CN103173794A - Method for improving photoelectrical-chemical activity of Ti-Fe2O3 membrane electrode - Google Patents

Method for improving photoelectrical-chemical activity of Ti-Fe2O3 membrane electrode Download PDF

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CN103173794A
CN103173794A CN 201310125925 CN201310125925A CN103173794A CN 103173794 A CN103173794 A CN 103173794A CN 201310125925 CN201310125925 CN 201310125925 CN 201310125925 A CN201310125925 A CN 201310125925A CN 103173794 A CN103173794 A CN 103173794A
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electrode
conductive glass
colloid
membrane electrode
photoelectrical
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童少平
上官鹏鹏
冷文华
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Zhejiang University of Technology ZJUT
Zhejiang University ZJU
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Zhejiang University of Technology ZJUT
Zhejiang University ZJU
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Abstract

The invention discloses the technical field of hydrogen production by semiconductor photoelectrical-catalysis water decomposition and in particular relates to a method for improving photoelectrical-chemical activity of titanium-doped hematite by an electrochemical reducing pretreatment method. The method comprises the following steps of: cleaning indium conductive glass by acetone and alcohol for 15 minutes under an ultrasonic condition, respectively; ultrasonically cleaning the indium conductive glass by deionized water; and drying the cleaned indium conductive glass by nitrogen gas for future use; adding alcohol and concentrated hydrochloric acid to the materials of ferric trichloride and titanate to prepare FeCl3-titanate colloid; and placing ITO (Indium Tin Oxide) conductive glass on a table spin coater, dropwise adding the Fe3Cl3-titanate colloid to the table spin coater, placing the table spin coater for roasting for 5 minutes under 350 DEG C, cooling to the room temperature and coating by repeating the process by eight times. The method disclosed by the invention has the advantages of greatly improving the photoelectric-chemical activity of the membrane electrode, so that the electrode after the electrochemical reducing treatment has good photoelectrical-chemical stability.

Description

A kind of raising Ti-Fe 2O 3The chemically active method of film electrode photoelectric
Technical field
The present invention relates to semiconductor photoelectrocatalysielectrode and decompose aquatic products hydrogen technical field, it is active that particularly a kind of electrochemical reduction pretreatment process improves the photoelectrochemistry of mixing haplotypite.
Background technology
Fujishima and Honda find TiO since the beginning of the seventies in last century 2Since electrode glazing electrochemical decomposition aquatic products hydrogen, utilize the conductor photocatalysis hydrogen production by water decomposition to become the research direction of common concern. its ultimate principle is as follows: when absorbing the rayed semi-conductor of threshold value with energy higher than semi-conductor, its valence band electronics generation band-to-band transition, produce electronics and hole, under thermodynamic condition allows, the hole and the electron donor steeping in water for reconstitution in solution that are migrated to the semiconductor particle surface are given birth to oxidizing reaction, and electronics and proton or the steeping in water for reconstitution former reaction generation hydrogen of surviving.Utilize solar photolysis water hydrogen as one of Future New Energy Source approach, be subject to people's great attention.In addition, the Photocatalitic Technique of Semiconductor range of application also constantly enlarges, and also has potential tempting prospect in fields such as degraded environmental pollutant and opto-electronic conversion.
through researcher man exploration and accumulation for many years, the research that semiconductor photoelectrocatalysielectrode decomposes aquatic products hydrogen technology has obtained huge progress. at numerous inorganic photocatalyst material such as zinc oxide, titanium dioxide, in the middle of rhombohedral iron ore and sulfide etc., rhombohedral iron ore has with low cost, good stability and the advantage such as nontoxic, particularly its energy gap is about 2.0-2.2eV, approach with the peak value of sunlight, visible light there is stronger absorption, can absorb 40% sunlight on principle, that following sun power transforms and utilize the more satisfactory candidate material in aspect. still, also there is poor electric conductivity in rhombohedral iron ore, slow shortcoming is shifted to compound fast and interfacial charge in light induced electron-hole. metal ion such as titanium doped its photoelectrochemistry activity that significantly improves, but up to the present, pure rhombohedral iron ore and mix the efficient of haplotypite sunlight water of decomposition also lower than its theoretical maximum (12.9%), so improve energetically its efficient for realizing that decomposing water with solar energy produces hydrogen etc. and will have important using value.
