CN105304340B - The preparation method of used by dye sensitization solar battery porous titanium dioxide thin-film - Google Patents
The preparation method of used by dye sensitization solar battery porous titanium dioxide thin-film Download PDFInfo
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- CN105304340B CN105304340B CN201510672868.0A CN201510672868A CN105304340B CN 105304340 B CN105304340 B CN 105304340B CN 201510672868 A CN201510672868 A CN 201510672868A CN 105304340 B CN105304340 B CN 105304340B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E10/542—Dye sensitized solar cells
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Abstract
The invention discloses a kind of preparation method of porous titanium dioxide thin-film in DSSC, belong to porous material preparation field.The preparation method comprises the following steps：(1) base material of surface cleaning is provided, titaniferous organic/inorganic composite film is deposited in substrate material surface using molecular-layer deposition technology；(2) base material that the surface of preparation is deposited to titaniferous organic/inorganic composite film is heat-treated 2 5h at 400 600 DEG C, obtains porous titanium dioxide thin-film.Porous titanium dioxide thin-film thickness prepared by the present invention accurately controls, and for distribution of pores than more uniform, specific surface area is big; uniformity and well-crystallized, impedance is smaller, and photogenerated current density significantly improves; its photoelectric properties can be greatly improved, in addition, process equipment is simple; operating process is few, and reaction condition is gentle, and production efficiency is high; cost and energy consumption are relatively low, pollution-free to ecological environment, and reproducible; practical effect is excellent, is suitable for scale application.
Description
Technical field
The invention belongs to porous material preparation field, more particularly to a kind of used by dye sensitization solar battery porous silica
The preparation method of titanium film.
Background technology
The sustainable development of energy and environment is just turning into two important development strategies of world today's human society.With section
The progress of skill and the development of human society, people sharply increase to the demand of the energy, and the exploitation and application of new energy are imperative.
As a kind of inexhaustible, nexhaustible clean reproducible energy, the research on utilization of solar energy causes whole world research people
The fervent concern of member.Wherein, DSSC is exactly such a photoelectric device for effectively utilizing solar energy, and it makes
Make that technique is simple, cost is cheap, stable performance, environmentally safe, thus there is good development prospect.However, dyestuff is quick
Changing solar cell, photoelectric transformation efficiency is relatively low in actual applications, and this greatly limits its development.As dye molecule
Support and absorption and the transmission of carrier and carrier of separating, nano-titanium dioxide film is because existing with excellent photoelectric properties
Very important role is play in terms of improving photoelectric transformation efficiency, and film specific surface area is to determine dye sensitization of solar electricity
An important factor for various performances in pond, wherein, it is the important of increase film specific surface area to prepare loose structure titanium deoxid film
One of approach.
In the prior art, Chinese patent CN201310677816.3, publication date is loose structure titanium deoxid film
On March 12nd, 2014, entitled " a kind of preparation method of porous titanium dioxide thin-film ", this method using hollow glass micropearl as
Matrix, using Cu-Zn or Cu-Mn alloys as target, magnetron sputtering C u-Zn or Cu-Mn alloy firm, then it is molten using acid or alkalescence
Liquid carries out de- Alloying Treatment, then is cleaned and dried with deionized water；Then by the glass microballoon of dried parcel Porous Cu
Again by magnetron sputtering deposition titanium dioxide, so as to prepare poriferous titanium dioxide.The porous silica prepared using this method
Titanium film has larger surface area, can improve optically catalytic TiO 2 effect under ultraviolet light, but improving photoelectric transformation efficiency
Aspect effect is limited.Chinese patent CN200610049154.5, publication date are on January 18th, 2006, and entitled " one kind prepares more
The method of porous titanium dioxide film ", for this method using iso-butyl titanate as presoma, ethylene glycol monomethyl ether is solvent, with hydroxyl fiber
Element is additive, and porous titanium dioxide thin-film is prepared by Best-Effort request using sol-gel process, this method prepare porous two
Thin film of titanium oxide has more preferable hydrophily and photocatalytic activity, and group when effectively prevent the hydrolysis of TiO 2 particles
It is poly-, and by changing Best-Effort request number, can be with the thickness of porous titanium dioxide thin-film, but improving photoelectric transformation efficiency side
Face effect is still limited.Chinese patent CN200910096794.5, publication date are on March 19th, 2009, entitled " a kind of double-deck
Nanostructured anatase titanium dioxide photoelectric film and preparation method thereof ", this method are received titanium dioxide using sol-gel process
Rice grain film is spun on titanium-base of the surface covered with poriferous titanium dioxide network layer, because interface titanium dioxide is received
The photo electric that cooperative effect be present and improve film is staggeredly inlayed between rice grain and mesh structural porous titanium dioxide network
Can, and film forming is uniform, and crystallinity is good, and purity is higher, however, the titanium dioxide nano-particle poor compatibility of boundary, its
Poor durability, it strongly limit DSSC industrialized development.
