S,
Cl, As, Se, Br, Sb, Te, or I, or a molecule con-taining at least one of these elements. Materials are
prepared by at least one of a method comprising substituting anions X for some the oxygen sites
of titanium oxide crystals, a method comprising doping anions X between lattices of a titanium
crystal and a method comprising doping grain boundaries of titanium oxide, or a combination of
these methods. The photocatalytic materials, described in this invention, acquired a new energy
level formed in a band gap of titanium oxide, which results in its increased photocatalytic activity
by absorbing visible light. Thus, the photocatalyst can exhibit satisfactory photocatalytic activity
even under solar or fluorescent light. Those material could be manufactured by the sol-gel
method, chemical reaction method, treatment in plasma containing anion species X, ion
implantation and RF magnetron sputtering. In the last method, substrate and titanium oxide target
are set in the vacuum chamber of a RF magnetron sputtering device. Then, an appropriate amount
of gas containing anions X (for example SO
+O
2
) and an inert gas (for example Ar) are introduced into the vacuum chamber to conduct sputtering.
Ti-O-X film is deposited on “substrate” surface serving as support. Various materials such as SiO
or ceramic were proposed for the support [56]. Furthermore, Ti-O-X can be applied not only in a
thin film but can also be included in binding materials for pain-tings such as silica, alumina,
fluororesin (polytetrafluoro-ethylene). Fig.
3 (a
) shows the Ti-O-X film /2/ formed on the SiO
substrate /1/ and film TiO
/3/ formed thereon. That is, TiO
/Ti-O-X film of gradient composition is formed in which the density of X atoms is diminishes closer
to the surface, and in which TiO
is exposed at the outmost surface. It is suitable that the TiO
/Ti-O-X photocatalyst of gradient composition be in the form of grains having Ti-O-X part /4/ on
the inside and TiO
part /5/ on the surface, as shown in Fig.
3 (b
). The gradient composition can be produced not only by heat treatment after lamination layer
formation of Ti-O-X and TiO
2
films, but also by changing the gas compo-sition in an atmosphere according to the deposition
state of the film [56]. The inventors suggested, that nonmetal-doping could improve the long-term
hydrophilicity compared to that of the TiO
film. TiO
/Ti-O-X film deposited on various surfaces could served as defogging agent and proofing against
the effects of organic substance decomposition. The US Patent No. 2008045410 pertains to doped
anatase-TiO
composition that exhibits enhanced photoca-talytic activity [57]. From the composition point of
view, this invention provides a nanosized, crystalline titanium dioxide (anatase) composition. The
composition is doped with phosphorus, and the doping level is between 0.10 and 0.55 weight
percent. Providing method includes: (1) spray drying of a phosphorus-doped solution of titanium
oxychloride, titanium oxysulphate or aqueous solution of another titanium salt to produce an
amorphous titanium dioxide solid inter-mediate with homogeneously distributed atoms of phos-
phorous through the matter; and (2) calcining the amorphous, solid intermediate at a
temperature between 300 and 900
C. Phosphoric acid could be used a phosphorus precursor. The optimal doping level is 0.33 weight
percent. The photocatalytic activity of the phosphorus-doped material is at least 100 percent
greater than the undoped material [57]. Phosphorus has a limited solubility in the anatase lattice.
In a calcination step, excess phosphorus is driven out from the lattice and ends up on the particle
surface. Depending on the calcination temperature, titanium phosphate, titanyl phosphate,
titanium pyrophosphate or their mixtures form on the particles surface. The enhanced
photodegradation activity is explained by creation a thin layer on the nanoanatase par-ticle by
excess phosphorus. Low concentration of phosphorus are evenly distributed throughout the
anatase crystal lattice and accordingly will not impact absorption properties of the material. At a
certain phosphorus content, a mono-molecular layer of titanium phosphate is formed on
the particle surface and this significantly increases the adsorption of organic compounds and
accelerated the photo-degradation efficiency. Further, increasing phosphorus concentration
induces the formation of a compact, thicker layer of titanium phosphate or pyrophosphate. The
adsorption of organic compounds on the particle surfaces is concomitantly increased, but the
photoactive TiO
2
core is
162
2008
insulated from the compounds and photoactivity is accordingly decreased [57]. The object of
another patent in this area is to provide ultraviolet and visible-light-sensitive titania based photo-
catalyst [58]. The photocatalysts, according to this invention, are characterized by their
composition as expressed by a general formula: TiSi
(2+2x-y)
(where 0.01<x<1 and 0.003<y<0.3). The invented photocatalysts have optical properties that the
relative absorbance at region from 300 nm to 450 nm is not lower than 0.1. In a regular titania of
anatase structure, Ti atoms are located in octahedral sites. When a titania is modified with silica,
the thermal stability of the material is improved significantly. In a silica-modified titania, Si atoms
are inserted to the tetrahedral holes of the anatase structure or Si atoms substitutes Ti atoms
located in the octahedral sites in the crystal structure. In the presented invention, nitrogen atoms
are introduced into the structure by NH
treatments at high temperatures. The thus-obtained materials are described as nitrogen-doped

