CN106068339A - There is insoluble anode and the manufacture method thereof of the porous film layer including electrode active material nanosphere - Google Patents
There is insoluble anode and the manufacture method thereof of the porous film layer including electrode active material nanosphere Download PDFInfo
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- CN106068339A CN106068339A CN201480076985.4A CN201480076985A CN106068339A CN 106068339 A CN106068339 A CN 106068339A CN 201480076985 A CN201480076985 A CN 201480076985A CN 106068339 A CN106068339 A CN 106068339A
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- electrode active
- active material
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
- C25D17/10—Electrodes, e.g. composition, counter electrode
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Abstract
The open a kind of insoluble anode of the present invention and manufacture method thereof, more specifically, insoluble anode and the manufacture method thereof of a kind of porous film layer having and including electrode active material nanosphere are disclosed, including: anode substrate, formed by being capable of anodised metal；Porous film layer, including sintered powder and the electrode active material nanosphere of described metal；Coating, is formed at the surface of described porous film layer inside and outside.Insoluble anode according to the present invention includes the porous film layer of electrode active material nanosphere by formation, compare existing insoluble anode, low resistance (lowresistivity) can be shown as significantly, described electrode active material nanosphere can be provided as the effecting reaction place of electron channel or reactant, therefore, it is possible to make reactant easily by thin layer inside, thus it is possible not only to improve the efficiency of insoluble anode, it is also possible to improve the life-span.
Description
Technical field
The present invention relates to a kind of insoluble anode and manufacture method thereof, particularly relate to a kind of following insoluble anode and
Manufacture method, is being formed and is including the sintered powder of described metal by being capable of the anode substrate that anodised metal formed
With the porous film layer of electrode active material nanosphere, thus reduce the electricity of electrode by means of electrode active material nanosphere
Resistance, and can be provided as reacting environment and electron channel, thus improve life-span and the function of anode.
Background technology
So far, although expensive, but height can be carried out because comparing solubility (soluable) anode (anode)
Capacity and uniform operation, and in electrolysis process, use the insoluble anode not interfering plating to react, and present and increase
Add its trend used.
In prior art, employ lead or metal as insoluble anode, but the lead of dissolution can cause environment dirty
The problems such as the quality reduction of dye and film.Therefore, just attempt developing and a kind of can replace the clean insoluble of lead system anode
Anode, the most especially has the titanium system anode of use titanium (Ti).
The electrode of iridium (Ir) or ruthenium (Ru) oxide isoreactivity material is coated because to producing oxygen at titanium (Ti) anode substrate
When gas or chlorine need overvoltage less and electrode life-span long, so being referred to as shape steady type anode (Dimensionally
Stable Anode；And be widely used in producing chlorine or the purpose of oxygen from aqueous solution DSA),.
Fig. 1 be medelling the figure of flow process of DSA manufacturing process according to prior art is shown, with reference to Fig. 1, can be at titanium
(Ti), after coating Ir or the Ru precursor of liquid on anode substrate, by dry and heat treatment, on titanium-base, coating is as electricity
The IrO of pole active substance2Or RuO2.In the case, exist and be difficult to be coated by precursor once and manufacture desired thickness
Shortcoming, therefore can by repeat precursor coat, be dried or high temperature under heat treatment and perform to manufacture the operation of final desired thickness.
In order to manufacture the most actually used several μm～the electrode active material of 50 μ m thick, need to repeat 5～8 times, even 20
Secondary above coating and heat treatment step, when the electrode active material layer of the highest thickness not only increases operation because repeating operation
Between, also product price can be caused to rise because using the catalyst material of high price.
In order to solve the problems referred to above, korean patent application the 10-2007-7015579th discloses following method:
Formed by spherical titanium (TiO2) sintered powder composition porous layer after, throughout the surface of porous layer and internal and form electricity
Pole active material layer, thus improve durability and decrease the usage amount (reference of high price electrode active material largely
Fig. 2).