Electrochemical reduction is from a kind of method of rhombohedral iron ore thing extracting metals iron, has no bibliographical information but be used for improving titano-hematite photoelectrochemistry activity. principle of the present invention is: the magnetite (Fe that produces when utilizing electrochemical reduction to mix haplotypite 3O 4) and the metallic iron recombination rate etc. that improves the electroconductibility, interfacial charge transfer rate of membrane electrode and reduce photo-generated carrier to improve the photoelectrochemistry of membrane electrode active.
Summary of the invention
The purpose of this invention is to provide a kind of short-cut method and improve significantly the photoelectrochemistry activity of mixing haplotypite.
The present invention is achieved by following technical proposals:
A kind of raising Ti-Fe 2O 3The chemically active method of film electrode photoelectric is characterized in that comprising the steps:
Step 1: cleaned the indium conductive glass each 15 minutes under ultrasound condition with acetone and ethanol successively, then spent ion ultrasonic cleaning 15 minutes, dry up at last stand-by with nitrogen;
Step 2: take iron trichloride, titanic acid ester as raw material, add ethanol, concentrated hydrochloric acid, be mixed with FeCl 3-titanic acid ester colloid; Wherein the mol ratio of the Ti:Fe in colloid is 1:10～13; FeCl 3Volumetric molar concentration in ethanol is 60mM, and wherein the mass concentration of concentrated hydrochloric acid is more than 35%, and the volume ratio of concentrated hydrochloric acid consumption and ethanol consumption is 0.10～0.15:200; The contriver found through experiments, and very cool with a certain amount of iron, titanium in the titanic acid ester colloid, its photoelectric activity all increases significantly than pure iron oxide.
Step 3: the ITO conductive glass is placed on desk-top sol evenning machine, is to drip FeCl under the rotating state of 600 rev/mins at rotating speed 3-titanic acid ester colloid rotates after 6 seconds, its taking-up to be inserted in retort furnace and calcined 5 minutes under 350 ℃ on the ITO conductive glass, and then the cooling room temperature of putting, complete once and film;
Step 4: by the identical mode of step 3, then be coated with membrane operations, carry out continuously 8 times; Then calcined 4 hours under 550 ℃, naturally cooling, and connect wire with copper conductive adhesive; Obtain crude product Ti-Fe after spontaneous curing 2O 3Membrane electrode, stand-by; In this step, the contriver finds to be coated with continuously membrane operations through 8 times by the contrast of different number of times, can obtain best effect, and this is also never to disclose in other prior art.Corresponding calcining temperature, time etc. are all the best effect of contriver through drawing after test of long duration.Wire in this step connects, except working portion, the film rest part is understood by the interior those skilled in the art of industry with technology such as 706 one-component silicone rubbers envelopes are coated with.
Step 5: with above-mentioned crude product Ti-Fe 2O 3Membrane electrode is working electrode, and platinum electrode is to electrode, and saturated calomel electrode is reference electrode, in the NaOH of 1M alkaline electrolyte or 0.5M Na 2SO 4Neutral electrolyte in carry out electrochemical reduction and process, reduction potential-1.2≤E＜-0.6V, time 5-40 minute; Get final product to get Ti-Fe 2O 3Membrane electrode.Result shows, it is active that electrochemical reduction is processed the photoelectrochemistry that has improved significantly membrane electrode.
As preferably, the mol ratio of the Ti:Fe in the colloid of above-mentioned steps 2 is 1:10; The volume ratio of concentrated hydrochloric acid consumption and ethanol consumption is 0.13:200.
