CN102522463B - 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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CN102522463B
CN102522463B CN2012100085759A CN201210008575A CN102522463B CN 102522463 B CN102522463 B CN 102522463B CN 2012100085759 A CN2012100085759 A CN 2012100085759A CN 201210008575 A CN201210008575 A CN 201210008575A CN 102522463 B CN102522463 B CN 102522463B
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phenylenediamine
trifluoromethyl
film
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platinum
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CN102522463A (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

A kind of preparation method of poly-(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
Reported the DSSC (DSSC) that relative high solar energy conversion efficiency is 8%～11% in 1991 with Gratzel since O ' Regan, DSSCs has caused the interest of Science and Technology widely.DSSCs, due to its high conversion efficiency and low cost, has become one of the most promising photovoltaic device.In general, DSSC comprises that three major parts form: 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 to electrode, be an essential condition that strengthens the DSSC performance, it is mainly used in collecting electronics, also having a Main Function is catalytic action, accelerates I -/ I 3 -and the electron exchange speed between cathode electronics, therefore need to carry out the modification to electrode, to improve its catalytic performance.The main method of modifying adopted is that platinum is modified at present, usually by load, has the electro-conductive glass of platinum catalyst to form, 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, cause the kind electrode preparation cost higher.Polyaniline and its derivative is because it is easily synthetic, and high conductivity, and unique redox property, 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 a kind of preparation method of poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film is provided.
The preparation method of a kind of poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film of the present invention carries out according to following steps:
One, electro-conductive glass is immersed in the water, ultrasonic processing 10～20min, then take out water and clean 1～2 time; Electro-conductive glass after above-mentioned cleaning is immersed in acetone soln, and ultrasonic processing 10～20min, then take out water and clean 1～2 time; Immerse again in distilled water ultrasonic processing 10～20min, then dry 0.5～2min at 50 ℃～80 ℃ temperature; Wherein, the supersonic frequency of ultrasonic processing is 40～50KHz;
Two, get pure platinized platinum and put into red fuming nitric acid (RFNA), the rear maintenance 1～3min that is heated to seethe with excitement, then be cooled to room temperature, stand-by;
The electro-conductive glass of three, usining after step 1 is processed is as work electrode, usings the pure platinized platinum processed through step 2 as to electrode, separately gets the Ag/AgCl electrode as reference electrode, be placed in electrolyte, using cyclic voltammetry, is-0.5～1.8V at voltage, and sweep speed is 15～25mV/s -1, under the condition that the voltage cycle number of times is 55 times, carry out electrochemical polymerization, obtain poly-(5-Trifluoromethyl-1,3-phenylenediamine) film;
Four, poly-(the 5-Trifluoromethyl-1 obtained with step 3, the 3-phenylenediamine) film is work electrode, using the pure platinized platinum processed through step 2 as to electrode, separately get the Ag/AgCl electrode as reference electrode, be placed in electrolyte B, using cyclic voltammetry, is-0.5～1.8V at voltage, and sweep speed is 15～25mV/s -1, under the condition that the voltage cycle number of times is 10～40 times, carry out electrochemical polymerization, obtain poly-(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 poly-(5-Trifluoromethyl-1,3-phenylenediamine) film by electrochemical method, and take this polyaniline film as substrate induction formation lamella globular platinum particle membrane.Poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film as DSSC to electrode, with respect to the pyrolysismethod platinum plating, have the platinum amount of carrying low, the effect that catalytic activity is strong.
The accompanying drawing explanation
Fig. 1 tests Pt prepared by 5 pyrolysismethods that obtain to electrode SEM pattern;
Fig. 2 tests 1 poly-(5-Trifluoromethyl-1,3-the phenylenediamine)/sheet platinum grain bulbec film SEM pattern obtained;
Fig. 3 tests 1 poly-(5-Trifluoromethyl-1,3-the phenylenediamine)/sheet platinum grain bulbec film obtained and amplifies the SEM pattern of 80 times;
Fig. 4 tests 2 poly-(5-Trifluoromethyl-1,3-the phenylenediamine)/sheet platinum grain bulbec film SEM patterns that obtain;
Fig. 5 tests 2 poly-(5-Trifluoromethyl-1,3-the phenylenediamine)/sheet platinum grain bulbec films that obtain and amplifies the SEM pattern of 80 times;
Fig. 6 tests 3 poly-(5-Trifluoromethyl-1,3-the phenylenediamine)/sheet platinum grain bulbec film SEM patterns that obtain;
Fig. 7 tests 3 poly-(5-Trifluoromethyl-1,3-the phenylenediamine)/sheet platinum grain bulbec films that obtain and amplifies the SEM pattern of 80 times;
Fig. 8 tests 4 poly-(5-Trifluoromethyl-1,3-the phenylenediamine)/sheet platinum grain bulbec film SEM patterns that obtain;
Fig. 9 tests 4 poly-(5-Trifluoromethyl-1,3-the phenylenediamine)/sheet platinum grain bulbec films that obtain and amplifies the SEM pattern of 80 times;
Pt film prepared by Figure 10 pyrolysismethod and the different thin polymer film of platinum amount that carries are as the voltage-to-current curve to electrode; Wherein, the 1 voltage-to-current curve for test 4, the 2 voltage-to-current curves for test 3, the 3 voltage-to-current curves for test 2, the 4 voltage-to-current curves for test 1, the 5 voltage-to-current curves for test 5.