But, the performance of the product with described DSA structure determines by magnitude of voltage, and described magnitude of voltage is by relatively applying
The product resistance of current value and determine, the resistance value of the material therefore used is important Consideration.That is, titanium dioxide
(TiO2) resistance be 0.29～3Wcm, it is significantly higher than IrO2Resistance (about 30mWcm), and actually by titanium dioxide
The resistance of porous membrane that titanium powder is formed also exist become to compare the resistance of material itself because of high interfacial tension and height very
Many problems.
Summary of the invention
Technical problem
The present invention is to solve that the problems referred to above propose, its object is to, it is provided that one forms electricity at porous film layer
Pole active substance nanosphere and there is the insoluble anode of effective DSA structure.
Further, another object of the present invention is to, it is provided that the manufacture method of described insoluble anode.
Technical scheme
According to for solving an aspect of of the present present invention of the problems referred to above, it is provided that one has and includes electrode active material nanometer
The insoluble electrode of the porous film layer of ball, it is characterised in that including:
Anode substrate, is formed by realizing anodised metal；
Porous film layer, including sintered powder and the electrode active material nanosphere of described metal；And
Electrode active material coating, is formed at the surface of described porous film layer inside and outside,
Wherein, described porous film layer includes: the sintered powder of the described metal of 60～90 volume %, and 10～
The electrode active material nanosphere of 40 volume %.
Further, according to a further aspect in the invention, it is provided that a kind of have the porous including electrode active material nanosphere
The manufacture method of the insoluble anode of thin layer, it is characterised in that
Described insoluble anode is by by realizing coating on the anode substrate that anodised metal is formed described gold
Carry out heat treatment after the sintered powder belonged to and high molecular nanometer sphere, then carry out at heat after electrode coated active substance precursors
Manage and manufacture,
The insoluble anode of described manufacture includes: anode substrate, is formed by realizing anodised metal；Porous is thin
Film layer, including sintered powder and the electrode active material nanosphere of described metal；And electrode active material coating, it is formed at
The surface of described porous film layer inside and outside.
Beneficial effect
The described insoluble anode according to the present invention includes the porous film of electrode active material nanosphere by formation
Layer, compares existing insoluble anode, can show as low resistance (low resistivity) significantly.Especially, described electrode
Active substance nanosphere can be provided as electron channel, and can include pore in inside, therefore, it is possible to as anti-
The effective reacting environment of thing is answered to be provided, it is possible to make reactant easily by thin layer inside, thus be possible not only to
Improve the efficiency of insoluble anode, it is also possible to improve the life-span.
Further, the method according to the invention, when manufacturing insoluble anode, it is possible to reduce be used for obtaining electrode active material
Activity duration of repetition of desired thickness, therefore there is raising productivity and the effect of economy.
Accompanying drawing explanation
Fig. 1 illustrates the schematic diagram of the flow process of the DSA processing technology according to prior art.
Fig. 2 is the figure illustrating the DSA manufacturing process including the porous film layer according to prior art.
Fig. 3 is the schematic diagram of the example of the insoluble anode illustrating the present invention.
Fig. 4 is medelling and illustrates the porous that includes the electrode active material nanosphere according to one embodiment of the invention
Electron channel that the formation of thin layer is adjoint or the effect of reacting environment.
Fig. 5 a, Fig. 5 b are to illustrate to pass through sweep electron microscope according under the different multiplying power of one embodiment of the invention
(SEM) and to including the porous film layer of electrode active material nanosphere and not including that electrode active material nanosphere is many
The photo of the surface analysis of permeability thin layer.
Fig. 6, Fig. 7 are medelling and illustrate the figure of the manufacturing process of the insoluble anode according to one embodiment of the invention.
Symbol description
10: substrate 20: the sintered powder of metal
30: electrode active material 40: high molecular nanometer sphere
50: electrode active material nanosphere
Detailed description of the invention
Hereinafter, referring to the drawings the insoluble anode of the present invention and the content of manufacture method thereof are described in detail.For
The thought of the present invention passed to the practitioner of this area fully and the accompanying drawing that is illustrated below is provided.Therefore, this
Bright it is not limited to accompanying drawing described below, and can embody with other forms.Now, academic when the technical term used and section
Language, when not having other to define, has in the art of the present invention and has what the personnel of ABC can be generally understood that
Implication, and following explanation and accompanying drawing eliminate known function and the structure that may unnecessarily obscure spirit of the invention
Become.
