CN106711337A - Preparation method of gold/TiO2 composite nanometer film and application of gold/TiO2 composite nanometer film - Google Patents

Preparation method of gold/TiO2 composite nanometer film and application of gold/TiO2 composite nanometer film Download PDF

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CN106711337A
CN106711337A CN201710075198.3A CN201710075198A CN106711337A CN 106711337 A CN106711337 A CN 106711337A CN 201710075198 A CN201710075198 A CN 201710075198A CN 106711337 A CN106711337 A CN 106711337A
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gold
tio
film
preparation
composite nano
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CN106711337B (en
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江林
梁志强
邵卫晶
文鹏
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Suzhou University
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/80—Constructional details
    • H10K30/81—Electrodes
    • 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
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K2102/00—Constructional details relating to the organic devices covered by this subclass
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/549—Organic PV cells

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  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
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  • Electromagnetism (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
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  • Inorganic Compounds Of Heavy Metals (AREA)
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Abstract

The invention relates to a preparation method of a gold/TiO2 composite nanometer film and an application of the gold/TiO2 composite nanometer film. The preparation method comprises the following steps of (a) dissolving chloroauric acid in a solvent so as to prepare a reaction solution; (b) preparing a TiO2 nanometer film; (c) putting a substrate on which the TiO2 nanometer film is formed into the reaction solution for reaction under ultrasonic conditions; (d) washing products of the step (c) with deionized water, and then blow-drying. Gold nanoparticles can grow on the surface of the TiO2 nanometer film under the ultrasonic conditions, and the preparation method has the advantages of simplicity, convenience, easiness in implementation, good repeatability, no toxicity and no pollution of the reaction solution and the like; the size and density of the gold nanoparticles can be adjusted and controlled by adjusting the concentration and growth time of the chloroauric acid; by adopting the gold/TiO2 composite nanometer film, the performance of a polymer solar cell can be effectively improved.