The content of the invention
In order to achieve the above object, the invention provides a kind of specific surface area is big, film forming uniformly, well-crystallized, purity it is high
Used by dye sensitization solar battery porous titanium dioxide thin-film preparation method.
The invention provides a kind of preparation method of used by dye sensitization solar battery porous titanium dioxide thin-film, it includes
Following steps：
Step A, there is provided the base material of surface cleaning, titaniferous is deposited in substrate material surface using molecular-layer deposition technology
Organic inorganic film；
Step B, the material that step A is obtained is heat-treated 2-5h at 400-600 DEG C, obtains porous titanium dioxide thin-film.
The beneficial effect of the preparation method of used by dye sensitization solar battery porous titanium dioxide thin-film provided by the invention
It is：
(1) nano-titanium dioxide film for preparing of the present invention is in loose structure, and pore scale is in nano-scale range, and hole
Distribution is than more uniform；
(2) present invention is combined by molecular-layer deposition technology with heat treatment prepares porous titanium dioxide thin-film, increases
The specific surface area of titanium deoxid film, simultaneously as guarantor's type characteristic of molecular-layer deposition technology, ensures substrate material surface deposition
The uniformity of titanium deoxid film.Porous titanium dioxide thin-film film forming prepared by the present invention is uniform, well-crystallized, and purity is high, with
Titanium deoxid film prepared by conventionally employed sol-gel process is compared, and impedance is smaller, and photogenerated current density significantly improves, greatly
Improve its photoelectric properties；
(3) present invention can be by adjusting number of deposition cycles come the accurate thickness for controlling porous titanium dioxide thin-film；
(4) porous titanium dioxide thin-film prepared by the present invention, process equipment is simple, and operating process is few, and reaction condition is gentle,
Production efficiency is high, and cost and energy consumption are relatively low, pollution-free to ecological environment, and reproducible, are suitable for scale application.
Brief description of the drawings
Fig. 1 is the structural representation for the porous titanium dioxide thin-film that the present invention is prepared.
Embodiment
As shown in figure 1, the invention provides a kind of preparation of used by dye sensitization solar battery porous titanium dioxide thin-film
Method, it comprises the following steps：
Step A, there is provided the base material 2 of surface cleaning, contained using molecular-layer deposition technology in the surface of base material 2 deposition
Titanium Organic inorganic film；
Step B, the material that step A is obtained is heat-treated 2-5h at 400-600 DEG C, obtains porous titanium dioxide thin-film 1.
Preferably, base material 2 is cleaned with organic solvent and deionized water under Ultrasonic Conditions in the step A, then
Base material 2 after cleaning is dried up with compressed nitrogen to obtain the base material 2 of surface cleaning.Specifically, the organic solvent
For one kind in isopropanol, alcohol, chloroform or acetone.
Preferably, the step B includes,
Step A1, the base material 2 of surface cleaning is put into the reaction for the atomic layer deposition apparatus that temperature is 80-150 DEG C
In chamber, 5-30min is purged with 50-100sccm high pure nitrogens；
Step A2, by TiCl4Or titanium tetraisopropylate is heated to 60-100 DEG C of formation TiCl4Or titanium tetraisopropylate steam, and with
Impulse form is by TiCl4Or titanium tetraisopropylate steam is sent into reaction cavity, burst length 0.05-0.2s, open-assembly time 8-
15s, then purged with high pure nitrogen, purge time 15-30s；
Step A3, dihydric alcohol or polyalcohol are heated to 100-200 DEG C and form dihydric alcohol or polynary alcohol vapor, then with pulse
Form is sent into reaction cavity, burst length 0.1-1s, open-assembly time 20-45s, then is purged with high pure nitrogen, purge time
For 30-45s, primary depositing circulation is completed, i.e., deposited one layer of titaniferous Organic inorganic film on the surface of base material 2；
Step A4, repeat step A2-A3 deposition cycle 100-20000 times.
