CN106711337B - A kind of gold/TiO2The application of composite nano film - Google Patents
A kind of gold/TiO2The application of composite nano film Download PDFInfo
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- H—ELECTRICITY
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- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
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- H10K30/82—Transparent electrodes, e.g. indium tin oxide [ITO] electrodes
- H10K30/83—Transparent electrodes, e.g. indium tin oxide [ITO] electrodes comprising arrangements for extracting the current from the cell, e.g. metal finger grid systems to reduce the serial resistance of transparent electrodes
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Abstract
The present invention relates to a kind of gold/TiO2The preparation method and gold/TiO of composite nano film2The application of composite nano film, it is configured to reaction solution the following steps are included: gold chloride is dissolved in solvent by (a)；(b) TiO is prepared2Nano thin-film;(c) TiO will be formed with2The substrate of nano thin-film is placed in the reaction solution, is placed under ultrasound condition and is reacted；(d) after the product of step (c) being rinsed with deionized water, drying.It can be in TiO under ultrasound condition2Nano thin-film surface grows gold nanoparticle, has many advantages, such as that simple and easy to do, reproducible and reaction solution is nontoxic, pollution-free；The size and density of gold nanoparticle can be regulated and controled by the concentration and growth time of adjusting gold chloride；Such gold/TiO2Composite nano film can effectively enhance the performance of polymer solar battery.
Description
Technical field
The invention belongs to field of nanometer material technology, are related to a kind of method in nano thin-film surface growth gold nanoparticle, tool
Body is related to a kind of gold/TiO2The preparation method and gold/TiO of composite nano film2The application of composite nano film.
Background technique
Surface plasma bulk optics propose the manipulation on nanoscale and control photon, this is the nanometer for developing higher performance
Photoelectric device provides a new effective way.Gold nanoparticle due to unique surface plasmon resonance effect,
It is set to be with a wide range of applications and prospect in the aspect of performance of enhancing nano photoelectric device.To polymer solar battery
(PSC) for, the organic semiconducting materials for constituting bulk-heterojunction active layer limit activity because its carrier mobility is low
The thickness of layer, and then affect absorption of the battery to incident light.Electronics and sky caused by how avoiding because of active layer thickness increase
Cave it is interior compound, further increase battery performance, become the emphasis of the concern of domestic and international researcher, and constantly make progress.
Active layer in polymer solar battery is to play the function for absorbing incident laser energy and generating electron-hole pair
Ergosphere, therefore the essence for enhancing battery light absorption is to enhance the light absorption of active layer；And gold nanoparticle is placed directly within PSC's
The near field enhancement effect that in active layer its surface plasma resonance can generate is distributed in active layer, can more effectively enhance work
The light absorption of property layer.In general, the method that PSC active layer is added in gold nanoparticle mainly includes following two: one is
Gold nanoparticle is first synthesized using liquid phase method, then again by it from separating and be dispersed in active layer solution in solution, then
The active layer of gold nanoparticle is mixed with by the method preparation of spin coating；Another kind is by the way of vacuum evaporation in buffering substrate
Or active layer surface Direct precipitation gold nanoparticle.The process flow of former approach is complicated, and work is being added in gold nanoparticle
Property layer solution and spin-coating film during agglomeration easily occurs.This agglomeration not only weakens its surface plasma
Resonance effects, and the structure of active layer can be destroyed, it is unfavorable for promoting battery performance.Later approach needs valuable deposition to set
Standby, harsh depositional environment, energy consumption is big, with high costs.
Summary of the invention
A kind of gold/TiO is provided the invention aims to overcome the deficiencies in the prior art2The preparation of composite nano film
Method.
In order to achieve the above objectives, the technical solution adopted by the present invention is that: a kind of gold/TiO2The preparation side of composite nano film
Method, which is characterized in that it the following steps are included:
(a) gold chloride is dissolved in solvent and is configured to reaction solution；
(b) TiO will be formed with2The substrate of nano thin-film is placed in the reaction solution, is placed under ultrasound condition and is carried out instead
It answers；
(c) after the product of step (b) being rinsed with deionized water, drying.
Optimally, the concentration of gold chloride is 0.1~5mmol/L in the reaction solution.
Optimally, the solvent is the mixed liquor of second alcohol and water, and volume ratio is 1:0.1~10.
Optimally, the power of the ultrasound is 50~150W, and frequency is 50~100KHz, and the reaction time is 0.5~1.5 small
When.
Optimally, in step (b), the preparation method of the titanium dioxide nano-film the following steps are included:
(1) TiO is taken2Presoma is added in alcohols solvent, stirs to obtain vitreosol；
(2) vitreosol is spin-coated on the ito glass surface through oxygen plasma treatment, after heat treatment.
