CN110359058B - Preparation method of lead zirconate titanate modified hematite nanorod array photoanode - Google Patents
Preparation method of lead zirconate titanate modified hematite nanorod array photoanode Download PDFInfo
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Abstract
The invention belongs to the field of photoelectric materials and catalysis, and particularly relates to a preparation method of a lead zirconate titanate modified hematite nanorod array photoanode, which comprises the following steps: s1, preparing alpha-Fe2O3The growth solution comprises a ferric salt and an auxiliary agent, and Fe in the growth solution3+The concentration is 0.15-0.3M; the auxiliary agent is sodium nitrate or urea; s2, immersing a conductive substrate into the growth liquid, and reacting for 4-12 hours at the temperature of 95-100 ℃; s3, preparing a lead zirconate titanate precursor solution; s4, spin-coating the precursor solution prepared in the step S3 on the conductive substrate processed in the step S2; and S5, calcining the conductive substrate after the spin coating in the step S4. The photo-anode prepared by the invention solves the problem that the hematite is fast in photoproduction electron hole recombination, improves the photoelectrocatalysis performance and stability, and can be better applied to catalytic hydrogen production.
Description
Technical Field
The invention belongs to the field of catalysis, and particularly relates to a preparation method of a lead zirconate titanate modified hematite nanorod array photoanode.
Background
With the decreasing of fossil fuel, solar energy has become an important part of energy used by human as an inexhaustible clean energy, however, the utilization efficiency of solar energy is low due to the dispersion and instability of solar energy. On the other hand, hydrogen has a high combustion heat value, and pollutants are not generated after combustion, so that hydrogen is known as one of the most green energy sources in the world. Therefore, the hydrogen production by solar energy (electro) catalytic decomposition of water is one of the ideal ways to solve the problems of energy shortage and environmental pollution at present.
Hematite (iron oxide alpha-Fe)2O3) As a narrow band gap (-2.1 eV) n-type semiconductor, the material has the advantages of strong ultraviolet and visible light absorption capability, excellent stability, low cost and the like, and is widely concerned by scientists as a photo-anode material. However, hematite has the defects of poor conductivity, serious photocarrier recombination, slow surface oxygen evolution kinetics and the like, and the hydrogen production efficiency of hematite is severely limited.
Disclosure of Invention
Aiming at the problem that the photo-generated carriers generated by a pure hematite photoanode prepared by the conventional hydrothermal method after illumination are seriously compounded, a layer of lead zirconate titanate film is loaded on the surface of a pure hematite nanorod through a simple spin coating process; because the lead zirconate titanate is a ferroelectric material, after the hematite nanorod is excited by light to generate electrons and holes, the internal electric field of the lead zirconate titanate film can influence the charge distribution in the hematite, so that the electrons and the holes are separated in space, and the recombination of the electrons and the holes is inhibited, thereby improving the efficiency of water photolysis; the lead zirconate titanate modified hematite nanorod composite photo-anode shows more excellent stability and photocatalytic hydrogen production performance.
The invention aims to overcome the problems in the prior art and provides a preparation method of a lead zirconate titanate modified hematite nanorod array photoanode.
Another object of the present invention is to provide a photo-anode prepared by the above method.
The invention also aims to provide the application of the photoanode in hydrogen production by photoelectrocatalytic decomposition of water.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a lead zirconate titanate modified hematite nanorod array photoanode comprises the following steps:
s1, preparing alpha-Fe2O3The growth solution comprises a ferric salt and an auxiliary agent, and Fe in the growth solution3+The concentration is 0.15-0.3M; the auxiliary agents are: sodium nitrate with the concentration of 1-2M or urea with the concentration of 0.1-0.2M;
s2, immersing a conductive substrate into the growth solution, and reacting for 4-12 hours at the temperature of 95-100 ℃ to generate an FeOOH film on the conductive substrate;
s3, preparing a lead zirconate titanate precursor solution, wherein the solute of the precursor solution is composed of lead acetate trihydrate, n-butyl zirconium and tetrabutyl titanate according to the molar ratio of 1.1: x (1-x) to 0.1-0.4, and the solvent is methanol or ethylene glycol monomethyl ether;
s4, spin-coating the precursor solution prepared in the step S3 on the FeOOH film formed on the substrate in the step S2;
s5, calcining the conductive substrate subjected to spin coating in the step S4 at 550-750 ℃ for 120-300 min.