Fig. 3 is the schematic diagram of the example of the insoluble anode illustrating the present invention, according to the spy of the insoluble anode of the present invention
Levy and be, include electrode active material nanosphere at porous film layer, and at the inside and outside table of described porous film layer
Topcoating is covered with electrode active material.
Therefore, according to an aspect of the present invention, it is provided that a kind of have include that the porous of electrode active material nanosphere is thin
The insoluble anode of film layer, it is characterised in that including: anode substrate, is formed by can carry out realizing anodised metal；Porous
Property thin layer, including sintered powder and the electrode active material nanosphere of described metal；Electroactive material coating, is formed at institute
Stating the surface of porous film layer inside and outside, wherein, described porous film layer includes the described metal of 60～90 volume %
Sintered powder, and the electrode active material nanosphere of 10～40 volume %.
The insoluble anode of the described present invention utilizes thin with the sintered powder of anode substrate same metal formation porous
Film layer, thus there is the biggest surface area (40～80m2g-1), even if the electrode active material therefore forming thinner thickness is coated with
Layer, compares the situation used as the form of existing two dimensional surface by electrode active material, can have broader reaction
Place, and also include electrode active material nanosphere, such that it is able to compare metal when forming described porous film layer
Sintered powder and there is relatively the lowest resistance, therefore have and be prevented from the feature that electrode performance is low.
Now, as shown in Fig. 3 (a), described porous film layer can include that inside is full of by described electrode active material
Nanosphere, or as shown in Fig. 3 (b), the part in includable portion has leachy electrode active material nanosphere.
In connection with this, Fig. 4 illustrates the situation forming the porous film layer not including electrode active material nanosphere, with
And it is formed with the situation of the porous film layer including described electrode active material nanosphere, with reference to described Fig. 4, do not including electricity
In the situation (a) of pole active substance nanosphere, the mobile needs of electronics burn through the powder forming the metal of porous film layer
Knot body, therefore suffers from more restriction.On the contrary, the porous including electrode active material nanosphere it is being formed with according to the present invention
In the case of thin layer, become easy by the movement of the electronics of porous film layer because of electrode active material.Further, in institute
A part for the inside stating electronically active material includes in the situation (c) of pore, can maximize by assuring that sufficient pore
As reactant passage effect and as the effect of reacting environment.
Further, in the present invention, in described anode substrate use be capable of anodised metal can from titanium, tantalum,
Zirconium, niobium, tungsten or the group formed by their alloy select more than one.Now, the shape of described anode substrate and size
Shape and the size of the insoluble anode that can manufacture as required and properly select.Further, formed on the substrate
Porous film layer include that the sintered powder of metal is formed, now, the shape of the sintered powder of described metal is permissible
Being spherical, unsetting etc., its shape is unrestricted, it is contemplated that the permeability of electrode active material and anode substrate is tight
Patch property etc., are preferably used the sintered powder of spherical metal.
In the preferred embodiments of the present invention, described insoluble anode is utilizing titanium dioxide (TiO2) nanometer powder and to by
Titanium formed anode substrate surface formed porous film layer time, economy angularly on be more suitable for, but, by titanium
In the case of the surface of the anode substrate formed forms the porous film layer being made up of other metals in addition to titanium, permissible
It is manufactured into the anode that economy is at a relatively high according to the described kind being capable of anodised metal.In the case,
The porous film layer preferably formed by tantalum.
Further, thickness preferably 1～50 μm of described porous film layer.If the thickness of described thin layer is the thinnest, then because of
Not enough for the durability of porous film layer or the infiltration capacity of electrode active material, and be difficult to obtain predetermined effect.On the contrary, exist
In the case of its layer thickness is blocked up, the usage amount of agglutinating matter or the infiltration capacity of electrode active material increase to desirable value with
On, therefore can reduce economy.