silica-modified titania. The catalytic materials obtained in this invention can be widely used for
various practical fields, such as air-cleaning, water-purification, self-cleaning, anti-fogging,
disinfection, chemical synthesis, and hydrogen production via water decomposition. According to
inventors, this material is safe, nontoxic and inexpensive. It could be utilized also as coating
substance of various equipments, appliances and utensils, which are used for glasses, mirrors,
lightings, papers, or clothes, as well as construction materials [58]. Another invention in this
category, presents a sulfur-doped TiO
2
having enhanced activity in the presence of visible light, the production method and use of the
same [59]. A sulfur-containing titanium dioxide hydrate precipitate is obtained from an acid
titanium oxysulphate solution at a temperature below the boiling point of the solution, e.g. in the
range from 70 to 100°C, using crystal nuclei and without addition of base. The precipitate is
separated, washed and calcinated. Calcination of the hydrate precipitate is conducted in the
temperature range 100 to 500°C, most preferably in the temperature range 200 to 500°C. The
catalytic activity has been observed to decrease above and under this calcinations temperature
range. The photocatalytic titanium dioxide thus obtained has a specific area in the range from 100
to 250 m
/g and a 0.3 to 5% sulfur concentration. The calcinated end product is stable, and it has been
stated to have an excellent photo-catalytic effect at visible light wavelengths in different reactions.
Higher photocatalytic activity has been confirmed in acetaldehyde decomposition and in anionic
(SNC
radical formation. The sulfur built in the product in accordance with the invention is based on
precipitation from the sulfate solution conducted in acid conditions. Besides the presence of
sulfur, the observed high catalytic activity may relate to the precipitation of titanium as
orthotitanic acid. The precipitate has been confirmed to dissolve into 43% sulphuric acid at a
temperature of 60°C forming a 22% TiO
solution. Ortho-titanic acid produces a large specific area in the product, which is favorable in
terms of photocatalytic activity. According to inventors, S-TiO
could be used as a photocatalyst operating at visible light in the decomposition of organic

compounds or microorganisms and in cleaning of aquarium water containing algae [59]. The next
invention deals with a carbon-doped nanostruc-tured TiO
2
material having the following characteristics: an optical band gap lower than 2.1 eV and an optical
transmittance below 90%, 50% and 10% for wavelengths lower than 650 nm, 500 nm, and 400 nm,
respectively [60]. The C-TiO
can be obtained by thermal assembling of TiO
nanoparticles in the presence of a carbon source, which is preferably a carbon-containing

atmosphere such as the air. It was observed that under thermal annealing the grain growth is
modest, the nanostructure is retained and the rapid diffusion of C atoms present as contaminants
in the atmosphere into titania nanocrystalline lattice is highly favored. A process for preparing a
carbon-doped nanostructured TiO
material comprises: a) providing TiO
nanoparticles having average diameter below 10 nm assembled in a porous structure with density
in the range from 2.4 to 2.8 g/cm
; b) thermally treating the nanostructured TiO
at temperatures ranging from 900 to 1100
C in the presence of a carbon source. Nanostructured titanium dioxide is preferably obtained by

means of supersonic cluster beam deposition
Fig. (3)
. Gradient composition of TiO
doped with nonmetal anions according to [56].