It is further preferred that dihydric alcohol is one kind in ethylene glycol, propane diols or butanediol in the step A3；Polyalcohol
For one kind in glycerine, trimethylolethane, pentaerythrite, xylitol or sorbierite.
It is further preferred that each deposition cycle makes obtained titaniferous Organic inorganic film thickness in the step A3
Increase as 0.06-0.12nm.
It is further preferred that in the step A4 repeat step A2-A3 deposition cycle 1000-10000 times.
Preferably, described base material 2 is the silica electro-conductive glass of doping fluorine, i.e. FTO electro-conductive glass, indium tin oxygen
Compound electro-conductive glass, i.e. ITO electro-conductive glass, mix the zinc oxide electro-conductive glass of aluminium, i.e. AZO electro-conductive glass, monocrystalline silicon piece, copper foil or
One kind in non-woven fabrics.
Preferably, it is heat-treated in the step B and is carried out in air, oxygen or inert atmosphere.
Preferably, the specific surface area that the specific surface area for porous titanium dioxide thin-film 1 being obtained in the step B is is 60-
400m2/ g, pore scale is in 8~10nm..
With reference to specific embodiment, further the present invention will be described in detail.Certainly described embodiment is only
The part of the embodiment of the present invention, rather than whole embodiments, based on the embodiment in the present invention, those skilled in the art are not having
There is the every other embodiment made and obtained under the premise of creative work, belong to protection scope of the present invention.
Embodiment 1
First, FTO electro-conductive glass is cleaned with isopropanol under Ultrasonic Conditions, then the FTO electro-conductive glass after cleaning is pressed
Contracting nitrogen dries up；
Secondly, FTO electro-conductive glass is put into the reaction chamber for the atomic layer deposition apparatus that temperature is 80 DEG C, with 50sccm height
Pure nitrogen gas purges 5min；
Then, by purity be 97% TiCl4It is heated to 60 DEG C of formation TiCl4Steam, and with impulse form by TiCl4Steam
Pneumatic transmission enters reaction cavity, burst length 0.05s, open-assembly time 8s, then is purged with high pure nitrogen, purge time 15s；
Next, ethylene glycol is heated into 100 DEG C of formation ethylene glycol steams, then reaction cavity, arteries and veins are sent into impulse form
It is 0.1s, open-assembly time 20s to rush the time, then is purged with high pure nitrogen, purge time 30s, completes primary depositing circulation, i.e.,
One layer of titaniferous Organic inorganic film is deposited in substrate material surface；
Method repeats this deposition cycle 20000 times according to this；
Finally, obtained surface deposited to the FTO electro-conductive glass of the doping fluorine of titaniferous Organic inorganic film in air
5h is heat-treated in atmosphere at 450 DEG C, the organic component in titaniferous Organic inorganic film is removed, so as to obtain porous dioxy
Change titanium film.
The porous TiO prepared using above-mentioned technological parameter2Film, titaniferous that each deposition cycle may be such that is organic-nothing
The increase of machine composite film thickness is 0.06nm, therefore, porous titanium dioxide thin-film thickness 1200nm, specific surface area 400m2/ g, put down
Equal aperture 8nm.
Embodiment 2
First, alcohol washes ITO electro-conductive glass is used under Ultrasonic Conditions, then the ITO electro-conductive glass after cleaning is compressed
Nitrogen dries up；
Secondly, ITO electro-conductive glass is put into the reaction chamber for the atomic layer deposition apparatus that temperature is 150 DEG C, uses 100sccm
High pure nitrogen purges 30min；
Then, the titanium tetraisopropylate that purity is 97% is heated to 65 DEG C of formation titanium tetraisopropylate steams, and with pulse form
Titanium tetraisopropylate steam is sent into reaction cavity, burst length 0.2s, open-assembly time 15s by formula, then is purged with high pure nitrogen,
Purge time is 30s；
Next, glycerine is heated into 120 DEG C of formation glycerine steams, then reaction cavity, arteries and veins are sent into impulse form
It is 1s, open-assembly time 30s to rush the time, then is purged with high pure nitrogen, purge time 45s, completes primary depositing circulation, that is, exists
Substrate material surface deposited one layer of titaniferous Organic inorganic film；
Method repeats this deposition cycle 10000 times according to this；
Finally, obtained surface deposited to the ITO electro-conductive glass of the doping fluorine of titaniferous Organic inorganic film in air
2h is heat-treated in atmosphere at 600 DEG C, the organic component in titaniferous Organic inorganic film is removed, so as to obtain porous dioxy
Change titanium film.