Further, as other composition requirements of described porous film layer, the sintered powder of described metal or electrode
The size of active substance nanosphere is the most important.If the size of described electrode active material nanosphere is too small, then cause mixing
The quantitative change of sinter from metal powder many, and increase to more than desirable value, therefore can reduce economy.On the contrary, if electrode active
Property material nanosphere size excessive, then can reduce the amount of the sinter from metal powder of mixing, it can be difficult to obtain as electricity
Subchannel, effective reactant path and the effect of reacting environment.Therefore, in order to along with including that described electrode active material is received
Rice ball and play the electron channel of low resistance (low resistivity), effective reactant path and the work of reacting environment
With, the size preferably 50～1000nm of described electrode active material nanosphere, more preferably 200～500nm.
Further, the thickness including the porous film layer of described sinter from metal powder and electrode active material nanosphere is excellent
Select 1～50 μm, for forming the sinter from metal powder of the thin film of described thickness it is also preferred that 50～1000nm, more preferably 200～
500nm。
Further, other as porous film layer constitute requirement, and sintered powder and the electrode active material of metal are received
The mixing ratio of rice ball is the most important, if the mixed proportion of this electrode active material nanosphere is too small, then and the gold that resistance is high
The volume ratio of the sintered powder belonged to uprises relatively, therefore can reduce the performance of electrode, and be difficult to maximize as electronics
The effect of passage, the passage of reactant or the effect of reacting environment.On the contrary, if the mixing of described electrode active material nanosphere
Ratio is too high, and the import volume of the most described electrode active material increases to more than desirable value, therefore can reduce economy.Further, as
Upper described, can show as electron channel, effective reactant path according to the size of electrode active material nanosphere
Or the effect of reacting environment is therefore when determining described mixing ratio, bigger in the nanosphere size of described electrode active material
In the case of, it is possible to reduce the amount of the volume of mixing；And diminish along with the size of described electrode active material nanosphere and increase
The amount of the volume of mixing, such that it is able to maximize effect.Therefore, described porous film layer preferably includes: 60～90 volume %
The sintered powder of described metal, and the electrode active material nanosphere of 10～40 volume %.
Further, it is a feature of the present invention that described electrode active material is for selected from platinum, nickel, palladium, ruthenium, osmium, rhodium, iridium and palladium
More than one.
Further, described insoluble anode can manufacture by the following method: is being formed by can realize anodised metal
Anode substrate on coat the sintered powder of described metal and high molecular nanometer sphere after carry out heat treatment, be then coated with electrode active
Property precursors and carry out heat treatment.Fig. 6, Fig. 7 be medelling and illustrate manufacture according to one embodiment of the invention insoluble
The figure of the technique of anode.
Therefore, according to a further aspect in the invention, it is provided that a kind of have the porous including electrode active material nanosphere
The manufacture method of the insoluble anode of thin layer, it is characterised in that described insoluble anode is by by realizing anodic oxidation
The anode substrate that formed of metal on coat the sintered powder of described metal and high molecular nanometer sphere after carry out heat treatment, then
Carrying out heat treatment after electrode coated active substance precursors and manufacture, the insoluble anode of described manufacture includes: anode substrate, by
Anodised metal can be realized formed；Porous film layer, receives including described sinter from metal powder and electrode active material
Rice ball；Electrode active material coating, is formed at the surface of described porous film layer inside and outside.
With reference to Fig. 6 to Fig. 7, in order to form described porous film layer, first by realizing anodised metal shape
Coat the sintered powder of described metal and high molecular nanometer sphere on the anode substrate become and carry out heat treatment.More specifically,
Utilize the sintered powder of described metal to manufacture slurry, be then coated onto anode substrate, when making described slurry, also
Can include that high molecular nanometer sphere mixes, thus described slurry is being coated on substrate and is entering by means of heat treatment
During row sintering, macromolecule can be removed by burning.