The growth liquid in the above step S1 uses water as a solvent.
Lead zirconate titanate (PZT) is a ferroelectric material, and its spontaneous polarization can promote the formation of a uniform internal electric field inside the material, and promote the separation of electron-hole pairs in itself and in adjacent semiconductors, but its poor conductivity and wide band gap structure lead to low utilization of solar energy. Hematite has also been limited in its application to the field of photocatalysis due to poor electrical conductivity and the problem of photogenerated carrier recombination. The composite photo-anode obtained by modifying the conductive substrate by hematite and lead zirconate titanate for the first time has good photoelectric effect and catalytic effect. The problem of electron-hole recombination of hematite is effectively solved by utilizing the spontaneous polarization effect of lead zirconate titanate. On the other hand, the current of the composite light anode is obviously improved, the conductivity is greatly improved, and the composite material is not easy to generate light corrosion and has better stability.
Preferably, in step S3, x = 0.2.
Preferably, the spin coating of the precursor solution in the step S4 is completed in two steps, wherein the first step is maintained at 500-1000rpm for 5-10S; the second step 3000-.
The invention is completed in two steps when the precursor solution is spin-coated on the conductive substrate. If repeated too many times, the lead zirconate titanate layer may be too thick, which may affect the hematite light absorption and carrier transport. The two-step spin coating is adopted to complete the preparation, the thickness of the lead zirconate titanate layer on the surface of the obtained composite electrode is moderate, and the surface aperture of the material is moderate and is more suitable for photocatalysis.
Preferably, the calcining of step S5 adopts a temperature rise rate of 5 ℃/min to raise the temperature to 550-750 ℃.
Preferably, the conductive substrate is conductive glass, a silicon wafer, a titanium foil or a copper foil.
Preferably, in step S2, the conductive substrate is immersed in the growth solution for reaction by hydrothermal synthesis using a stainless steel reaction kettle lined with polytetrafluoroethylene.
Compared with the prior art, the invention has the following technical effects:
the invention loads a layer of lead zirconate titanate film on the surface of a pure hematite nanorod through a simple spin coating process; because the lead zirconate titanate is a ferroelectric material, after the hematite nanorod is excited by light to generate electrons and holes, the internal electric field of the lead zirconate titanate film can influence the charge distribution in the hematite, so that the electrons and the holes are separated in space, and the recombination of the electrons and the holes is inhibited, thereby improving the efficiency of water photolysis; the lead zirconate titanate modified hematite nanorod composite electrode shows more excellent stability and photocatalytic hydrogen production performance. A layer of lead zirconate titanate thin layer is loaded on the hematite nanorod by adopting a simple spin coating-annealing method, and the method is simple in process and easy to operate.
Drawings
FIG. 1 is a surface topography of a composite electrode;
FIG. 2 Linear sweep voltammogram of a composite electrode, hematite electrode;
FIG. 3 switching photocurrent density versus time curves for a composite electrode, hematite electrode, under a bias of 0.23V vs Ag/AgCl;
FIG. 4 shows a composite electrode stability performance test curve; and
FIG. 5 XRD contrast for composite electrode, simple hematite electrode and lead zirconate titanate powder.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below with reference to specific examples and comparative examples. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Unless otherwise specified, the equipment used in the present examples, comparative examples and experimental examples was conventional experimental equipment, and the materials and reagents used were commercially available.
