CN102522463A - Preparation method of poly(5-trifluoromethyl-1,3-phenylenediamine)/laminar platinum particula film - Google Patents

Preparation method of poly(5-trifluoromethyl-1,3-phenylenediamine)/laminar platinum particula film Download PDF

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CN102522463A
CN102522463A CN2012100085759A CN201210008575A CN102522463A CN 102522463 A CN102522463 A CN 102522463A CN 2012100085759 A CN2012100085759 A CN 2012100085759A CN 201210008575 A CN201210008575 A CN 201210008575A CN 102522463 A CN102522463 A CN 102522463A
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film
phenylenediamine
trifluoromethyl
platinum
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CN102522463B (en
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牛海军
郝丽苹
张琳
白续铎
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Heilongjiang University
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Abstract

The invention provides a preparation method of a poly(5-trifluoromethyl-1,3-phenylenediamine)/laminar platinum particula film, relating to a preparation method of a platinum particula film and aiming to solve the problem that the cost is high by using a platinum electrode as a counter electrode in the prior art. The preparation method for the poly(5-trifluoromethyl-1,3-phenylenediamine)/laminar platinum particula film is as follows: 1, ultrasonically washing conducting glass; 2, processing a pure platinum sheet; 3, carrying out electro-chemical polymerization by using cyclic voltammetry; and 4, immersing into chloro-platinic acid, and obtaining the poly(5-trifluoromethyl-1,3-phenylenediamine)/laminar platinum particula film by using the cyclic voltammetry. The poly(5-trifluoromethyl-1,3-phenylenediamine)/laminar platinum particula film prepared with the preparation method provided by the invention is used as a counter electrode of a dye-sensitized solar cell, and has the effects of low platinum carrying quantity and strong catalytic activity compared with a platinized electrode based on pyrolysis. The method provided by the invention is applied to the field of solar cells.

Description

The preparation method of a kind of gathering (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film
Technical field
The present invention relates to a kind of preparation method of platinum grain bulbec film.
Background technology
Since O ' Regan and Gratzel have reported that in 1991 high relatively solar energy converting efficient is 8%～11% DSSC (DSSC), DSSCs has caused the interest of Science and Technology widely.DSSCs is because its high conversion efficiency and low cost have become one of the most promising photovoltaic device.In general, DSSC comprises three major parts compositions: the transparent conducting glass substrate of the nano-crystalline titanium dioxide film of a dyestuff covering, I -/ I 3 -Organic solvent as electrolyte and one to electrode.High electrochemical activity be an essential condition that strengthens the DSSC performance to electrode, it is mainly used in the collection electronics, also having a main effect is catalytic action, accelerates I -/ I 3 -And the electron exchange speed between the cathode electronics, therefore need carry out modification, to improve its catalytic performance to electrode.The main at present method of modifying that adopts is that platinum is modified, and has the electro-conductive glass of platinum catalyst to constitute by load usually, and platinum can make the charge migration on the electrode and electrolyte liquor interface is rapidly and efficiently carried out, and suppresses dark current, improves the open circuit voltage of battery.But the costliness of platinum and rare causes the kind electrode preparation cost higher.Polyaniline and derivative thereof are because it is prone to syntheticly, and high conductivity and unique redox property are as being one of very potential conducting polymer to electrode.
Summary of the invention
The objective of the invention is in order to solve existing platinum electrode as to the high problem of electrode cost, and provide a kind of and gather the preparation method of (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film.
The preparation method of a kind of gathering of the present invention (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film carries out according to following steps:
One, electro-conductive glass is immersed in the water, sonicated 10～20min takes out water then and cleans 1～2 time; Electro-conductive glass after the above-mentioned cleaning is immersed in the acetone soln, and sonicated 10～20min takes out water then and cleans 1～2 time; Immerse in the distilled water sonicated 10～20min, dry 0.5～2min under 50 ℃～80 ℃ temperature then again; Wherein, the supersonic frequency of sonicated is 40～50KHz;
Two, get pure platinized platinum and put into red fuming nitric acid (RFNA), be heated to the boiling back and keep 1～3min, be cooled to room temperature then, for use;
Three, with the electro-conductive glass after step 1 is handled as work electrode, as to electrode, other gets the Ag/AgCl electrode as reference electrode with the pure platinized platinum handled through step 2; Place electrolyte; Using cyclic voltammetry, is-0.5～1.8V at voltage, and sweep speed is 15～25mV/s -1, the voltage cycle number of times is under 55 times the condition, to carry out electrochemical polymerization, promptly gets and gathers (5-Trifluoromethyl-1,3-phenylenediamine) film;
Four, gather (5-Trifluoromethyl-1 with what step 3 obtained; The 3-phenylenediamine) film is a work electrode, and as to electrode, other gets the Ag/AgCl electrode as reference electrode with the pure platinized platinum handled through step 2; Place electrolyte B; Using cyclic voltammetry, is-0.5～1.8V at voltage, and sweep speed is 15～25mV/s -1, the voltage cycle number of times is under 10～40 times the condition, to carry out electrochemical polymerization, promptly gets and gathers (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film; Wherein, the 5-Trifluoromethyl-1 that the described electrolyte A of step 3 is 0.1～0.5mol/L, the sulfuric acid solution of 3-phenylenediamine; The platinum solution chlorate that the described electrolyte B of step 4 is 0.001～0.01mol/L.