As preferably, in above-mentioned steps 2, titanic acid ester used is butyl (tetra) titanate, titanium propanolate or isopropyl titanate.
The ITO conductive glass refers on the basis of sodium calcium base or silicon boryl substrate glass in the present invention, utilizes the method for magnetron sputtering to plate indium oxide layer tin (being commonly called as ITO) film and manufactures.
Beneficial effect: electrochemical reduction pre-treatment Ti-Fe in the present invention 2O 3Electrode equipment is simple, and step is few, and is with low cost, and electrochemical reduction current potential and recovery time are easily regulated; The electrochemical reduction pre-treatment can improve the photoelectrochemistry activity of membrane electrode significantly; The pretreated electrode of electrochemical reduction has good Photoelectrochemical stabilization.
Description of drawings
Under Fig. 1 white light (UV-vis) and visible light (vis) illumination, pure rhombohedral iron ore (Fe 2O 3) and mix haplotypite (Ti-Fe 2O 3) the active comparison diagram of rear (with ER) photoelectrochemistry of electrochemical reduction (ER) processing front (w/o), Fe 2O 3Current-voltage curve, electrochemical reduction current potential are-1.1V that the recovery time is 20 minutes;
Under Fig. 2 white light (UV-vis) and visible light (vis) illumination, pure rhombohedral iron ore (Fe 2O 3) and mix haplotypite (Ti-Fe 2O 3) the active comparison diagram of rear (with ER) photoelectrochemistry of electrochemical reduction (ER) processing front (w/o), Ti-Fe 2O 3Current-voltage curve, electrochemical reduction current potential are-1.1V that the recovery time is 20 minutes;
Under Fig. 3 white light (UV-vis) and visible light (vis) illumination, pure rhombohedral iron ore (Fe 2O 3) and mix haplotypite (Ti-Fe 2O 3) the active comparison diagram of rear (with ER) photoelectrochemistry of electrochemical reduction (ER) processing front (w/o), Fe 2O 3Electric current-time curve, electrochemical reduction current potential are-1.1V that the recovery time is 20 minutes;
Under Fig. 4 white light (UV-vis) and visible light (vis) illumination, pure rhombohedral iron ore (Fe 2O 3) and mix haplotypite (Ti-Fe 2O 3) the active comparison diagram of rear (with ER) photoelectrochemistry of electrochemical reduction (ER) processing front (w/o), Ti-Fe 2O 3Electric current-time curve;
Under Fig. 5 white light (UV-vis) and visible light (vis) illumination, pure rhombohedral iron ore (Fe 2O 3) and mix haplotypite (Ti-Fe 2O 3) the active comparison diagram of rear (with ER) photoelectrochemistry of electrochemical reduction (ER) processing front (w/o), Ti-Fe 2O 3The relation of photoelectric current and electrochemical reduction current potential;
Under Fig. 6 white light (UV-vis) and visible light (vis) illumination, pure rhombohedral iron ore (Fe 2O 3) and mix haplotypite (Ti-Fe 2O 3) the active comparison diagram of rear (with ER) photoelectrochemistry of electrochemical reduction (ER) processing front (w/o), Ti-Fe 2O 3The relation of photoelectric current and electrochemical reduction time;
Under the illumination of Fig. 7 visible light, Ti-Fe 2O 3The relation of photoelectric current and electrochemical reduction current potential, 0.5M Na 2SO 4(neutrality) is ionogen, and the recovery time is 5 minutes;
(100mWcm under the illumination of Fig. 8 simulated solar -2), Ti-Fe 2O 3Electric charge interfacial migration rate constant before and after the electrode electro Chemical reduction (
Figure BDA00003038418400031
) and transfer resistance (R ct);
(100mWcm under the illumination of Fig. 9 simulated solar -2), Ti-Fe 2O 3Electric charge interfacial migration rate constant before and after the electrode electro Chemical reduction (
Figure BDA00003038418400041
) and series resistance (R s) variation diagram;
Figure 10 Ti-Fe 2O 3Photoabsorption and reflection comparison diagram before and after the electrode electro Chemical reduction, the electrochemical reduction current potential is-1.1V that the recovery time is 10 minutes;