Example 1
A preparation method of a lead zirconate titanate modified hematite nanorod array photoanode comprises the following steps:
s1, preparing FeCl containing 0.3M3·6H2O (0.3 mol/L) and 2M NaNO3(2 mol/L) of the aqueous solution as a growth liquid of the hematite;
s2, taking conductive glass as a conductive substrate, obliquely placing the conductive glass in a stainless steel reaction kettle with a polytetrafluoroethylene lining, enabling the conductive surface to face downwards, and pouring a precursor solution into the lining until 3/4 of the lining is filled; placing the reaction kettle in an oven, heating at 100 ℃ for 8h, naturally cooling to room temperature, synthesizing a FeOOH film on conductive glass by a hydrothermal synthesis method, cleaning with deionized water, and drying in the air for later use;
s3, preparing a lead zirconate titanate precursorAnd (3) a bulk solution. 0.22M Pb (CH)3COO)2·3H2O (10% excess), 0.04M Zr (OC)4H9)4And 0.16M Ti (OC)4H9)4Dissolving in methanol or ethylene glycol monomethyl ether, and stirring at 60 deg.C for about 60min until solute is completely dissolved;
s4, spin-coating the lead zirconate titanate precursor solution in the step S3 on the FeOOH film obtained in the step S1 under the spin-coating condition of maintaining at 500rpm for 5S and then maintaining at 4000rpm for 30S. Repeating the spin coating process for 3 times;
s5, placing the conductive substrate with the lead zirconate titanate/FeOOH film in the step S3 in a muffle furnace, heating to 700 ℃ at a speed of 5 ℃/min, preserving heat for 3h, and naturally cooling to room temperature.
Example 2
A preparation method of a lead zirconate titanate modified hematite nanorod array photoanode is different from that of example 1 in that: the hematite growth liquid in the step S1 is 0.15M FeCl3·6H2O and 1M NaNO3An aqueous solution of (a); the reaction temperature is 95 ℃ and the reaction time is 4 h.
Example 3
A preparation method of a lead zirconate titanate modified hematite nanorod array photoanode is different from that of example 1 in that: the hematite growth liquid in the step S1 is 0.15M FeCl3·6H2An aqueous solution of O and 0.2M urea; the reaction temperature is 100 ℃, and the reaction time is 12 h.
Example 4
A preparation method of a lead zirconate titanate modified hematite nanorod array photoanode is different from that of example 1 in that: after the temperature is raised to 650 ℃ in the step S4, the heat preservation time is 1 h.
Example 5
A preparation method of a composite photoanode, which is different from that of example 1 in that: in this embodiment, the spin coating conditions in step S4 were 500rpm maintained for 10S, and then 4000rpm maintained for 40S. This spin coating process was repeated 3 times.
Example 6
Lead zirconate titanate repairThe preparation method of the decorated hematite nanorod array photoanode is different from that of the example 1 in that: the solute of the lead zirconate titanate precursor solution in the step S3 is 0.33M Pb (CH)3COO)2·3H2O (10% excess), 0.06M Zr (OC)4H9)4 and 0.24M Ti (OC)4H9)4。
Comparative example 1
A preparation method of a lead zirconate titanate modified hematite nanorod array photoanode is different from that of example 1 in that: the spin coating process of step S4 in this embodiment is repeated 10 times.
This comparative example spin-coating step was repeated a greater number of times. The thickness of the obtained lead zirconate titanate layer is thicker, and the excessively thick lead zirconate titanate layer influences the light absorption of hematite and the transmission of carriers, so that the photocatalytic performance is influenced.
Comparative example 2
A preparation method of a lead zirconate titanate modified hematite nanorod array photoanode is different from that of example 1 in that: the spin coating condition in step S4 in this example was 6000rpm spin coating for 60S.
This comparative example employed one spin coating. The obtained lead zirconate titanate layer is not uniformly distributed, and the contact between the electrode material and the conducting solution is influenced by the non-uniform surface aperture of the material, so that the catalytic performance is influenced.
Comparative example 3
The preparation process of the modified lead zirconate titanate/hematite nanorod core-shell structure composite photoanode is the same as that in example 1, except that in the step S3 in the embodiment, Pb (CH) in the lead zirconate titanate precursor solution is used3COO)2·3H2O content was 0.2M (without excess), and under this test condition, the film component obtained was not completely Pb (Zr) due to loss of lead during heating0.8Ti0.2)O3The performance improvement effect is significantly lower than that of the sample obtained under the experimental conditions in example 1.
Performance testing
The sample obtained in example 1 above was subjected to a performance test.