Doped-TiO
2008
, Vol. 2, No. 3
163
using a pulsed microplasma cluster source, using the appa-ratus disclosed in US6392188. The
carbon-doped nanostructured TiO
material could be utilized as photocatalysts, in solar energy conversion devices and gas sensors.
The last invention in this section relates to titanium oxide-based photocatalysts which are
activated in the visible light and o self-cleaning materials that are prepared by substituting O of
pure TiO
with C and N [61]. The photo-catalyst has a general formula of TiO
2-x-
C
wherein 0 < x+
< 0.22, 0 < x < 0.2, and 0 <
< 0.02. A preparation method comprising a formation process of thin films by using Ti and inert
gas, N
and CO as mixed gas by reactive sputtering, and heat treating process of the formed thin film at a
temperature between 450 and 550°C for 2 to 4 hours, thereby crystallizing. The titanium oxide-
based photocatalysts having a general formula of TiO
2-x-
and self-cleaning materials according to this invention have a smaller optical band gap compared
to pure titanium oxides, and therefore, the photocatalysts can be activated under the visible light
range. In addition, they comprise only pure anatase crystallization phase, and since the
crystallized particles are small in size, the efficiency and self-cleaning effect of the photocatalysts is
very high [61].
4. CURRENT & FUTURE DEVELOPMENTS
The number of new publications, including patents, has been growing exponentially for the last
decade. The increa-sing number of papers, reports, conference proceedings and patents results
primarily from commercial interest in applications being developed in Japan in the early 70-ties.
The photocatalytic oxidation of organic compounds in aqueous environment has received the
most attention, but there is a rapidly increasing focus on the oxidation of volatile organic or
inorganic compounds in the gas phase, including NO
and SO
. Photocatalytic reduction of organic compounds and metal-containing ions and studies on cell
killing and disinfection by illuminated titanium dioxide have also received increasing attention.
Consequently, primarily in Japan, but also in the United States and latterly in China,
commercialization of TiO
photocatalysis has been initiated in various fields. In Japan, the commercialization of TiO
-based photocatalytic products commenced in the mid-1990s. More than 2000 companies have
joined in this new industry, whose products including: exterior construction materials (e.g. self-
cleaning tiles, glass and tents), interior furnishing materials (e.g. self-cleaning and antibacterial
tiles, wallpapers and window blinds), road construction materials (e.g. self-cleaning and air-
cleaning tunnel walls, soundproof walls and lamp covers), purification facilities (e.g. air cleaners,
air conditioners, purification system for wastewater and sewage, purification system for pools)
and household goods (e.g. self-cleaning and antibacterial fibers, clothes and sprays). Presently,
visible light-type TiO
(MPT-621) photo-catalyst based on the metal doping method, have been commercially available
in the form of powders and colloidal solutions in Japan. The visible light photocatalyst MPT-621 is
produced by treating platinum compound onto photocatalytic titanium dioxide which can be
sensitized by visible light. MPT-621 potentially will be used for indoor antibacterial and self-
cleaning applications and water cleanup with solar light. The current problem with doped TiO
may be the loss of photoactivity during recycling and long-term storage. It was assumed, that the
efficiency of metal doped-TiO
2
under visible light strongly depended on the preparation method used. In same cases, such doped
photocatalysts showed no activity under visible light and/or lower activity in the UV spectral range
compared to the non-doped TiO
because of high carrier recombination rates through the metal ion levels. The main present
problem with nonmetal-doped TiO
photocatalyst is that the photocatalytic activity under visible light is much lower than that under
ultraviolet light. Therefore, development of new and optimization of existing photocatalyts
exhibiting activity upon visible light with surface characteristics of improved performance and of
the high chemical and physical stability are crucial for broader scale utilization of photocatalytic
systems in commercial application. Such materials together with the development of technically
applicable self aligning photo-catalytic coating systems adaptable to the major substrates
(polymers, glass, ceramics or metals) will represent a ground breaking step change in this field
particularly in the economic viability of a range of potential processes. None-metal doping seems
to be more promising than metal doped-TiO
. One of the major challenges for the scientific and industrial community involved in photocatalytic
research is to increase the spectral sensitivity of TiO
-based photoca-talysts to visible light. A major area of future research would be the development
of new dopants, new method of dopant incorporation into TiO
structure as well as new application for environmental technology. Future patents would deal
with visible light-activated TiO
functioning in the presence of solar irradiation. The most important challenge which faces titania-
based catalysis is stable TiO
with predictable photoactivity in UV and visible light.
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Paper Title:
Influence of Doping on the Antibacterial Effect of TiO2 Nanoparticles
DOI 10.4028/www.scientific.net/MSF.510-511.86
Abstract
TiO2 nanoparticles doped with V, Mn or Zn, respectively, were synthesized from pure TiO2 and
dopants calcinating at definite temperature. The physical properties of prepared TiO2
nanoparticles were characterized by TEM, XRD and UV-vis spectrum. The TEM images showed
that the diameters of the particles were 20~50 nm. There was no peak of doping elements in
the XRD spectrum of nano-sized TiO2 doped, but the peak of a little amount of rutile was
observed, which demonstrated that V, Mn and Zn might locate in the TiO2 octahedral lattice, or
might be highly dispersed within crystalline of TiO2. In the meanwhile, doping of the TiO2
decreased the temperature for TiO2 transforming from anatase into rutile, and promoted the
transforming. It was found that a little amount of V5+ may take the place of Ti4+ in the lattice
of TiO2. The red-shift was clearly observed in the UV-vis spectrum of TiO2 nanopowders doped
with V. As a result, the band gap was changed and the TiO2 nanopowders doped with V enable
to absorb visible light. The red-shift could be assigned to the charge transfer transition between
the 3d orbital of V5+ and the TiO2 conduction or valance band. The red-shift was not observed
in the UV-vis spectrum of TiO2 nanopowders doped with Mn and with Zn, the shape of which
was similar to that of pure TiO2. The results of the minimum inhibition concentration (MIC) for
Escherichia coli and Staphylococcus aureus showed that vanadium ions doping intensely
improved the antibacterial efficiency of nanocrystallites. This was attributed to the change of
surface properties of metal ions doped semiconductor, such as O vacancies, Ti interstitial ions
and vanadium ions which took the place of titanium
All access types
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Sleep disturbances are common in pregnancy and may be influenced by a multitude of factors. Pregnancy
physiology may predispose to sleep disruption but may also result in worsening of some underlying sleep
disorders, and the de novo development of others. Apart from sleep disordered breathing, the impact of
sleep disorders on pregnancy, fetal, and neonatal outcomes is poorly understood. In this article, we review
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These include restless legs syndrome, insomnia, circadian pattern disturbances, narcolepsy, and sleep-
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Recent Patents on Engineering (2008), 2, 157-164