The porous TiO prepared using above-mentioned technological parameter2Film, titaniferous that each deposition cycle may be such that is organic-nothing
The increase of machine composite film thickness is 0.08nm, therefore, porous titanium dioxide thin-film thickness 800nm, the ratio surface of titanium deoxid film
Product is 220m2/ g, pore scale is in 8.325nm.
Embodiment 3
First, copper foil is cleaned with chloroform under Ultrasonic Conditions, then the copper foil after cleaning is dried up with compressed nitrogen；
Secondly, copper foil is put into the reaction chamber for the atomic layer deposition apparatus that temperature is 100 DEG C, with 70sccm high pure nitrogens
Purge 20min；
Then, the titanium tetraisopropylate that purity is 97% is heated to 65 DEG C of formation titanium tetraisopropylate steams, and with pulse form
Titanium tetraisopropylate steam is sent into reaction cavity, burst length 0.2s, open-assembly time 15s by formula, then is purged with high pure nitrogen,
Purge time is 30s；
Next, glycerine is heated into 120 DEG C of formation glycerine steams, then reaction cavity, arteries and veins are sent into impulse form
It is 1s, open-assembly time 30s to rush the time, then is purged with high pure nitrogen, purge time 45s, completes primary depositing circulation, that is, exists
Substrate material surface deposited one layer of titaniferous Organic inorganic film；
Method repeats this deposition cycle 1000 times according to this；
Finally, obtained surface deposited to the copper foil of the doping fluorine of titaniferous Organic inorganic film in air atmosphere
5h is heat-treated at 400 DEG C, removes the organic component in titaniferous Organic inorganic film, it is thin so as to obtain poriferous titanium dioxide
Film.
The porous TiO prepared using above-mentioned technological parameter2Film, titaniferous that each deposition cycle may be such that is organic-nothing
The increase of machine composite film thickness is 0.96nm, therefore, porous titanium dioxide thin-film thickness 96nm, the specific surface area of titanium deoxid film
For 106m2/ g, pore scale is in 9.45nm..
Embodiment 4
First, non-woven fabrics is cleaned with acetone under Ultrasonic Conditions, then the non-woven fabrics after cleaning is dried up with compressed nitrogen；
Secondly, non-woven fabrics is put into the reaction chamber for the atomic layer deposition apparatus that temperature is 100 DEG C, with 70sccm High Purity Nitrogens
20min is swept in air-blowing；
Then, by purity be 97% TiCl4It is heated to 60 DEG C of formation TiCl4Steam, and with impulse form by TiCl4Steam
Pneumatic transmission enters reaction cavity, burst length 0.05s, open-assembly time 8s, then is purged with high pure nitrogen, purge time 15s；
Next, ethylene glycol is heated into 100 DEG C of formation ethylene glycol steams, then reaction cavity, arteries and veins are sent into impulse form
It is 0.1s, open-assembly time 20s to rush the time, then is purged with high pure nitrogen, purge time 30s, completes primary depositing circulation, i.e.,
One layer of titaniferous Organic inorganic film is deposited in substrate material surface；
Method repeats this deposition cycle 100 times according to this；
Finally, obtained surface deposited to the non-woven fabrics of the doping fluorine of titaniferous Organic inorganic film in air atmosphere
In be heat-treated 4h at 500 DEG C, the organic component in titaniferous Organic inorganic film is removed, so as to obtain poriferous titanium dioxide
Film.
The porous TiO prepared using above-mentioned technological parameter2Film, titaniferous that each deposition cycle may be such that is organic-nothing
The increase of machine composite film thickness is 0.12nm, therefore, porous titanium dioxide thin-film thickness 12nm, the specific surface area of titanium deoxid film
For 60m2/ g, pore scale is in 9.854nm..