Beneficial effect of the present invention is: synthesized through electrochemical method and gathered (5-Trifluoromethyl-1,3-phenylenediamine) film, and be that substrate induction forms lamella globular platinum particle membrane with this polyaniline film.Gather (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film as DSSC to electrode, have with respect to the pyrolysismethod platinum plating that to carry the platinum amount low, the effect that catalytic activity is strong.
Description of drawings
Fig. 1 tests the Pt of the 5 pyrolysismethod preparations that obtain to electrode SEM pattern;
Fig. 2 test 1 obtain gather (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film SEM pattern;
Fig. 3 test 1 obtain gather the SEM pattern that (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film amplifies 80 times;
Fig. 4 test 2 obtain gather (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film SEM pattern;
Fig. 5 test 2 obtain gather the SEM pattern that (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film amplifies 80 times;
Fig. 6 test 3 obtain gather (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film SEM pattern;
Fig. 7 test 3 obtain gather the SEM pattern that (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film amplifies 80 times;
Fig. 8 test 4 obtain gather (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film SEM pattern;
Fig. 9 test 4 obtain gather the SEM pattern that (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film amplifies 80 times;
The Pt film of Figure 10 pyrolysismethod preparation and the different voltage-to-current curves that carry the thin polymer films conduct of platinum amount to electrode; Wherein, 1 voltage-to-current curve, 2 voltage-to-current curves, 3 voltage-to-current curves, 4 voltage-to-current curves, 5 voltage-to-current curves for test 5 for test 1 for test 2 for test 3 for test 4.
Embodiment
Technical scheme of the present invention is not limited to following cited embodiment, also comprises the combination in any between each embodiment.
Embodiment one: the preparation method of a kind of the gathering of this execution mode (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film carries out according to following steps:
One, electro-conductive glass is immersed in the water, sonicated 10～20min takes out water then and cleans 1～2 time; Electro-conductive glass after the above-mentioned cleaning is immersed in the acetone soln, and sonicated 10～20min takes out water then and cleans 1～2 time; Immerse in the distilled water sonicated 10～20min, dry 0.5～2min under 50 ℃～80 ℃ temperature then again; Wherein, the supersonic frequency of sonicated is 40～50KHz;
Two, get pure platinized platinum and put into red fuming nitric acid (RFNA), be heated to the boiling back and keep 1～3min, be cooled to room temperature then, for use;
Three, with the electro-conductive glass after step 1 is handled as work electrode, as to electrode, other gets the Ag/AgCl electrode as reference electrode with the pure platinized platinum handled through step 2; Place electrolyte; Using cyclic voltammetry, is-0.5～1.8V at voltage, and sweep speed is 15～25mV/s -1, the voltage cycle number of times is under 55 times the condition, to carry out electrochemical polymerization, promptly gets and gathers (5-Trifluoromethyl-1,3-phenylenediamine) film;
Four, gather (5-Trifluoromethyl-1 with what step 3 obtained; The 3-phenylenediamine) film is a work electrode, and as to electrode, other gets the Ag/AgCl electrode as reference electrode with the pure platinized platinum handled through step 2; Place electrolyte B; Using cyclic voltammetry, is-0.5～1.8V at voltage, and sweep speed is 15～25mV/s -1, the voltage cycle number of times is under 10～40 times the condition, to carry out electrochemical polymerization, promptly gets and gathers (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film; Wherein, the 5-Trifluoromethyl-1 that the described electrolyte A of step 3 is 0.1～0.5mol/L, the sulfuric acid solution of 3-phenylenediamine; The platinum solution chlorate that the described electrolyte B of step 4 is 0.001～0.01mol/L.