Now, described high molecular nanometer sphere is characterised by, be by select free polystyrene (PS), polrvinyl chloride (PVC),
The height that more than one the macromolecule selected in the group that Merlon (PC) and polymethyl methacrylate (PMMA) are formed is formed
Molecule nano ball.
Further, described sintering preferably sinters at 400～600 DEG C, so that described high molecular nanometer sphere can burn, and makes
The sintered powder of metal can be deposited on anode substrate.
Then, electrode coated active substance precursors carry out heat treatment.More specifically, along with described electrode active material
Precursor is applied, meeting lead-in portion or whole electrode active material in the removed nanosphere of described macromolecule, and also can
It is applied to the surface of the sinter from metal powder being deposited.By the most again carrying out heat treatment, can formed
While the sintered powder of metal and the porous film layer of electrode active material nanosphere, at described porous film
The surface of layer inside and outside forms electrode active material coat.
Now, in order to form described electrode active material nanosphere, need to enable the electrode active material precursor of liquid
Rest on the high molecular nanosphere of removal, electrode active material the most just can be made to be imported into the high molecular nanosphere of described removal.
To this end, the size removing high molecular nanosphere is particularly important, when a diameter of the 50～1000nm of nanosphere, before described liquid
Body can rest on nanosphere and be imported into.Preferred a diameter of the 200 of described nanosphere～500nm.
Further, with reference to Fig. 6 and Fig. 7, described electrode active material nanosphere can be according to described liquid electrode active substance
The importing degree of precursor, and make electrode active material fill (with reference to Fig. 6) in the way of forming pore in an internal part, or
Person forms electrode active material nanosphere in the way of inside is filled up (Fig. 7) by electrode active material.
Further, in order to reduce by means of described electrode active material nanosphere electrode resistance and play electron channel,
Effective reactant path or the effect of reacting environment, as it has been described above, described porous film layer preferably includes: 60～90 bodies
The sintered powder of the described metal of long-pending %, and the electrode active material nanosphere of 10～40 volume %.
Now, more preferably, it is contemplated that the durability of porous film layer as above or oozing of electrode active material
Penetration, thickness preferably 1～50 μm of described porous film layer, for forming the powder sintered of the metal of the thin film of described thickness
Body it is also preferred that 50～1000nm, more preferably 200～500nm.
As it has been described above, insoluble anode and the manufacture method thereof of the present invention are illustrated with reference to the accompanying drawing limited, but
This example being intended merely to contribute to overall understanding of the present invention and providing, the art in the present invention has to be known substantially
The personnel known can realize multiple amendment and deformation according to these records.
Therefore, the thought of the present invention should not be limited to the accompanying drawing of explanation and determines, the thought range of the present invention should include power
Content in profit claimed range and there are all schemes of the deformation identical or of equal value with right.
Claims (8)
1. an insoluble anode, it has the porous film layer including electrode active material nanosphere, it is characterised in that bag
Include:
Anode substrate, is formed by being capable of anodised metal；
Porous film layer, including sintered powder and the electrode active material nanosphere of described metal；
Coating, is formed at the surface of described porous film layer inside and outside,
Wherein, described porous film layer includes: the sintered powder of the described metal of 60～90 volume %, and 10～40 bodies
The electrode active material nanosphere of long-pending %.
2. insoluble anode as claimed in claim 1, it is characterised in that
Described electrode active material nanosphere includes pore in an internal part.
3. insoluble anode as claimed in claim 1, it is characterised in that
The sintered powder of described metal or a diameter of the 50 of electrode active material nanosphere～1000nm.
4. insoluble anode as claimed in claim 1, it is characterised in that
The thickness of described porous film layer is 1～50 μm.
5. insoluble anode as claimed in claim 1, it is characterised in that
Described electrode active material is more than one in platinum, nickel, palladium, ruthenium, osmium, rhodium, iridium and palladium.