Further, the TiO2Presoma is bis- (levulinic ketone group) diisopropyl titanate esters, and the alcohols solvent is
N-butanol.
Further, the ito glass first successively uses weakly alkaline washing agent, water, acetone before through oxygen plasma treatment
It is cleaned by ultrasonic with isopropanol.
Further, the heat treatment removes the alcohols solvent for first heating, then heats at 300~500 DEG C.
Another object of the present invention is to provide a kind of above-mentioned gold/TiO2Composite nano film is in polymer solar battery
In application, gold/TiO on ito glass surface2Active layer, anode buffer layer and electrode are sequentially formed on composite nano film
Layer obtains inversion type polymer solar battery.
Optimally, in the gold/TiO2TiO is also formed between composite nano film and the active layer2Protective layer.
Due to the above technical solutions, the present invention has the following advantages over the prior art: gold/TiO of the present invention2It is multiple
The preparation method for closing nano thin-film, can grow on titanium dioxide nano-film surface under ultrasound condition has good dispersion
Gold nanoparticle, have many advantages, such as that simple and easy to do, reproducible and reaction solution is nontoxic, pollution-free；Adjusting can be passed through
The concentration and growth time of gold chloride regulate and control the size and density of gold nanoparticle；Such gold/TiO2Composite nano film can
The effectively performance of enhancing polymer solar battery.
Detailed description of the invention
Attached drawing 1 is the SEM figure of nano material in embodiment 1: (a) TiO2The SEM of nano thin-film schemes, (b) compound gold nano
The TiO of particle2Nano thin-film SEM figure (scale bar of illustration is 100nm in b)；
Attached drawing 2 is composite Ti O made from present invention reaction different time2The SEM of nano thin-film schemes: (a) 0.5 hour (real
Apply example 2), (b) 1 hour (embodiment 1), (c) 1.5 hours (embodiment 3)；
Attached drawing 3 is gold/TiO of the present invention2The application of composite nano film: (a) gold/TiO containing gold nanoparticle2It is compound
The polymer solar battery structural schematic diagram of nano thin-film；(b) schematic diagram of polymer solar battery；
Attached drawing 4 is that (scale bar of illustration is for gold nanoparticle SEM figure in embodiment 4 after depositing Ti O2 protective layer
100nm)；
Attached drawing 5 is J-V curve when nano thin-film is applied to polymer solar battery in embodiment 1 and comparative example 1.
Specific embodiment
Gold/TiO of the present invention2The preparation method of composite nano film, it the following steps are included: (a) gold chloride is dissolved in it is molten
Reaction solution is configured in agent；(b) substrate for being formed with titanium dioxide nano-film is placed in the reaction solution, is placed in super
It is reacted under the conditions of sound；(c) after the product of step (b) being rinsed with deionized water, drying.Under ultrasound condition
Gold nanoparticle is grown on titanium dioxide nano-film surface, the nontoxic, nothing with simple and easy to do, reproducible and reaction solution
The advantages that pollution；And the particle diameter distribution of gold nanoparticle is about 20~100nm, soilless sticking and favorable dispersibility.And it can be with
By adjust the concentration (preferably 0.1~5mmol/L) of gold chloride, growth time (preferably~0.5-1.5 hours minute) and
Ultrasonic power (power of the preferably described ultrasound is 50~150W, and frequency is 50~100KHz) etc., regulates and controls gold nanoparticle
Size and density；Such gold/TiO2Composite nano film can effectively enhance the performance of polymer solar battery.It is described molten
Agent is preferably the mixed liquor of second alcohol and water, and volume ratio is 1:0.1~10, and optimal be volume ratio is 1:1, and gold chloride is molten at this time
Solution property and the wettability of substrate are best.
Above-mentioned TiO2The preparation method of nano thin-film is the following steps are included: (1) takes TiO2Presoma is added in alcohols solvent,
Stir to obtain vitreosol；(2) vitreosol is spin-coated on the ito glass surface through oxygen plasma treatment, after heat treatment
?.Using nano thin-film surface compact made from this method, it is smooth, without hole.TiO2Presoma and alcohols solvent are using normal
Rule, can select: TiO2Presoma is bis- (levulinic ketone group) diisopropyl titanate esters, and alcohols solvent is n-butanol.
Ito glass is first successively carried out with weakly alkaline washing agent, water, acetone and isopropanol ultrasonic clear preferably before through oxygen plasma treatment
It washes.The heat treatment first to remove alcohols solvents in 100~180 DEG C of heating, then heated at 300~500 DEG C (usually 10~
40 minutes) processing.
Gold/TiO made from the above method2Composite nano film can be applicable to slow as cathode in polymer solar battery
Layer is rushed, specifically: gold/TiO on ito glass surface2Active layer, anode buffer layer and electricity are sequentially formed on composite nano film
Pole layer obtains inversion type polymer solar battery.In the gold/TiO2Between composite nano film and the active layer further preferably
It is formed with TiO2Protective layer improves poly- for avoiding the direct contact of active layer and gold nanoparticle from causing electronic quenching effect
Close short circuit current, fill factor and the incident photon-to-electron conversion efficiency of object solar battery.