The beneficial effect of this execution mode is: synthesized through electrochemical method and gathered (5-Trifluoromethyl-1,3-phenylenediamine), and be that substrate induction forms lamella globular platinum particle membrane with this polyaniline film.Gather (5-Trifluoromethyl-1,3-phenylenediamine) platinum particles film as DSSC to electrode, have with respect to the pyrolysismethod platinum plating that to carry the platinum amount low, the effect that catalytic activity is strong.
Embodiment two: this execution mode and embodiment one are different: the described water of step 1 cleans and is meant with distilled water or deionized water and carries out.Other is identical with embodiment one.
Embodiment three: what this execution mode and embodiment one to two were different is: the described red fuming nitric acid (RFNA) of step 2 is that mass percentage content is 65%～68% nitric acid.Other is identical with embodiment one to two.
Embodiment four: what this execution mode was different with one of embodiment one to three is: the described voltage of step 3 and step 4 is direct voltage.Other is identical with one of embodiment one to three.
Through following verification experimental verification effect of the present invention:
Test 1
The preparation method of a kind of the gathering of this test (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film carries out according to following steps:
One, the FTO electro-conductive glass is immersed in the distilled water, sonicated 15min takes out with washed with de-ionized water 1 time then; FTO electro-conductive glass after the above-mentioned cleaning is immersed in the acetone soln, and sonicated 15min takes out with washed with de-ionized water 1 time then; Immerse in the distilled water sonicated 15min, dry 1min under 60 ℃ of temperature then again; Wherein, supersonic frequency 45KHz;
Two, getting pure platinized platinum, to put into mass percentage content be 65% salpeter solution, is heated to 83 ℃ and keeps 2min, is cooled to room temperature, for use;
Three, with the electro-conductive glass after step 1 is handled as work electrode; As to electrode, other gets the Ag/AgCl electrode as reference electrode, places the 5-Trifluoromethyl-1 of 0.3mol/L with the pure platinized platinum handled through step 2; In the sulfuric acid solution of 3-phenylenediamine; Using cyclic voltammetry, is 1V at direct voltage, and sweep speed is 20mV/s -1, the voltage cycle number of times is under 55 times the condition, to carry out electrochemical polymerization, promptly gets and gathers (5-Trifluoromethyl-1,3-phenylenediamine) film;
Four, gather (5-Trifluoromethyl-1 with what step 3 obtained; The 3-phenylenediamine) film is a work electrode, and as to electrode, other gets the Ag/AgCl electrode as reference electrode with the pure platinized platinum handled through step 2; Place the platinum solution chlorate of 0.003mol/L; Using cyclic voltammetry, is 1V at direct voltage, and sweep speed is 20mV/s -1, the voltage cycle number of times is under 10 times the condition, to carry out electrochemical polymerization, promptly gets and gathers (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film;
Five, (5-Trifluoromethyl-1,3-the phenylenediamine)/sheet platinum grain bulbec film that gathers that step 4 is obtained is put into vacuum drying chamber, is 70 ℃ in temperature, vacuum degree is-condition of 0.1MPa under oven dry 12h subsequent use.
Test 2
The preparation method of a kind of the gathering of this test (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film carries out according to following steps:
One, the FTO electro-conductive glass is immersed in the distilled water, sonicated 15min takes out with washed with de-ionized water 1 time then; FTO electro-conductive glass after the above-mentioned cleaning is immersed in the acetone soln, and sonicated 15min takes out with washed with de-ionized water 1 time then; Immerse in the distilled water sonicated 15min, dry 1min under 60 ℃ of temperature then again; Wherein, supersonic frequency 45KHz;
Two, getting pure platinized platinum, to put into mass percentage content be 65% salpeter solution, is heated to 83 ℃ and keeps 2min, is cooled to room temperature, for use;
Three, with the electro-conductive glass after step 1 is handled as work electrode; As to electrode, other gets the Ag/AgCl electrode as reference electrode, places the 5-Trifluoromethyl-1 of 0.3mol/L with the pure platinized platinum handled through step 2; In the sulfuric acid solution of 3-phenylenediamine; Using cyclic voltammetry, is 1V at direct voltage, and sweep speed is 20mV/s -1, the voltage cycle number of times is under 55 times the condition, to carry out electrochemical polymerization, promptly gets and gathers (5-Trifluoromethyl-1,3-phenylenediamine) film;
Four, gather (5-Trifluoromethyl-1 with what step 3 obtained; The 3-phenylenediamine) film is a work electrode, and as to electrode, other gets the Ag/AgCl electrode as reference electrode with the pure platinized platinum handled through step 2; Place the platinum solution chlorate of 0.003mol/L; Using cyclic voltammetry, is 1V at direct voltage, and sweep speed is 20mV/s -1, the voltage cycle number of times is under 20 times the condition, to carry out electrochemical polymerization, promptly gets and gathers (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film;
Five, (5-Trifluoromethyl-1,3-the phenylenediamine)/sheet platinum grain bulbec film that gathers that step 4 is obtained is put into vacuum drying chamber, is 70 ℃ in temperature, vacuum degree is-condition of 0.1MPa under oven dry 12h subsequent use.