6. a manufacture method for insoluble anode, described insoluble anode has the porous including electrode active material nanosphere
Property thin layer, it is characterised in that
Described insoluble anode is by by being capable of on the anode substrate that anodised metal is formed coating described metal
Sintered powder and high molecular nanometer sphere after carry out heat treatment, be then coated with electrode active material precursor and carry out heat treatment and
Manufacture,
The insoluble anode of described manufacture includes: anode substrate, is formed by being capable of anodised metal；Porous film
Layer, including sintered powder and the electrode active material nanosphere of described metal；And electrode active material coating, it is formed at institute
State the surface of porous film layer inside and outside.
7. the manufacture method of insoluble anode as claimed in claim 6, it is characterised in that
The insoluble anode of described manufacture is the insoluble anode according to any one in claim 1 to 5.
8. the manufacture method of insoluble anode as claimed in claim 6, it is characterised in that
Described high molecular nanometer sphere is formed by selecting free polystyrene, polrvinyl chloride, Merlon and polymethyl methacrylate
Group in more than one macromolecule formed.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020140054000A KR101565844B1 (en) | 2014-05-07 | 2014-05-07 | Insoluble anode and method of preparing insoluble anode |
| KR10-2014-0054000 | 2014-05-07 | ||
| PCT/KR2014/010289 WO2015170808A1 (en) | 2014-05-07 | 2014-10-30 | Insoluble anode with porous film layer comprising nanosphere of electrode active material, and method for preparing same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106068339A true CN106068339A (en) | 2016-11-02 |
| CN106068339B CN106068339B (en) | 2018-02-02 |
Family
ID=54392643
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201480076985.4A Active CN106068339B (en) | 2014-05-07 | 2014-10-30 | Insoluble anode and its manufacture method with the porous film layer including electrode active material nanosphere |
Country Status (3)
| Country | Link |
|---|---|
| KR (1) | KR101565844B1 (en) |
| CN (1) | CN106068339B (en) |
| WO (1) | WO2015170808A1 (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0407355A1 (en) * | 1989-06-07 | 1991-01-09 | Permelec Electrode Ltd | Insoluble electrode for electroplating and process for producing the same |
| JP2000178791A (en) * | 1998-12-11 | 2000-06-27 | Nikon Corp | Production of porous titanium oxide film |
| CN101098990A (en) * | 2005-01-07 | 2008-01-02 | 大曹株式会社 | Insoluble electrode |
| KR20110011001A (en) * | 2009-07-27 | 2011-02-08 | 일진머티리얼즈 주식회사 | Insoluble anode and method of preparing insoluble anode |
| KR20120001896A (en) * | 2010-06-30 | 2012-01-05 | 서강대학교산학협력단 | Photoelectrode for dye-sensitized solar cell, preparing method of the same, and dye-sensitized solar cell having the same |
-
2014
- 2014-05-07 KR KR1020140054000A patent/KR101565844B1/en active IP Right Grant
- 2014-10-30 CN CN201480076985.4A patent/CN106068339B/en active Active
- 2014-10-30 WO PCT/KR2014/010289 patent/WO2015170808A1/en active Application Filing
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0407355A1 (en) * | 1989-06-07 | 1991-01-09 | Permelec Electrode Ltd | Insoluble electrode for electroplating and process for producing the same |
| JP2000178791A (en) * | 1998-12-11 | 2000-06-27 | Nikon Corp | Production of porous titanium oxide film |
| CN101098990A (en) * | 2005-01-07 | 2008-01-02 | 大曹株式会社 | Insoluble electrode |
| KR20110011001A (en) * | 2009-07-27 | 2011-02-08 | 일진머티리얼즈 주식회사 | Insoluble anode and method of preparing insoluble anode |
| KR20120001896A (en) * | 2010-06-30 | 2012-01-05 | 서강대학교산학협력단 | Photoelectrode for dye-sensitized solar cell, preparing method of the same, and dye-sensitized solar cell having the same |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106068339B (en) | 2018-02-02 |
| KR101565844B1 (en) | 2015-11-05 |
| WO2015170808A1 (en) | 2015-11-12 |
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