Figure 11 Ti-Fe 2O 3The scanning electron microscope (SEM) photograph contrast of photoabsorption and reflection before and after the electrode electro Chemical reduction, the electrochemical reduction current potential is-1.1V that the recovery time is 10 minutes;
Embodiment
The below illustrates enforcement of the present invention:
Embodiment 1
A kind of raising Ti-Fe 2O 3The chemically active method of film electrode photoelectric, carry out as follows:
Step 1: cleaned the indium conductive glass each 15 minutes under ultrasound condition with acetone and ethanol successively, then spent ion ultrasonic cleaning 15 minutes, dry up at last stand-by with nitrogen;
Step 2: take iron trichloride, titanic acid ester as raw material, take the iron trichloride (FeCl of 3.24g 3.6H 2O) transfer in reagent bottle, add ethanol, concentrated hydrochloric acid, be mixed with FeCl 3-titanic acid ester colloid; FeCl 3Volumetric molar concentration in ethanol is 60mM, and wherein the mass concentration of concentrated hydrochloric acid is more than 35%, adds the ethanol of 200ml, the butyl (tetra) titanate of 0.4ml, and the concentrated hydrochloric acid of 0.13ml mixes, and makes 60mM FeCl 3, 6mM butyl (tetra) titanate colloid;
Step 3: the ITO conductive glass is placed on desk-top sol evenning machine, is to drip the FeCl of 0.5ml under the rotating state of 600 rev/mins at rotating speed 3-titanic acid ester colloid rotates after 6 seconds, its taking-up to be inserted in retort furnace and calcined 5 minutes under 350 ℃ on the ITO conductive glass, and then the cooling room temperature of putting, complete once and film;
Step 4: by the identical mode of step 3, then be coated with membrane operations, carry out continuously 8 times; Then calcined 4 hours under 550 ℃, naturally cooling, and connect wire with copper conductive adhesive; Except working portion, the film rest part is coated with 706 one-component silicone rubber envelopes, obtains crude product Ti-Fe after spontaneous curing 2O 3Membrane electrode, stand-by;
Step 5: with above-mentioned crude product Ti-Fe 2O 3Membrane electrode is working electrode, and platinum electrode is to electrode, and saturated calomel electrode is reference electrode, in the NaOH of 1M alkaline electrolyte or 0.5M Na 2SO 4Neutral electrolyte in carry out electrochemical reduction and process, reduction potential-1.2≤E＜-0.6V, time 5-40 minute; Get final product to get Ti-Fe 2O 3Membrane electrode.
Membrane electrode before and after processing take above-mentioned electrochemical reduction is as working electrode, and platinum electrode is to electrode, and saturated calomel electrode is reference electrode, and its photoelectrochemistry of test is active in alkalescence (1M NaOH) electrolytic solution.Result shows, it is active that electrochemical reduction is processed the photoelectrochemistry that has improved significantly membrane electrode, concrete outcome such as Fig. 1, Fig. 2, Fig. 3, Fig. 4, Fig. 5, shown in Figure 6.
Embodiment 2
Press the identical step of embodiment 1, not titaniferous Fe 2O 3The preparation of membrane electrode: cleaned indium conductive glass (ITO) each 15 minutes under ultrasound condition with acetone and ethanol successively, then spent ion ultrasonic cleaning 15 minutes, dry up at last stand-by with nitrogen; Take the iron trichloride (FeCl of 3.24g 3.6H 2O) transfer in reagent bottle, add the ethanol of 200ml, the concentrated hydrochloric acid of 0.13ml mixes, and makes FeCl 3Colloid; The ITO conductive glass is placed on desk-top sol evenning machine, and (600 rev/mins of rotating speeds) drips the FeCl of 0.5ml under rotating state 3Colloid is on the ITO conductive glass, rotate after 6 seconds, its taking-up to be inserted in retort furnace and calcined 5 minutes in 350 ℃ of lower air, the cooling room temperature of putting, complete once and film. repeat the certain number of times of the above-mentioned step of filming (unless outside explanation, filming 8 times), it was calcined 4 hours under 550 ℃ at last, naturally cooling, and connect wire with copper conductive adhesive. except working portion, the film rest part is coated with 706 one-component silicone rubber envelopes, obtains not titaniferous Fe after spontaneous curing 2O 3Membrane electrode, stand-by.