Test 3
The preparation method of a kind of the gathering of this test (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film carries out according to following steps:
One, the FTO electro-conductive glass is immersed in the distilled water, sonicated 15min takes out with washed with de-ionized water 1 time then; FTO electro-conductive glass after the above-mentioned cleaning is immersed in the acetone soln, and sonicated 15min takes out with washed with de-ionized water 1 time then; Immerse in the distilled water sonicated 15min, dry 1min under 60 ℃ of temperature then again; Wherein, supersonic frequency 45KHz;
Two, getting pure platinized platinum, to put into mass percentage content be 65% salpeter solution, is heated to 83 ℃ and keeps 2min, is cooled to room temperature, for use;
Three, with the electro-conductive glass after step 1 is handled as work electrode; As to electrode, other gets the Ag/AgCl electrode as reference electrode, places the 5-Trifluoromethyl-1 of 0.3mol/L with the pure platinized platinum handled through step 2; In the sulfuric acid solution of 3-phenylenediamine; Using cyclic voltammetry, is 1V at direct voltage, and sweep speed is 20mV/s -1, the voltage cycle number of times is under 55 times the condition, to carry out electrochemical polymerization, promptly gets and gathers (5-Trifluoromethyl-1,3-phenylenediamine) film;
Four, gather (5-Trifluoromethyl-1 with what step 3 obtained; The 3-phenylenediamine) film is a work electrode, and as to electrode, other gets the Ag/AgCl electrode as reference electrode with the pure platinized platinum handled through step 2; Place the platinum solution chlorate of 0.003mol/L; Using cyclic voltammetry, is 1V at direct voltage, and sweep speed is 20mV/s -1, the voltage cycle number of times is under 30 times the condition, to carry out electrochemical polymerization, promptly gets and gathers (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film;
Five, (5-Trifluoromethyl-1,3-the phenylenediamine)/sheet platinum grain bulbec film that gathers that step 4 is obtained is put into vacuum drying chamber, is 70 ℃ in temperature, vacuum degree is-condition of 0.1MPa under oven dry 12h subsequent use.
Test 4
The preparation method of a kind of the gathering of this test (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film carries out according to following steps:
One, the FTO electro-conductive glass is immersed in the distilled water, sonicated 15min takes out with washed with de-ionized water 1 time then; FTO electro-conductive glass after the above-mentioned cleaning is immersed in the acetone soln, and sonicated 15min takes out with washed with de-ionized water 1 time then; Immerse in the distilled water sonicated 15min, dry 1min under 60 ℃ of temperature then again; Wherein, supersonic frequency 45KHz;
Two, getting pure platinized platinum, to put into mass percentage content be 65% salpeter solution, is heated to 83 ℃ and keeps 2min, is cooled to room temperature, for use;
Three, with the electro-conductive glass after step 1 is handled as work electrode; As to electrode, other gets the Ag/AgCl electrode as reference electrode, places the 5-Trifluoromethyl-1 of 0.3mol/L with the pure platinized platinum handled through step 2; In the sulfuric acid solution of 3-phenylenediamine; Using cyclic voltammetry, is 1V at direct voltage, and sweep speed is 20mV/s -1, the voltage cycle number of times is under 55 times the condition, to carry out electrochemical polymerization, promptly gets and gathers (5-Trifluoromethyl-1,3-phenylenediamine) film;
Four, gather (5-Trifluoromethyl-1 with what step 3 obtained; The 3-phenylenediamine) film is a work electrode, and as to electrode, other gets the Ag/AgCl electrode as reference electrode with the pure platinized platinum handled through step 2; Place the platinum solution chlorate of 0.003mol/L; Using cyclic voltammetry, is 1V at direct voltage, and sweep speed is 20mV/s -1, the voltage cycle number of times is under 40 times the condition, to carry out electrochemical polymerization, promptly gets and gathers (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film;
Five, (5-Trifluoromethyl-1,3-the phenylenediamine)/sheet platinum grain bulbec film that gathers that step 4 is obtained is put into vacuum drying chamber, is 70 ℃ in temperature, vacuum degree is-condition of 0.1MPa under oven dry 12h subsequent use.