Embodiment
Technical solution 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 poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film of present embodiment carries out according to following steps:
One, electro-conductive glass is immersed in the water, ultrasonic processing 10～20min, then take out water and clean 1～2 time; Electro-conductive glass after above-mentioned cleaning is immersed in acetone soln, and ultrasonic processing 10～20min, then take out water and clean 1～2 time; Immerse again in distilled water ultrasonic processing 10～20min, then dry 0.5～2min at 50 ℃～80 ℃ temperature; Wherein, the supersonic frequency of ultrasonic processing is 40～50KHz;
Two, get pure platinized platinum and put into red fuming nitric acid (RFNA), the rear maintenance 1～3min that is heated to seethe with excitement, then be cooled to room temperature, stand-by;
The electro-conductive glass of three, usining after step 1 is processed is as work electrode, usings the pure platinized platinum processed through step 2 as to electrode, separately gets the Ag/AgCl electrode as reference electrode, be placed in electrolyte, using cyclic voltammetry, is-0.5～1.8V at voltage, and sweep speed is 15～25mV/s -1, under the condition that the voltage cycle number of times is 55 times, carry out electrochemical polymerization, obtain poly-(5-Trifluoromethyl-1,3-phenylenediamine) film;
Four, poly-(the 5-Trifluoromethyl-1 obtained with step 3, the 3-phenylenediamine) film is work electrode, using the pure platinized platinum processed through step 2 as to electrode, separately get the Ag/AgCl electrode as reference electrode, be placed in electrolyte B, using cyclic voltammetry, is-0.5～1.8V at voltage, and sweep speed is 15～25mV/s -1, under the condition that the voltage cycle number of times is 10～40 times, carry out electrochemical polymerization, obtain poly-(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 present embodiment is: synthesized poly-(5-Trifluoromethyl-1,3-phenylenediamine) by electrochemical method, and take this polyaniline film as substrate induction formation lamella globular platinum particle membrane.Poly-(5-Trifluoromethyl-1,3-phenylenediamine) platinum particles film as DSSC to electrode, with respect to the pyrolysismethod platinum plating, have the platinum amount of carrying low, the effect that catalytic activity is strong.
Embodiment two: present embodiment is different from embodiment one: the described water of step 1 cleans and to refer to and carry out with distilled water or deionized water.Other is identical with embodiment one.
Embodiment three: present embodiment is different from embodiment one to two: the described red fuming nitric acid (RFNA) of step 2 is the nitric acid that mass percentage content is 65%～68%.Other is identical with embodiment one to two.
Embodiment four: present embodiment is different from one of embodiment one to three: the described voltage of step 3 and step 4 is direct voltage.Other is identical with one of embodiment one to three.