Below in conjunction with figure embodiment, invention is further explained.
Embodiment 1
The present embodiment provides a kind of gold/TiO2The preparation method of composite nano film, it the following steps are included:
(a) gold chloride that appropriate concentration is 10mM is added in the water and alcohol mixed solution that volume ratio is 1:1, is configured to
Concentration is the reaction solution of 0.5mM；
(b) (1) compound concentration is 0.5mol/L TiO2Colloidal sol: taking n-butanol 7.5ml that storage bottle is added, and it is 2 that concentration, which is added,
Then bis- (levulinic ketone group) diisopropyl titanate esters 2.5ml of mol/L carry out magnetic agitation 1 hour or so i.e. at room temperature
Obtain pale yellow transparent colloidal sol；
(2) TiO is prepared2Nano thin-film: suitable TiO is taken2Colloidal sol drop overlays on through alkalescent cleaning agent (Micro-90), surpasses
Pure water, acetone and isopropanol ultrasonic cleaning and with the surface ITO after oxygen plasma treatment, are revolved with the revolving speed of 3000rmp/min
It applies 30s and obtains uniform wet film；Then wet film is toasted at 150 DEG C 10min, then be heat-treated half an hour at 380 DEG C to obtain the final product
To TiO2Nano thin-film, SEM figure is as shown in Fig. 1 (a).As it can be seen that TiO2Nano thin-film surface compact, it is smooth, without hole.
(c) TiO will be formed with2The substrate of nano thin-film is vertically placed in reaction solution, then will fill the reaction solution
Container sealing be placed in the supersonic generator that power is 100W, frequency is 80KHz and react 1 hour；Then taking out should
ITO/TiO2Substrate is rinsed well with deionized water, uses N2Air-blowing is dry, and the TiO that surface growth has gold nanoparticle can be obtained2
Nano thin-film, SEM figure is as shown in Fig. 1 (b).As it can be seen that in TiO2The surface of film, the particle diameter distribution of gold nanoparticle is about 20
In the range of~100nm, soilless sticking phenomenon between gold nano grain, favorable dispersibility.
Embodiment 2
The present embodiment provides a kind of gold/TiO2In the preparation method of composite nano film, its preparation step and embodiment 1
It is almost the same, unlike: in step (c), the container sealing for filling reaction solution is placed on that power is 100W, frequency is
It is reacted 0.5 hour in the supersonic generator of 80KHz, SEM figure is as shown in Fig. 2 (a).
Embodiment 3
The present embodiment provides a kind of gold/TiO2In the preparation method of composite nano film, its preparation step and embodiment 1
It is almost the same, unlike: in step (c), the container sealing for filling reaction solution is placed on that power is 100W, frequency is
It is reacted 1.5 hours in the supersonic generator of 80KHz, SEM figure is as shown in Fig. 2 (c).The results show that when by extending reaction
Between can increase the size of gold nanoparticle.
Embodiment 4
The present embodiment provides a kind of gold/TiO2The application of composite nano film uses gold/TiO2Composite nano film is real
Apply the gold/TiO prepared in example 12Composite nano film.Pass through gold/TiO on ito glass surface2On composite nano film successively
Form TiO2Protective layer, active layer, anode buffer layer and electrode layer obtain inversion type polymer solar battery (Fig. 3 (a)).?
Set the preparation process flow of type polymer solar battery specifically:
(1) it prepares active layer solution: weighing suitable P3HT and PCBM, with 1,2- dichloro-benzenes for solvent, compound concentration is
20mgml-1P3HT and concentration 20mg ml-1PCBM mixed solution；P3HT:PCBM mixed solution is heated at 70 DEG C
Stirring 2 hours or more, then with 0.2 μm of organic phase filter filtration treatment；
(2) method for using atomic layer deposition, in gold/TiO2Composite nano film surface deposited one layer it is ultra-thin (about
With a thickness of 10nm) TiO2As protective layer (as shown in Figure 4), cause for avoiding active layer from directly contacting with gold nanoparticle
Electronic quenching effect.