Test 5
The preparation method of a kind of plating platinum film of this test carries out according to following steps:
One, the FTO electro-conductive glass is immersed in the distilled water, sonicated 15min takes out with washed with de-ionized water 1 time then; FTO electro-conductive glass after the above-mentioned cleaning is immersed in the acetone soln, and sonicated 15min takes out with washed with de-ionized water 1 time then; Immerse in the distilled water sonicated 15min, dry 1min under 60 ℃ of temperature then again; Wherein, supersonic frequency 45KHz;
Two, the 0.003mol/L platinum chloric acid ethanolic solution with 0.1mL drips on the electro-conductive glass, puts into Muffle furnace then, at 400 ℃ of sintering temperature 30min, promptly gets pure Pt film.
That adopts ESEM (SEM, FEI QUANTA200F and Mx2600fe) viewing test 1 to 4 gathers (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film, and the surface topography of testing 5 pure Pt film, shown in Fig. 1 to 9.
The platinum particles aggregate shape of gathering (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film that can draw this test by Fig. 1 to Fig. 9 is tending towards the sphere of rule, and diameter increases gradually, can improve as the battery performance of solar cell to electrode.
Gather (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film with what test 1 to 4 obtained, and test the 5 pure Pt films that obtain, carry out application test:
With test 1 to 5 film that makes respectively with TiO 2Film is processed the solar-electricity pool model, the performance of test solar-electricity pool model, and test group is set verifies the effect of gathering (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film that makes with control group.
TiO 2Preparation method's concrete steps of film are following:
One, takes by weighing the colloidal sol of 3mL and the P25 titanium dioxide of 0.668g and mix, promptly get mixed solution; Wherein, described colloidal sol is the butyl titanate by 20mL, and the absolute ethyl alcohol of 50mL and 4mL redistilled water are formed;
Two, the FTO electro-conductive glass is immersed in the distilled water, sonicated 15min takes out with washed with de-ionized water 1 time then; FTO electro-conductive glass after the above-mentioned cleaning is immersed in the acetone soln, and sonicated 15min takes out with washed with de-ionized water 1 time then; Immerse in the distilled water sonicated 15min, dry 1min under 60 ℃ of temperature then again; Wherein, supersonic frequency 45KHz;
Three, Muffle furnace is put on the whole surface of FTO electro-conductive glass after the even blade coating of mixed solution that step 1 is obtained is handled to step 2 then, at 450 ℃ of sintering temperature 30min, promptly gets TiO 2Film;
Four, the TiO that step 2 is obtained 2It is 3x10 that film immerses concentration -4Soak 12h in the N719 dyestuff of mol/L, clean 1 time with absolute ethyl alcohol then, put into baking oven, dry 15min under 70 ℃ of temperature, subsequent use.
Test group:
Test group 1: with TiO 2Film is assembled into together with (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film that gathers that test 1 obtains, and injects I -/ I 3 -Electrolyte obtains the solar-electricity pool model.
Test group 2: with TiO 2Film is assembled into together with (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film that gathers that test 2 obtains, and injects I -/ I 3 -Electrolyte obtains the solar-electricity pool model.
Test group 3: with TiO 2Film is assembled into together with (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film that gathers that test 3 obtains, and injects I -/ I 3 -Electrolyte obtains the solar-electricity pool model.
Test group 4: with TiO 2Film is assembled into together with (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film that gathers that test 4 obtains, and injects I -/ I 3 -Electrolyte obtains the solar-electricity pool model.
Control group: will test the 5 pure Pt film and the TiO that obtain 2Film is assembled into together, injects I -/ I 3 -Electrolyte obtains the solar-electricity pool model.
Wherein, the I in this application test -/ I 3 -Electrolyte is the I by 0.05mol/L 2, 0.1mol/L tert .-butylpyridine and the iodate (1-butyl-3-methylimidazole) of 0.6mol/L of LiI, 0.6mol/L form.