Take above-mentioned membrane electrode as working electrode, platinum electrode is to electrode, and saturated calomel electrode is reference electrode, carries out electrochemical reduction and process in alkalescence (1M NaOH) electrolytic solution, reduction potential E=-1.1V, 20 minutes time.
Membrane electrode before and after processing take above-mentioned electrochemical reduction is as working electrode, and platinum electrode is to electrode, and saturated calomel electrode is reference electrode, and its photoelectrochemistry of test is active in alkalescence (1M NaOH) electrolytic solution.Result shows, it is active that electrochemical reduction is processed the photoelectrochemistry that has improved significantly membrane electrode, result such as Fig. 1, Fig. 2, Fig. 3, Fig. 4, Fig. 5, shown in Figure 6.
Embodiment 3
Ti-Fe 2O 3The preparation method of membrane electrode is identical with embodiment 1.
Take above-mentioned membrane electrode as working electrode, platinum electrode is to electrode, and saturated calomel electrode is reference electrode, at 0.5M Na 2SO 4Carry out electrochemical reduction in neutral electrolyte and process, reduction potential-1.2≤E≤-0.4V, 5 minutes time.
Membrane electrode before and after processing take above-mentioned electrochemical reduction is as working electrode, and platinum electrode is to electrode, and saturated calomel electrode is reference electrode, at 0.5M Na 2SO 4In neutral electrolyte, its photoelectrochemistry of test is active.Result shows, it is active that electrochemical reduction is processed the photoelectrochemistry that has improved significantly membrane electrode, as shown in Figure 7.
With preparation-obtained river membrane electrode (100mWcm under simulated solar illumination -2) test, to Ti-Fe 2O 3Electric charge interfacial migration rate constant before and after the electrode electro Chemical reduction (
Figure BDA00003038418400061
) and transfer resistance (R ct) situation analyzes, and obtains result shown in Figure 8;
With preparation-obtained river membrane electrode (100mWcm under simulated solar illumination -2) test, to Ti-Fe 2O 3Electric charge interfacial migration rate constant before and after the electrode electro Chemical reduction (
Figure BDA00003038418400062
) and series resistance (R s) mutation analysis, obtain result shown in Figure 9;
With preparation-obtained river membrane electrode at Ti-Fe 2O 3Before and after electrode electro Chemical reduction, test comparison is carried out in photoabsorption and reflection, and electrochemical reduction current potential wherein is-1.1V, and the recovery time is 10 minutes, and result as shown in figure 10;
With preparation-obtained river membrane electrode at Ti-Fe 2O 3Before and after the electrode electro Chemical reduction, the scanning electron microscope (SEM) photograph of photoabsorption and reflection is measured contrast, and wherein the electrochemical reduction current potential is-1.1V, and the recovery time is 10 minutes, and result as shown in figure 11.