Claims (9)
1. a kind of preparation method of used by dye sensitization solar battery porous titanium dioxide thin-film, it comprises the following steps：
Step A, there is provided the base material of surface cleaning, had using molecular-layer deposition technology in substrate material surface deposition titaniferous
Machine-inorganic substances compound membrane；
Step B, the material that step A is obtained is heat-treated 2-5h at 400-600 DEG C, obtains porous titanium dioxide thin-film；
The step A includes,
Step A1, the base material of surface cleaning is put into the reaction chamber for the atomic layer deposition apparatus that temperature is 80-150 DEG C,
5-30min is purged with 50-100sccm high pure nitrogens；
Step A2, titanium tetraisopropylate is heated to 60-100 DEG C of formation titanium tetraisopropylate steam, and with impulse form by four isopropyls
Alcohol titanium tetrachloride vapor is sent into reaction cavity, burst length 0.05-0.2s, open-assembly time 8-15s, then is purged with high pure nitrogen, blows
Flyback time is 15-30s；
Step A3, dihydric alcohol or polyalcohol are heated to 100-200 DEG C and form dihydric alcohol or polynary alcohol vapor, then with impulse form
Reaction cavity, burst length 0.1-1s, open-assembly time 20-45s are sent into, then is purged with high pure nitrogen, purge time 30-
45s, primary depositing circulation is completed, i.e., deposited one layer of titaniferous Organic inorganic film in substrate material surface；
Step A4, repeat step A2-A3 deposition cycle 100-20000 times.
2. the preparation method of used by dye sensitization solar battery porous titanium dioxide thin-film as claimed in claim 1, its feature
It is：In the step A base material is cleaned under Ultrasonic Conditions with organic solvent and deionized water, then by the base after cleaning
Bottom material is dried up to obtain the base material of surface cleaning with compressed nitrogen.
3. the preparation method of used by dye sensitization solar battery porous titanium dioxide thin-film as claimed in claim 2, its feature
It is：The organic solvent is one kind in isopropanol, alcohol, chloroform or acetone.
4. the preparation method of used by dye sensitization solar battery porous titanium dioxide thin-film as claimed in claim 1, its feature
It is：Dihydric alcohol is one kind in ethylene glycol, propane diols or butanediol in the step A3；Polyalcohol is glycerine, three hydroxyl first
One kind in base ethane, pentaerythrite, xylitol or sorbierite.
5. the preparation method of used by dye sensitization solar battery porous titanium dioxide thin-film as claimed in claim 1, its feature
It is：The titaniferous Organic inorganic film thickness increase that each deposition cycle makes to obtain in the step A3 is 0.06-
0.12nm。
6. the preparation method of used by dye sensitization solar battery porous titanium dioxide thin-film as claimed in claim 1, its feature
It is：Repeat step A2-A3 deposition cycle 1000-10000 times in the step A4.
7. the preparation method of used by dye sensitization solar battery porous titanium dioxide thin-film as claimed in claim 1, its feature
It is：Described base material is silica electro-conductive glass, indium tin oxide electro-conductive glass, the zinc oxide for mixing aluminium of doping fluorine
One kind in electro-conductive glass, monocrystalline silicon piece, copper foil or non-woven fabrics.
8. the preparation method of used by dye sensitization solar battery porous titanium dioxide thin-film as claimed in claim 1, its feature
It is：Heat treatment is carried out in air, oxygen or inert atmosphere in the step B.
9. the preparation method of used by dye sensitization solar battery porous titanium dioxide thin-film as claimed in claim 1, its feature
It is：The specific surface area that porous titanium dioxide thin-film is obtained in the step B is 60-400m2/ g, pore scale is in 8~10nm.
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| CN110512189A (en) * | 2019-06-14 | 2019-11-29 | 邱越 | A kind of aperture adjustable porous metal oxide preparation method based on molecular-layer deposition |
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| CN101752093A (en) * | 2010-02-26 | 2010-06-23 | 上海交通大学 | Preparation method for photonic crystal structure film electrode of dye solar cell |
| CN101779258A (en) * | 2007-07-25 | 2010-07-14 | 聚合物华润有限公司 | Solar cell and method for preparation thereof |
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| CN101779258A (en) * | 2007-07-25 | 2010-07-14 | 聚合物华润有限公司 | Solar cell and method for preparation thereof |
| CN101752093A (en) * | 2010-02-26 | 2010-06-23 | 上海交通大学 | Preparation method for photonic crystal structure film electrode of dye solar cell |
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