Description

A kind of gold/TiO2The preparation method and gold/TiO of composite nano film2Composite Nano is thin The application of film
Technical field
The invention belongs to field of nanometer material technology, it is related to a kind of method in nano thin-film superficial growth golden nanometer particle, has Body is related to a kind of gold/TiO2The preparation method and gold/TiO of composite nano film2The application of composite nano film.
Background technology
Surface plasma bulk optics proposes that, in nanoscale upper-pilot and control photon, this is the nanometer of development higher performance Photoelectric device provides a new effective way.Golden nanometer particle 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 have impact on absorption of the battery to incident light.How to avoid because of the electronics and sky that active layer thickness increase causes The interior of cave is combined, and further improves battery performance, the emphasis of the concern as domestic and international researcher, and constantly makes progress.
Active layer in polymer solar battery is to play the work(for absorbing incident light energy and producing electron-hole pair Ergosphere, therefore the essence of enhancing battery light absorbs is the light absorbs for strengthening active layer；And golden nanometer particle is placed directly within PSC's The near field enhancement effect that in active layer its surface plasma resonance can produce is distributed in active layer, can more effectively strengthen work Property layer light absorbs.In general, it is following two to add the method for PSC active layers mainly to include golden nanometer particle：One kind is Golden nanometer particle is first synthesized using liquid phase method, then it is separated and be dispersed in active layer solution from solution again, then The active layer for being mixed with golden nanometer particle is prepared by the method for spin coating；Another kind is in buffering substrate by the way of vacuum evaporation Or active layer surface Direct precipitation golden nanometer particle.The technological process of former approach is complicated, and golden nanometer particle is adding work Property layer solution and spin-coating film during easily there is agglomeration.This agglomeration not only weakens its surface plasma Resonance effects, and the structure of active layer can be destroyed, it is unfavorable for lifting battery performance.Later approach needs valuable deposition to set Standby, harsh depositional environment, energy resource consumption is big, with high costs.
The content 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.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：A kind of gold/TiO2The preparation side of composite nano film Method, it is characterised in that it is comprised the following steps：
A be dissolved in gold chloride in solvent and be configured to reaction solution by ()；
B () will be formed with TiO2The substrate of nano thin-film is placed in the reaction solution, be placed under ultrasound condition carry out it is anti- Should；
C () dries up after the product deionized water rinsing of step (b).
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 its 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 is comprised the following steps：
(1) TiO is taken2Presoma is added in alcohols solvent, stirs to obtain vitreosol；
(2) vitreosol is spin-coated on the ito glass surface processed through oxygen plasma, after heat treatment.
Further, the TiO2Presoma is double (levulinic ketone group) diisopropyl titanate esters, and the alcohols solvent is N-butanol.
Further, the ito glass is first using weakly alkaline washing agent, water, acetone successively through oxygen plasma before processing It is cleaned by ultrasonic with isopropanol.
Further, the heat treatment is the first heating removing alcohols solvent, then in 300~500 DEG C of heating.
A further object of the present invention is to provide a kind of above-mentioned gold/TiO2Composite nano film is in polymer solar battery In application, in the 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.
Because above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：Gold/TiO of the present invention2It is multiple The preparation method of nano thin-film is closed, there can be good dispersion in titanium dioxide nano-film superficial growth under ultrasound condition Golden nanometer particle, have the advantages that simple and easy to do, reproducible and reaction solution is nontoxic, pollution-free；Can be by regulation The concentration and growth time of gold chloride, regulate and control the size and density of golden nanometer particle；Such gold/TiO2Composite nano film can Effectively strengthen the performance of polymer solar battery.
Brief description of the drawings
Accompanying drawing 1 is the SEM figures of nano material in embodiment 1：(a)TiO2The SEM figures of nano thin-film, (b) is combined gold nano The TiO of particle2Nano thin-film SEM figures (engineer's scale of illustration is 100nm in b)；
The composite Ti O obtained in present invention reaction different time of accompanying drawing 22The SEM figures of nano thin-film：(a) 0.5 hour (reality Apply example 2), (b) 1 hour (embodiment 1), (c) 1.5 hours (embodiment 3)；
Accompanying drawing 3 is gold/TiO of the present invention2The application of composite nano film：Gold/the TiO of (a) containing golden nanometer particle2It is compound The polymer solar battery structural representation of nano thin-film；The schematic diagram of (b) polymer solar battery；
Accompanying drawing 4 is that (engineer's scale of illustration is for golden nanometer particle SEM figures in embodiment 4 after depositing Ti O2 protective layers 100nm)；
Accompanying drawing 5 is J-V curves 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 is comprised the following steps：A be dissolved in for gold chloride molten by () Reaction solution is configured in agent；B () will be formed with the substrate of titanium dioxide nano-film and be placed in the reaction solution, be placed in super Reacted under the conditions of sound；C () dries up after the product deionized water rinsing of step (b).Under ultrasound condition In titanium dioxide nano-film superficial growth golden nanometer particle, with simple and easy to do, reproducible and reaction solution is nontoxic, nothing The advantages of pollution；And the particle diameter distribution of golden nanometer particle is about 20~100nm, soilless sticking and favorable dispersibility.And 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 preferably described ultrasound is 50~150W, and frequency is 50~100KHz) etc., regulates and controls golden nanometer particle Size and density；Such gold/TiO2Composite nano film can effectively strengthen the performance of polymer solar battery.It is described molten Agent is preferably the mixed liquor of second alcohol and water, and its volume ratio is 1：0.1~10, it is optimal for volume ratio is 1：1, now gold chloride is molten The wettability of solution property and substrate is best.