By following verification experimental verification effect of the present invention:
Test 1
The preparation method of a kind of poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film of this test carries out according to following steps:
One, the FTO electro-conductive glass is immersed in distilled water, ultrasonic processing 15min, then take out and use washed with de-ionized water 1 time; FTO electro-conductive glass after above-mentioned cleaning is immersed in acetone soln, and ultrasonic processing 15min, then take out and use washed with de-ionized water 1 time; Immerse again in distilled water ultrasonic processing 15min, then dry 1min at 60 ℃ of temperature; Wherein, supersonic frequency 45KHz;
Two, get pure platinized platinum and put into the salpeter solution that mass percentage content is 65%, be heated to 83 ℃ and keep 2min, be cooled to room temperature, stand-by;
The electro-conductive glass of three, usining after step 1 is processed is as work electrode, using the pure platinized platinum processed through step 2 as to electrode, separately get the Ag/AgCl electrode as reference electrode, be placed in the 5-Trifluoromethyl-1 of 0.3mol/L, in the sulfuric acid solution of 3-phenylenediamine, using cyclic voltammetry, is 1V at direct voltage, and sweep speed is 20mV/s -1, under the condition that the voltage cycle number of times is 55 times, carry out electrochemical polymerization, obtain poly-(5-Trifluoromethyl-1,3-phenylenediamine) film;
Four, poly-(the 5-Trifluoromethyl-1 obtained with step 3, the 3-phenylenediamine) film is work electrode, using the pure platinized platinum processed through step 2 as to electrode, separately get the Ag/AgCl electrode as reference electrode, be placed in the platinum solution chlorate of 0.003mol/L, using cyclic voltammetry, is 1V at direct voltage, and sweep speed is 20mV/s -1, under the condition that the voltage cycle number of times is 10 times, carry out electrochemical polymerization, obtain poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film;
Five, poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film step 4 obtained is put into vacuum drying chamber, in temperature, is 70 ℃, vacuum degree be-condition of 0.1MPa under oven dry 12h standby.
Test 2
The preparation method of a kind of poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film of this test carries out according to following steps:
One, the FTO electro-conductive glass is immersed in distilled water, ultrasonic processing 15min, then take out and use washed with de-ionized water 1 time; FTO electro-conductive glass after above-mentioned cleaning is immersed in acetone soln, and ultrasonic processing 15min, then take out and use washed with de-ionized water 1 time; Immerse again in distilled water ultrasonic processing 15min, then dry 1min at 60 ℃ of temperature; Wherein, supersonic frequency 45KHz;
Two, get pure platinized platinum and put into the salpeter solution that mass percentage content is 65%, be heated to 83 ℃ and keep 2min, be cooled to room temperature, stand-by;
The electro-conductive glass of three, usining after step 1 is processed is as work electrode, using the pure platinized platinum processed through step 2 as to electrode, separately get the Ag/AgCl electrode as reference electrode, be placed in the 5-Trifluoromethyl-1 of 0.3mol/L, in the sulfuric acid solution of 3-phenylenediamine, using cyclic voltammetry, is 1V at direct voltage, and sweep speed is 20mV/s -1, under the condition that the voltage cycle number of times is 55 times, carry out electrochemical polymerization, obtain poly-(5-Trifluoromethyl-1,3-phenylenediamine) film;
Four, poly-(the 5-Trifluoromethyl-1 obtained with step 3, the 3-phenylenediamine) film is work electrode, using the pure platinized platinum processed through step 2 as to electrode, separately get the Ag/AgCl electrode as reference electrode, be placed in the platinum solution chlorate of 0.003mol/L, using cyclic voltammetry, is 1V at direct voltage, and sweep speed is 20mV/s -1, under the condition that the voltage cycle number of times is 20 times, carry out electrochemical polymerization, obtain poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film;
Five, poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film step 4 obtained is put into vacuum drying chamber, in temperature, is 70 ℃, vacuum degree be-condition of 0.1MPa under oven dry 12h standby.
Test 3
The preparation method of a kind of poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film of this test carries out according to following steps:
One, the FTO electro-conductive glass is immersed in distilled water, ultrasonic processing 15min, then take out and use washed with de-ionized water 1 time; FTO electro-conductive glass after above-mentioned cleaning is immersed in acetone soln, and ultrasonic processing 15min, then take out and use washed with de-ionized water 1 time; Immerse again in distilled water ultrasonic processing 15min, then dry 1min at 60 ℃ of temperature; Wherein, supersonic frequency 45KHz;
Two, get pure platinized platinum and put into the salpeter solution that mass percentage content is 65%, be heated to 83 ℃ and keep 2min, be cooled to room temperature, stand-by;
The electro-conductive glass of three, usining after step 1 is processed is as work electrode, using the pure platinized platinum processed through step 2 as to electrode, separately get the Ag/AgCl electrode as reference electrode, be placed in the 5-Trifluoromethyl-1 of 0.3mol/L, in the sulfuric acid solution of 3-phenylenediamine, using cyclic voltammetry, is 1V at direct voltage, and sweep speed is 20mV/s -1, under the condition that the voltage cycle number of times is 55 times, carry out electrochemical polymerization, obtain poly-(5-Trifluoromethyl-1,3-phenylenediamine) film;
Four, poly-(the 5-Trifluoromethyl-1 obtained with step 3, the 3-phenylenediamine) film is work electrode, using the pure platinized platinum processed through step 2 as to electrode, separately get the Ag/AgCl electrode as reference electrode, be placed in the platinum solution chlorate of 0.003mol/L, using cyclic voltammetry, is 1V at direct voltage, and sweep speed is 20mV/s -1, under the condition that the voltage cycle number of times is 30 times, carry out electrochemical polymerization, obtain poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film;
Five, poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film step 4 obtained is put into vacuum drying chamber, in temperature, is 70 ℃, vacuum degree be-condition of 0.1MPa under oven dry 12h standby.
