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type I electrochromic materials are soluble in both the reduced state and the
oxidized state. Examples are the prototype viologen, N,N - dimethyl-4,4
-bipyridylium [methyl viologen (MV)] and numerous metal complex and organic
redox indicators. Type II electrochromic materials are soluble in one redox state
but form a solid film on the surface of an electrode following electron transfer.
Examples are N,N -bis(nheptyl)-4,4 -bipyridylium [heptyl viologen (HV)] in
water and the reversible electrodeposition of metals. In type III electrochromic
materials, such as tungsten oxide (WO3), polymeric viologens, conjugated
conducting polymers, metallopolymers, and the metal hexacyanometallate
Prussian blue (PB), both or all redox states are solid, and these systems are
studied as thin films on electrode surfaces.
For types II and III, once the redox state has been switched, no further charge
injection is needed to retain the new electrochromic state, and such systems
have optical memory. In contrast, for type I electrochromic materials, diffusion
of the soluble electrochemically generated product material away from the
electrode occurs, and it is necessary to keep current flowing until the whole
solution has been electrolyzed
This review surveys the main classes of electrochromic materials, namely,
metal oxide films (especially tungsten oxide); viologens (4,4 -bipyridylium salts,
in solution and as polymer films); conjugated conducting polymers; metal
coordination complexes as polymeric, evaporated, or sublimed films; and PB.
The oxides of the following (transition) metals are electrochromic: cerium,
chromium, cobalt, copper, iridium, iron, manganese, molybdenum, nickel,
niobium, palladium, praseodymium, rhodium, ruthenium, tantalum, titanium,
tungsten, and vanadium (1). Most of the electrochromic colors derive from
intervalence charge-transfer optical transitions; the more highly colored form of
most metal oxide electrochromic materials are in the range of blue or gray
through black. The oxides of tungsten, molybdenum, iridium, and nickel show
the most intense electrochromic color changes. Other metal oxides of lesser
colorability are however useful in ECDs as the optically passive secondary
electrode material. Those metal oxides that are available as (essentially)
colorless thin films and that can be chemically or electrochemically reduced to
a nonstoichiometric redox state with an intense electronic absorption band
have the most applicability to ECDs.
WO3 colorless + x(H+ + e) = HxWVI (1x) WV x O3 deep blue .
WO3 colorless + x(Li+ + e) = LixWVI (1x) WV x O3 deep blue .

As noted above, many other thin-film metal oxides (13), for example, the
oxides of molybdenum and vanadium (13), are electrochromic:
MoO3 colorless + x(M+ + e) = HxMoVI (1x) MoV x O3 deep blue
V2O5 brown-yellow + x(M+ + e) = MxVIV (1x) VV x O5 very pale blue .
In his device, electrochromic coloration occurred on application of 104 V cm1
across a thin film of highly disordered, vacuum-deposited WO3 on quartz.
In these examples, the more intensely absorbing redox state is produced on
reduction, with concurrent cation insertion. In contrast, group VIII metal oxides
become colored on electrochemical oxidation, as in the case of hydrated
iridium oxide (iridium hydroxide). The mechanism of coloration is uncertain;
both proton extraction and anion insertion routes are proposed:
Ir(OH)3 colorless = IrO2 H2O + H+ + e blue-gray ,
Ir(OH)3 + OH colorless = IrO2 H2O + H2O + e blue-black .
Ni(OH)2 pale green + OH = NiO OH brown-black + H2O + e.
Preparation of Thin-Film Metal Oxides For ECD application,
metal oxides must be deposited on a conducting substrate as a thin, even film,
typically in the range of 0.20.5 m. Such thin films are either amorphous or
polycrystalline, sometimes both admixed, and the morphology depends
strongly on the mode of film preparation. Granqvists book (3) and reviews give
extensive detail on the preparation of metal oxide films. Deposition methods
have been outlined (1) and comprise chemical vapor deposition,
electrodeposition, sol-gel techniques (spray pyrolysis, dip and spin coating),
sputtering in vacuo (using dc magnetron, electron beam, and radio frequency
radiation), thermal deposition in vacuo, and Langmuir-Blodgett deposition.
This type of ECD therefore requires passage of a continuous small current for
replenishment of the colored electroactive species lost by their mutual selferasing solution redox reaction. A solution-phase electrochromic system in
acetonitrile comprising nine solution-phase electrochromic thin-layer cells
based on HV perchlorate and N,N ,N,N -tetramethyl-1,4-phenylenediamine
(TMPD) has been investigated for display applications (43). Equation 9 shows
the spontaneous reaction between the radical cations that is associated with
bleaching, whereas the electrolytic reverse reaction generates an intense blue
coloration:

The influences of operating voltage and cell gap have been investigated in a
solution-phase ECD containing HV and TMPD in propylene carbonate, with 0.5
mol dm3 tetrabutylammonium tetrafluoroborate as supporting electrolyte
(44). Reversible electrochromism was achieved only when the cell gap was kept
at 0.28 mm. On/off application of 1.0 V was sufficient to observe the color
change.

NanoChromicsTM displays are of a monolith construction and consist of a

multilayer printed structure on a single substrate. A conducting ITO on
poly(ethylene terephthalate) (PET) substrate acts as the negative electrode
(the cathode on coloration) and is coated with a 4-m-thick TiO2 film, followed
by a monolayer of self-assembled, chemisorbed, phosphonated viologen
molecules. The positive counterelectrode (the anode on coloration) carries a 3m-thick film of high-surfacearea antimony tin oxide (SnO2:Sb) on a conductive
carbon/PET substrate. Application of 1.0 V reversibly reduces the dicationic
viologen to its blue radical cation. Placing an ion-permeable nanostructured
TiO2 layer (as diffuse reflector) between the electrodes results, on coloration, in
the visual effect of ink on pure white paper.
ECDs operate as rechargeable electrochemical cells, with each containing a
minimum of two electrodes separated by a layer of ion-containing electrolyte. A
liquid, gel, or solid electrolyte is sandwiched between the primary
electrochromic electrode and a charge-balancing secondary electrode. Color
switching takes place on charge/discharge by application of an appropriate
electrical potential. ECDs are designed to operate in either
absorptive/transmissive or reflective modes.
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http://0-pubs.acs.org.millenium.itesm.mx/doi/pdf/10.1021/am502929p?

https://www.youtube.com/watch?v=oVN9DV1LmSU
https://www.youtube.com/watch?v=mF_Z8RUZjJE
http://jp.ricoh.com/technology/tech/pdf/EP1-1.pdf
http://pubs.acs.org/doi/ipdf/10.1021/am404226e
http://www.investigacionyciencia.es/revistas/investigacion-yciencia/numero/447/materiales-electrocrmicos-11627
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http://0-pubs.acs.org.millenium.itesm.mx/doi/abs/10.1021/cm1021245
http://0-pubs.acs.org.millenium.itesm.mx/doi/abs/10.1021/am404226e