Above-mentioned TiO2The preparation method of nano thin-film is comprised the following steps：(1) TiO is taken2Presoma is added in alcohols solvent, Stir to obtain vitreosol；(2) vitreosol is spin-coated on the ito glass surface processed through oxygen plasma, after heat treatment .Using nano thin-film surface compact obtained in the method, it is smooth, without hole.TiO2Presoma and alcohols solvent are using normal Rule, can select：TiO2Presoma is double (levulinic ketone group) diisopropyl titanate esters, and alcohols solvent is n-butanol. Ito glass is preferably first carrying out ultrasound clearly with weakly alkaline washing agent, water, acetone and isopropanol successively through oxygen plasma before processing Wash.The heat treatment first to remove alcohols solvents in 100~180 DEG C of heating, then 300~500 DEG C of heating (usually 10~ 40 minutes) treatment.
Gold/TiO obtained in the above method2Composite nano film delays in can be applicable to polymer solar battery as negative electrode Layer is rushed, specially：In the 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, the directly contact for avoiding active layer and golden nanometer particle causes electronic quenching effect, improves poly- The short circuit current of compound solar cell, fill factor, curve factor and electricity conversion.
The present invention is further described below in conjunction with accompanying drawing embodiment.
Embodiment 1
The present embodiment provides a kind of gold/TiO2The preparation method of composite nano film, it is comprised the following steps：
A () is 1 in volume ratio:The gold chloride for adding appropriate concentration to be 10mM in 1 water and alcohol mixed solution, is configured to Concentration is the reaction solution of 0.5mM；
B () (1) compound concentration is 0.5mol/L TiO2Colloidal sol：N-butanol 7.5ml addition storage bottles are taken, addition concentration is Double (levulinic ketone group) diisopropyl titanate esters 2.5ml of 2mol/L, then 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：Take appropriate TiO2Colloidal sol drop is overlayed on through alkalescent cleaning agent (Micro-90), surpassed Pure water, acetone and isopropanol are cleaned by ultrasonic and with the ITO surfaces after oxygen plasma treatment, are revolved with the rotating speed of 3000rmp/min Apply 30s and obtain uniform wet film；Then wet film is toasted into 10min at 150 DEG C, then is heat-treated half an hour at 380 DEG C and obtained final product To TiO2Nano thin-film, its SEM figures are as shown in Fig. 1 (a).It can be seen that, TiO2Nano thin-film surface compact, it is smooth, without hole.
C () will be formed with TiO2The substrate of nano thin-film is vertically placed in reaction solution, then will fill the reaction solution Container sealing after be placed in power for 100W, frequency for 80KHz supersonic generator in react 1 hour；Then taking out should ITO/TiO2Substrate, is rinsed well with deionized water, uses N2Air-blowing is done, you can obtaining superficial growth has the TiO of golden nanometer particle2 Nano thin-film, its SEM figures are as shown in Fig. 1 (b).It can be seen that, in TiO2The surface of film, the particle diameter distribution of golden nanometer particle 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 process and embodiment 1 It is basically identical, unlike：In step (c), power is placed in after the container sealing for filling reaction solution for 100W, frequency are Reacted 0.5 hour in the supersonic generator of 80KHz, its SEM figures are 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 process and embodiment 1 It is basically identical, unlike：In step (c), power is placed in after the container sealing for filling reaction solution for 100W, frequency are Reacted 1.5 hours in the supersonic generator of 80KHz, its SEM figures are as shown in Fig. 2 (c).Result shows, by extending during reaction Between can increase the size of golden nanometer particle.
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.By the 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)).It is inverted The preparation technology flow of type polymer solar battery is specially：
(1) active layer solution is prepared：Appropriate P3HT and PCBM is weighed, with 1,2- dichloro-benzenes for solvent, compound concentration is 20mgml-1P3HT and concentration 20mg ml-1PCBM mixed solutions；By P3HT：PCBM mixed solutions are heated at 70 DEG C Stirring more than 2 hours, then with 0.2 μm of organic phase filter filtration treatment；
(2) using the method for ald, in gold/TiO2Composite nano film surface deposited one layer it is ultra-thin (about Thickness is 10nm) TiO2As protective layer (as shown in Figure 4), for avoiding active layer from causing with golden nanometer particle directly contact Electronic quenching effect.
(3) spin coating active layer：In TiO2(growth has the TiO of golden nanometer particle to film surface in embodiment 12Nano thin-film) Drop covers appropriate P3HT/PCBM mixed solutions, and battery-active layer is obtained with the rotating speed spin coating 30s of 700rmp；
(4) active layer post processing：First to P3HT：PCBM active layers carry out ambient solvent annealing, then at 120 DEG C Lower annealing, finally scrapes cell cathode；
(5) it is deposited with MoO3Layer：It is 1 × 10 in vacuum using thermal evaporation vacuum coating equipment-4Evaporation is thick in the vacuum chamber of Pa Spend the MoO of about 10nm3Anode buffer layer, evaporation rate is about
(6) Ag electrodes are deposited with：It is 1 × 10 in vacuum using thermal evaporation vacuum coating equipment-4Evaporation is thick in the vacuum chamber of Pa The Ag electrodes of about 100nm are spent, evaporation rate is about
The bill of materials used in the embodiment 4 of table 1
Reagent, medicine 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 TiO2It is basically identical in the application of nano thin-film, its preparation process and embodiment 4, it is different It is：Using the TiO used in embodiment 12Nano thin-film, but not load gold nano particle.
The test of polymer solar battery：Carried out in air ambient, use the Newport through AM1.5 filters Used as simulated solar spectrum radiation source, irradiation intensity is 100mW cm to 91160 sun simulating light sources (300W)-2.Use The test cells of Keithley 2400 carry out data acquisition and calculate (to ensure the accuracy of test result, to be used before test The calibration light source intensity of Newport Si batteries 91150, and adjust sample centering), specific test data is shown in Table 2.
TiO in the embodiment 4 of table 2 and comparative example 12The test data table of polymer solar battery obtained in 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/the TiO in embodiment 12Composite nano film) organic solar batteries J-V curves.It can be seen that, adopt With ultrasonic wave added method in TiO2Nano thin-film surface prepares golden nanometer particle and can effectively improve the performance of polymer solar battery. The lifting of battery PCE is mostly derived from short circuit current (JSC) and fill factor, curve factor (FF) lifting.Short circuit current (JSC) lifting come from The surface plasmon resonance effect and scattering effect of various sizes of golden nanometer particle enhance the light absorbs level of battery, enter And increased the photogenerated current of battery.The lifting of fill factor, curve factor (FF) comes from golden nanometer particle to TiO2Nano thin-film electric property Improvement.
The above embodiments merely illustrate the technical concept and features of the present invention, its object is to allow person skilled in the art Scholar will appreciate that present disclosure and implement according to this that it is not intended to limit the scope of the present invention, all according to the present invention The equivalent change or modification that Spirit Essence is made, should all be included within the scope of the present invention.