Test 4
The preparation method of a kind of poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film of this test carries out according to following steps:
One, the FTO electro-conductive glass is immersed in distilled water, ultrasonic processing 15min, then take out and use washed with de-ionized water 1 time; FTO electro-conductive glass after above-mentioned cleaning is immersed in acetone soln, and ultrasonic processing 15min, then take out and use washed with de-ionized water 1 time; Immerse again in distilled water ultrasonic processing 15min, then dry 1min at 60 ℃ of temperature; Wherein, supersonic frequency 45KHz;
Two, get pure platinized platinum and put into the salpeter solution that mass percentage content is 65%, be heated to 83 ℃ and keep 2min, be cooled to room temperature, stand-by;
The electro-conductive glass of three, usining after step 1 is processed is as work electrode, using the pure platinized platinum processed through step 2 as to electrode, separately get the Ag/AgCl electrode as reference electrode, be placed in the 5-Trifluoromethyl-1 of 0.3mol/L, in the sulfuric acid solution of 3-phenylenediamine, using cyclic voltammetry, is 1V at direct voltage, and sweep speed is 20mV/s -1, under the condition that the voltage cycle number of times is 55 times, carry out electrochemical polymerization, obtain poly-(5-Trifluoromethyl-1,3-phenylenediamine) film;
Four, poly-(the 5-Trifluoromethyl-1 obtained with step 3, the 3-phenylenediamine) film is work electrode, using the pure platinized platinum processed through step 2 as to electrode, separately get the Ag/AgCl electrode as reference electrode, be placed in the platinum solution chlorate of 0.003mol/L, using cyclic voltammetry, is 1V at direct voltage, and sweep speed is 20mV/s -1, under the condition that the voltage cycle number of times is 40 times, carry out electrochemical polymerization, obtain poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film;
Five, poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film step 4 obtained is put into vacuum drying chamber, in temperature, is 70 ℃, vacuum degree be-condition of 0.1MPa under oven dry 12h standby.
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 distilled water, ultrasonic processing 15min, then take out and use washed with de-ionized water 1 time; FTO electro-conductive glass after above-mentioned cleaning is immersed in acetone soln, and ultrasonic processing 15min, then take out and use washed with de-ionized water 1 time; Immerse again in distilled water ultrasonic processing 15min, then dry 1min at 60 ℃ of temperature; Wherein, supersonic frequency 45KHz;
Two, the 0.003mol/L platinum chloric acid ethanolic solution of 0.1mL is dripped on electro-conductive glass, then put into Muffle furnace, sintering 30min at 400 ℃ of temperature, obtain pure Pt film.
Adopt poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film of ESEM (SEM, FEI QUANTA200F and Mx2600fe) viewing test 1 to 4, and the surface topography of testing 5 pure Pt film, as shown in Figure 1 to 9.
Can be drawn poly-(the 5-Trifluoromethyl-1 of this test by Fig. 1 to Fig. 9, the platinum particles aggregate shape of the 3-phenylenediamine)/sheet platinum grain bulbec film is tending towards the spherical of rule, and diameter increases gradually, can improve the battery performance to electrode as solar cell.
Poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film that test 1 to 4 is obtained, and test the 5 pure Pt films that obtain, carry out application test:
By the test 1 to 5 film made respectively with TiO 2film is made the solar-electricity pool model, the performance of test solar-electricity pool model, and the effect of gathering (5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film that test group and control group checking make is set.