1872-2121/08 $100.00+.00 © 2008 Bentham Science Publishers Ltd.

Department of Chemical Technology, Gdansk University of Technology, 80-952-Gdansk, Poland

could be prepared by metal-ion implantation, reducing of TiO

, non-metal doping or sensitizing of TiO

with dyes. This paper reviews preparation methods of doped-TiO

, metal-doping, monmetal-doping, TiO

preparation methods, heterogeneous photocatalysis.

Strong oxidation and reduction power of photoexcited titanium dioxide (TiO

) was realized from the discovery of Honda-Fujishima effect. In 1972, Fujishima

. [1] reported photoinduced decomposition of water on TiO

to decompose cyanide in water, there has been an increasing interest in environmental

modification have been proposed: metal-ion implanted TiO

photocatalysts [7-8], non-metal doped-TiO

(N, S, C, B, P, I, F) [9-11], composites of TiO

with dyes (e.g. thionine) [13] and TiO

*Address correspondence to this author at the Department of Chemical Technology, Gdansk

mechanism of heterogeneous photocatalysis in the presence of TiO

1.1. Mechanism of Photoactivity of Pure TiO

Doped with Metal and Nonmetal Species

The photocatalytic mechanism is initiated by the absorption of the photon

with energy equal to or greater than the band gap of TiO

nanoparticle as schematized in Fig. (

Recent Patents on Engineering

, Vol. 2, No. 3 Adriana Zaleska

The visible light photoactivity of metal-doped TiO

by the dispersion of metal nanoparticles in the TiO

matrix. As shown in Fig. (

) electron can be excited from the defect state to the TiO

conduction band by photon with energy equals

Band gap narrowing: Asashi,

[18] found N 2p state hybrids with O 2p states in anatase TiO

is narrowed and able to absorb visible light. 2.

Impurity energy level: Irie,

[19] stated that TiO

Oxygen vacancies: Ihara,

[21]. They investigated N-TiO

and concluded that TiO

1.2. Doping Moieties and Preparation Methods

and methods of its preparation are shown in Table

obtained by an advanced high-voltage metal ion-implantation method [34]. The electronic

C. Obtained photocatalysts worked effectively in decomposition of NO into N

under visible light (

was prepared by the hydrothermal method [36]. Titanium (IV) tetra-

-butoxide and FeCl

C. Photocatalyst doped with FeCl

photocatalysts were synthesized by two modified sol-gel methods by Wu

C, pulverized and calcined at 400

C). Then, the solution was dried at 110

C, pulverized and calcined. Obtained vanadium-doped TiO

was described in 1986 by Sato,

[37]. They obtained N-TiO

films by sputtering the TiO

(67%)/Ar atmosphere at 600

Recent Patents on Engineering

2. RELATED PATENTS OF METAL-DOPED TIO

Oxonica Ltd. is a developer of innovative surface-doped particles of TiO

and ZnO [49]. This invention relates to

Table 1. Doping Moieties and Preparation Methods of Doped-Titanium Dioxide Photocatalysts

Kind of dopant Doped element Preparation method Potential application References

C with continuous stirring. Then TIP and HNO

were added and the reaction was maintained at 50

C for 24 h. The prepared sol was dried at 105