Adopt the 500W xenon lamp as light source, simulated solar irradiation light intensity 100mW/cm -2, the photovoltaic performance of the solar-electricity pool model that makes with electrochemical analysis system (LK98B II, Tianjin Lan Like Co., Ltd) testing experiment group and control group, like table 1 with shown in Figure 10.
Table 1 is different carry the platinum amounts gather (5-Trifluoromethyl-1,3-phenylenediamine) film as solar cell properties to electrode
Figure BDA0000130464060000071
Can know by table 1, gather (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film and have good catalytic effect.Under the identical condition of platinum content, gather (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film and have higher efficient as solar cell to electrode preparation.
Can know from Figure 10, gather (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film and have good catalytic effect.Under the identical condition of platinum content, gather (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film and have preferable performance as solar cell to electrode preparation.

Claims (4)

1. preparation method who gathers (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film is characterized in that the preparation method of described gathering (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film carries out according to following steps:
One, electro-conductive glass is immersed in the water, sonicated 10～20min takes out water then and cleans 1～2 time; Electro-conductive glass after the above-mentioned cleaning is immersed in the acetone soln, and sonicated 10～20min takes out water then and cleans 1～2 time; Immerse in the distilled water sonicated 10～20min, dry 0.5～2min under 50 ℃～80 ℃ temperature then again; Wherein, the supersonic frequency of sonicated is 40～50KHz;
Two, get pure platinized platinum and put into red fuming nitric acid (RFNA), be heated to the boiling back and keep 1～3min, be cooled to room temperature then, for use;
Three, with the electro-conductive glass after step 1 is handled as work electrode, as to electrode, other gets the Ag/AgCl electrode as reference electrode with the pure platinized platinum handled through step 2; Place electrolyte A; Using cyclic voltammetry, is-0.5～1.8V at voltage, and sweep speed is 15～25mV/s -1, the voltage cycle number of times is under 55 times the condition, to carry out electrochemical polymerization, promptly gets and gathers (5-Trifluoromethyl-1,3-phenylenediamine) film;
Four, gather (5-Trifluoromethyl-1 with what step 3 obtained; The 3-phenylenediamine) film is a work electrode, and as to electrode, other gets the Ag/AgCl electrode as reference electrode with the pure platinized platinum handled through step 2; Place electrolyte B; Using cyclic voltammetry, is-0.5～1.8V at voltage, and sweep speed is 15～25mV/s -1, the voltage cycle number of times is under 10～40 times the condition, to carry out electrochemical polymerization, promptly gets and gathers (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film; Wherein, the 5-Trifluoromethyl-1 that the described electrolyte A of step 3 is 0.1～0.5mol/L, the sulfuric acid solution of 3-phenylenediamine; The platinum solution chlorate that the described electrolyte B of step 4 is 0.001～0.01mol/L.
2. the preparation method of a kind of gathering according to claim 1 (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film is characterized in that the described water of step 1 cleans to be meant and to carry out with distilled water or deionized water.
3. the preparation method of a kind of gathering according to claim 1 (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film is characterized in that the described red fuming nitric acid (RFNA) of step 2 is that mass percentage content is 65%～68% nitric acid.
4. the preparation method of a kind of gathering according to claim 1 (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film is characterized in that the described voltage of step 3 and step 4 is direct voltage.
CN2012100085759A 2012-01-12 2012-01-12 Preparation method of poly(5-trifluoromethyl-1,3-phenylenediamine)/laminar platinum particula film Expired - Fee Related CN102522463B (en)

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* Cited by examiner, † Cited by third party
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CN1312032C (en) * 2004-06-08 2007-04-25 中国科学院化学研究所 Prepn process of composite material of metal or metal oxide and carbon nanotube
CN101373670B (en) * 2008-10-09 2011-01-05 彩虹集团公司 Method for preparing porous platinum electrode of solar cell
CN101515505B (en) * 2009-03-31 2011-04-13 彩虹集团公司 Method for preparing platinum electrode of dye sensitized solar cell

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1312032C (en) * 2004-06-08 2007-04-25 中国科学院化学研究所 Prepn process of composite material of metal or metal oxide and carbon nanotube
CN101373670B (en) * 2008-10-09 2011-01-05 彩虹集团公司 Method for preparing porous platinum electrode of solar cell
CN101515505B (en) * 2009-03-31 2011-04-13 彩虹集团公司 Method for preparing platinum electrode of dye sensitized solar cell

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