TiO 2preparation method's concrete steps of film are as follows:
One, take the colloidal sol of 3mL and the P25 titanium dioxide of 0.668g and mix, obtain mixed solution; Wherein, described colloidal sol is the butyl titanate by 20mL, and the absolute ethyl alcohol of 50mL and 4mL redistilled water form;
Two, the FTO electro-conductive glass is immersed in distilled water, ultrasonic processing 15min, then take out and use washed with de-ionized water 1 time; FTO electro-conductive glass after above-mentioned cleaning is immersed in acetone soln, and ultrasonic processing 15min, then take out and use washed with de-ionized water 1 time; Immerse again in distilled water ultrasonic processing 15min, then dry 1min at 60 ℃ of temperature; Wherein, supersonic frequency 45KHz;
Three, the whole surface of FTO electro-conductive glass after the even blade coating of mixed solution step 1 obtained is processed to step 2, then put into Muffle furnace, and sintering 30min at 450 ℃ of temperature, obtain TiO 2film;
Four, TiO step 2 obtained 2it is 3x10 that film immerses concentration -4soak 12h in the N719 dyestuff of mol/L, then clean 1 time with absolute ethyl alcohol, put into baking oven, dry 15min at 70 ℃ of temperature, standby.
Test group:
Test group 1: by TiO 2film is assembled into together with poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film that test 1 obtains, and injects I -/ I 3 -electrolyte, obtain the solar-electricity pool model.
Test group 2: by TiO 2film is assembled into together with poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film that test 2 obtains, and injects I -/ I 3 -electrolyte, obtain the solar-electricity pool model.
Test group 3: by TiO 2film is assembled into together with poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film that test 3 obtains, and injects I -/ I 3 -electrolyte, obtain the solar-electricity pool model.
Test group 4: by TiO 2film is assembled into together with poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film that test 4 obtains, and injects I -/ I 3 -electrolyte, obtain the solar-electricity pool model.
Control group: will test 5 pure Pt film and the TiO that obtain 2film is assembled into together, injects I -/ I 3 -electrolyte, obtain the solar-electricity pool model.
Wherein, the I in this application test -/ I 3 -electrolyte is the I by 0.05mol/L 2, the tert .-butylpyridine of LiI, 0.6mol/L of 0.1mol/L and the iodate (1-butyl-3-methylimidazole) of 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 made with electrochemical analysis system (LK98B II, Tianjin Lan Like Co., Ltd) testing experiment group and control group, as shown in table 1 and Figure 10.
Different poly-(5-Trifluoromethyl-1, the 3-phenylenediamine) films of platinum amount that carry of table 1 are as the solar cell properties to electrode
As shown in Table 1, poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film has good catalytic effect.At platinum content, under identical condition, poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film has higher efficiency as solar cell prepared by electrode.
As can be seen from Figure 10, poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film has good catalytic effect.At platinum content, under identical condition, poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film has performance preferably as solar cell prepared by electrode.

Claims (4)

1. the preparation method of poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film is characterized in that the preparation method of described poly-(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, ultrasonic processing 10～20min, then take out water and clean 1～2 time; Electro-conductive glass after above-mentioned cleaning is immersed in acetone soln, and ultrasonic processing 10～20min, then take out water and clean 1～2 time; Immerse again in distilled water ultrasonic processing 10～20min, then dry 0.5～2min at 50 ℃～80 ℃ temperature; Wherein, the supersonic frequency of ultrasonic processing is 40～50KHz;
Two, get pure platinized platinum and put into red fuming nitric acid (RFNA), the rear maintenance 1～3min that is heated to seethe with excitement, then be cooled to room temperature, stand-by;
The electro-conductive glass of three, usining after step 1 is processed is as work electrode, usings the pure platinized platinum processed through step 2 as to electrode, separately gets the Ag/AgCl electrode as reference electrode, be placed in electrolyte A, using cyclic voltammetry, is-0.5～1.8V at voltage, and sweep speed is 15～25mV/s -1, under the condition that the voltage cycle number of times is 55 times, carry out electrochemical polymerization, obtain poly-(5-Trifluoromethyl-1,3-phenylenediamine) film;
Four, poly-(the 5-Trifluoromethyl-1 obtained with step 3, the 3-phenylenediamine) film is work electrode, using the pure platinized platinum processed through step 2 as to electrode, separately get the Ag/AgCl electrode as reference electrode, be placed in electrolyte B, using cyclic voltammetry, is-0.5～1.8V at voltage, and sweep speed is 15～25mV/s -1, under the condition that the voltage cycle number of times is 10～40 times, carry out electrochemical polymerization, obtain poly-(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 poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film according to claim 1, is characterized in that the described water of step 1 cleans to refer to and carry out with distilled water or deionized water.
3. the preparation method of a kind of poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film according to claim 1, is characterized in that the described red fuming nitric acid (RFNA) of step 2 is the nitric acid that mass percentage content is 65%～68%.
4. the preparation method of a kind of poly-(5-Trifluoromethyl-1,3-phenylenediamine)/sheet platinum grain bulbec film according to claim 1, 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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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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