(3) spin coating active layer: in TiO2(growth has the TiO of gold nanoparticle to film surface in embodiment 12Nano thin-film)
Drop covers suitable P3HT/PCBM mixed solution, obtains battery-active layer with the revolving speed spin coating 30s of 700rmp；
(4) active layer post-processes: ambient solvent annealing is carried out to P3HT:PCBM active layer first, then 120
It is made annealing treatment at DEG C, finally scrapes cell cathode；
(5) MoO is deposited3Layer: using thermal evaporation vacuum coating equipment, is 1 × 10 in vacuum degree-4Vapor deposition is thick in the vacuum chamber of Pa
Spend the MoO of about 10nm3Anode buffer layer, evaporation rate is about
(6) Ag electrode is deposited: using thermal evaporation vacuum coating equipment, is 1 × 10 in vacuum degree-4Vapor deposition is thick in the vacuum chamber of Pa
The Ag electrode of about 100nm is spent, evaporation rate is about
The bill of materials used in 1 embodiment 4 of table
| Reagent, drug and title material | Specification | Manufacturer |
| 1,2 dichloro-benzenes | Anhydrous, 99% | Sigma-Aldrich |
| P3HT | EG | Rieke Metals |
| PCBM | ADS61BFB, 99.0% | American Dye Source |
| Molybdenum trioxide | 99.99% | Middle promise green wood |
| Silver | 99.99% | Middle promise green wood |
Comparative example 1
This comparative example provides TiO2The application of nano thin-film, preparation process with it is almost the same in embodiment 4, it is different
It is: uses TiO used in embodiment 12Nano thin-film, but not load gold nano particle.
The test of polymer solar battery: carrying out in air environment, uses the Newport through AM1.5 optical filter
91160 sun simulating light sources (300W) are used as simulated solar spectrum radiation source, and irradiation intensity is 100mW cm-2.It uses
2400 test cell of Keithley carries out data acquisition and calculates (for the accuracy for guaranteeing test result, to use before testing
91150 calibration light source intensity of Newport Si battery, and adjust sample centering), specific test data is shown in Table 2.
TiO in 2 embodiment 4 of table and comparative example 12The test data table of polymer solar battery made from nano thin-film
Fig. 5 is based on TiO2Reference cell (the TiO in embodiment 1 of nano thin-film2Nano thin-film) and based on gold/TiO2
Composite nano film (gold/TiO in embodiment 12Composite nano film) organic solar batteries J-V curve.As it can be seen that adopting
With ultrasonic wave added method in TiO2Nano thin-film surface, which prepares gold nanoparticle, can effectively improve the performance of polymer solar battery.
The promotion of battery PCE is mostly derived from short circuit current (JSC) and fill factor (FF) promotion.Short circuit current (JSC) promotion be derived from
The light absorption that the surface plasmon resonance effect and scattering effect of various sizes of gold nanoparticle enhance battery is horizontal, into
And increase the photogenerated current of battery.The promotion of fill factor (FF) is derived from gold nanoparticle to TiO2Nano thin-film electric property
Improvement.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention, it is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (4)
1. a kind of gold/TiO2Application of the composite nano film in polymer solar battery, it is characterised in that: the gold/TiO2
The preparation method of composite nano film, it the following steps are included:
(a) gold chloride is dissolved in solvent and is configured to reaction solution；
(b) TiO will be formed with2The substrate of nano thin-film is placed in the reaction solution, is placed under ultrasound condition and is reacted；Institute
The preparation method of titanium dioxide nano-film is stated the following steps are included: (1) takes TiO2Presoma is added in alcohols solvent, stirs
Vitreosol；(2) vitreosol is spin-coated on the ito glass surface through oxygen plasma treatment, after heat treatment；Institute
State TiO2Presoma is bis- (levulinic ketone group) diisopropyl titanate esters, and the alcohols solvent is n-butanol；The ito glass exists
Through being first successively cleaned by ultrasonic with weakly alkaline washing agent, water, acetone and isopropanol before oxygen plasma treatment；The heat treatment
The alcohols solvent is removed first to heat, is then heated at 300~500 DEG C；
(c) after the product of step (b) being rinsed with deionized water, drying；Gold/TiO on ito glass surface2Composite Nano
Active layer, anode buffer layer and electrode layer are sequentially formed on film obtains inversion type polymer solar battery；In the gold/TiO2
TiO is also formed between composite nano film and the active layer2Protective layer, the gold/TiO2Composite nano film is slow for cathode
Rush layer.
2. gold/TiO according to claim 12Application of the composite nano film in polymer solar battery, feature exist
In: the concentration of gold chloride is 0.1~5mmol/L in the reaction solution.
3. gold/TiO according to claim 12Application of the composite nano film in polymer solar battery, feature exist
In: the solvent is the mixed liquor of second alcohol and water, and volume ratio is 1:0.1~10.
4. gold/TiO according to claim 12Application of the composite nano film in polymer solar battery, feature exist
In: the power of the ultrasound is 50~150W, and frequency is 50~100KHz, and the reaction time is 0.5~1.5 hour.
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| CN113649584B (en) * | 2020-11-06 | 2022-06-10 | 武汉大学 | Growth method of laser-induced morphology-controllable gold or gold composite nanostructure and application thereof |
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