Claims (10)

1. a kind of gold/TiO2The preparation method of composite nano film, it is comprised the following steps：
（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；
（c）By step（b）Product deionized water rinsing after, drying.
2. gold/TiO according to claim 12The preparation method of composite nano film, it is characterised in that：In the reaction solution The concentration of gold chloride is 0.1 ~ 5mmol/L.
3. gold/TiO according to claim 12The preparation method of composite nano film, it is characterised in that：The solvent is ethanol With the mixed liquor of water, its volume ratio is 1：0.1~10.
4. gold/TiO according to claim 12The preparation method of composite nano film, it is characterised in that：The power of the ultrasound It is 50 ~ 150W, frequency is 50 ~ 100KHz, and the reaction time is 0.5 ~ 1.5 hour.
5. TiO according to claim 12The preparation method of nano thin-film, it is characterised in that step（b）In, the titanium dioxide The preparation method of titanium nano thin-film is comprised the following steps：
（1）Take TiO2Presoma is added in alcohols solvent, stirs to obtain vitreosol；
（2）The vitreosol is spin-coated on the ito glass surface processed through oxygen plasma, after heat treatment.
6. TiO according to claim 52The preparation method of nano thin-film, it is characterised in that：The TiO2Presoma is double（Second Acyl acetonyl）Diisopropyl titanate esters, the alcohols solvent is n-butanol.
7. TiO according to claim 52The preparation method of nano thin-film, it is characterised in that：The ito glass through oxygen etc. from Daughter before processing is first cleaned by ultrasonic with weakly alkaline washing agent, water, acetone and isopropanol successively.
8. TiO according to claim 52The preparation method of nano thin-film, it is characterised in that：The heat treatment is removed for first heating The alcohols solvent is removed, then in 300 ~ 500 DEG C of heating.
9. a kind of gold/TiO2Application of the composite nano film in polymer solar battery, it is characterised in that：In ito glass table Gold/the TiO in face2Active layer, anode buffer layer and electrode layer are sequentially formed on composite nano film and obtains the inversion type polymer sun Can battery.
10. gold/TiO according to claim 92Application of the composite nano film in polymer solar battery, its feature exists In：In the gold/TiO2TiO is also formed between composite nano film and the active layer2Protective layer.
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CN108767113A (en) * 2018-05-07 2018-11-06 苏州大学 A kind of TiO2Nano-pillar-Au Nanocomposites array, preparation method and applications
CN113649584A (en) * 2020-11-06 2021-11-16 武汉大学 Growth method of laser-induced morphology-controllable gold or gold composite nanostructure and application thereof

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CN108767113A (en) * 2018-05-07 2018-11-06 苏州大学 A kind of TiO2Nano-pillar-Au Nanocomposites array, preparation method and applications
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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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