Claims (3)

1. one kind is improved Ti-Fe 2O 3The chemically active method of film electrode photoelectric is characterized in that comprising the steps:
Step 1: cleaned the indium conductive glass each 15 minutes under ultrasound condition with acetone and ethanol successively, then spent ion ultrasonic cleaning 15 minutes, dry up at last stand-by with nitrogen;
Step 2: take iron trichloride, titanic acid ester as raw material, add ethanol, concentrated hydrochloric acid, be mixed with FeCl 3-titanic acid ester colloid; Wherein the mol ratio of the Ti:Fe in colloid is 1:10～13; FeCl 3Volumetric molar concentration in ethanol is 60mM, and wherein the mass concentration of concentrated hydrochloric acid is more than 35%, and the volume ratio of concentrated hydrochloric acid consumption and ethanol consumption is 0.10～0.15:200;
Step 3: the ITO conductive glass is placed on desk-top sol evenning machine, is to drip FeCl under the rotating state of 600 rev/mins at rotating speed 3-titanic acid ester colloid rotates after 6 seconds, its taking-up to be inserted in retort furnace and calcined 5 minutes under 350 ℃ on the ITO conductive glass, and then the cooling room temperature of putting, complete once and film;
Step 4: by the identical mode of step 3, then be coated with membrane operations, carry out continuously 8 times; Then calcined 4 hours under 550 ℃, naturally cooling, and connect wire with copper conductive adhesive; Obtain crude product Ti-Fe after spontaneous curing 2O 3Membrane electrode, stand-by;
Step 5: with above-mentioned crude product Ti-Fe 2O 3Membrane electrode is working electrode, and platinum electrode is to electrode, and saturated calomel electrode is reference electrode, in the NaOH of 1M alkaline electrolyte or 0.5M Na 2SO 4Neutral electrolyte in carry out electrochemical reduction and process, reduction potential-1.2≤E＜-0.6V, time 5-40 minute; Get final product to get Ti-Fe 2O 3Membrane electrode.
2. method according to claim 1 is characterized in that the mol ratio of the Ti:Fe in the colloid of step 2 is 1:10; The volume ratio of concentrated hydrochloric acid consumption and ethanol consumption is 0.13:200.
3. method according to claim 1, is characterized in that titanic acid ester used is butyl (tetra) titanate, titanium propanolate or isopropyl titanate.
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Cited By (6)

* Cited by examiner, † Cited by third party
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CN104134495A (en) * 2014-08-13 2014-11-05 南京大学（苏州）高新技术研究院 Room temperature electrochemical oxidation method of coated conductor superconduction layer
CN109738502A (en) * 2019-01-03 2019-05-10 山东大学 A kind of Fe2O3The preparation method of membrane electrode and its application in optical electro-chemistry glucose sensor
CN111647908A (en) * 2020-07-01 2020-09-11 淮阴工学院 Method for improving photoelectric response of iron oxide nanorod array photoelectric anode
CN112088042A (en) * 2018-05-07 2020-12-15 国立大学法人神户大学 Photocatalyst electrode and method for producing photocatalyst electrode
CN114436370A (en) * 2022-01-25 2022-05-06 中南大学 Ilmenite-based electrode and preparation method and application thereof
CN115231659A (en) * 2022-07-15 2022-10-25 浙江大学 Cocatalyst modified iron-based anode for sewage treatment and method and application thereof

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104134495A (en) * 2014-08-13 2014-11-05 南京大学（苏州）高新技术研究院 Room temperature electrochemical oxidation method of coated conductor superconduction layer
CN112088042A (en) * 2018-05-07 2020-12-15 国立大学法人神户大学 Photocatalyst electrode and method for producing photocatalyst electrode
CN109738502A (en) * 2019-01-03 2019-05-10 山东大学 A kind of Fe2O3The preparation method of membrane electrode and its application in optical electro-chemistry glucose sensor
CN111647908A (en) * 2020-07-01 2020-09-11 淮阴工学院 Method for improving photoelectric response of iron oxide nanorod array photoelectric anode
CN114436370A (en) * 2022-01-25 2022-05-06 中南大学 Ilmenite-based electrode and preparation method and application thereof
CN115231659A (en) * 2022-07-15 2022-10-25 浙江大学 Cocatalyst modified iron-based anode for sewage treatment and method and application thereof
CN115231659B (en) * 2022-07-15 2023-09-08 浙江大学 Co-catalyst modified iron-based anode for sewage treatment and method and application thereof

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