All samplesThe photoelectric electrochemical test of the product is carried out by using a 300W xenon lamp and an AM1.5 optical filter at 100mW/cm2The test was performed under simulated sunlight with 1M NaOH solution as the electrolyte solution, using a three-electrode system, i.e. Ag/AgCl as the reference electrode, Pt sheet as the counter electrode, and the prepared sample as the working electrode.
The test results are shown in fig. 1 to 4.
FIG. 1 is a scanning electron microscope picture of the modified lead zirconate titanate/hematite nanorod core-shell structure composite photoanode prepared in example 1, and as can be seen from the scanning electron microscope in FIG. 1, a hematite nanorod grows perpendicular to FTO, and the length of the hematite nanorod is about 400-500 nm; the top end of the nano rod is covered with a lead zirconate titanate layer with the thickness of about 80 nm.
Fig. 2 is a linear sweep voltammogram of the hematite, lead zirconate titanate/hematite composite photoanode prepared in example 1. As can be seen from FIG. 2, compared with a hematite photoanode not loaded with lead zirconate titanate, the photocurrent of the lead zirconate titanate/hematite composite photoanode is greatly improved, which indicates that the lead zirconate titanate reduces the composition of photon-generated carriers, and has an effect of improving the catalytic performance of the hematite photoanode system.
FIG. 3 shows that the hematite, lead zirconate titanate/hematite composite photoanode prepared in example 1 is at 0.23VvsSwitching photocurrent density-time curves under bias of Ag/AgCl; as can be seen from FIG. 3, at 0.23VvsUnder the voltage of Ag/AgCl, the photocurrent density of the lead zirconate titanate/hematite composite photoanode reaches 0.96 mA/cm2(curve 2), 48 times that of the hematite photoanode not loaded with lead zirconate titanate (curve 1). The samples obtained under the conditions of the comparative example 1 (curve 3) and the comparative example 2 (curve 4) are improved compared with the pure hematite sample, but have larger performance difference with the samples obtained under the conditions of the example 1. The results show that the load of the lead zirconate titanate improves the problem that the hematite is faster in photoproduction electron hole recombination, and improves the photoelectrocatalysis performance of the hematite.
FIG. 4 shows that the lead zirconate titanate/hematite composite photoanode prepared in example 1 is at 0.23VvsThe current density-time curve under the bias of Ag/AgCl shows that the electricity is generated within 120h of illumination timeThe flow keeps 80% of the initial current, which shows that the composite light anode has better stability under simulated sunlight. Compared with traditional Co-Pi and CdS promoters, the lead zirconate titanate is not easy to generate light corrosion and has better practicability.
Fig. 5 is an XRD comparison graph of the modified lead zirconate titanate/hematite nanorod core-shell structure composite photoanode prepared in example 1, a simple hematite photoanode, and lead zirconate titanate powder, which shows that lead zirconate titanate is successfully loaded on hematite.
In summary, in the above embodiments, after the thin layer of lead zirconate titanate is loaded on the surface of the hematite nanorod, and after the hematite nanorod is excited by light to generate electrons and holes, the thin layer of lead zirconate titanate on the surface has a spontaneous polarization property, so that charge distribution in adjacent hematite is affected, photo-generated electrons and holes are spatially separated, and recombination of the photo-generated electrons and holes is reduced, thereby improving the efficiency of water photolysis; the modified lead zirconate titanate/hematite nanorod core-shell structure composite electrode shows more excellent stability and photocatalytic hydrogen production performance.
It should be finally noted that the above examples are only intended to illustrate the technical solutions of the present invention, and not to limit the scope of the present invention, and that other variations and modifications based on the above description and thought may be made by those skilled in the art, and that all embodiments need not be exhaustive. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (8)
1. A preparation method of a lead zirconate titanate modified hematite nanorod array photoanode is characterized by comprising the following steps:
s1, preparing alpha-Fe2O3The growth solution comprises a ferric salt and an auxiliary agent, and Fe in the growth solution3+The concentration is 0.15-0.3M; the auxiliary agents are: sodium nitrate with the concentration of 1-2M or urea with the concentration of 0.1-0.2M;
s2, immersing a conductive substrate into the growth liquid, and reacting for 4-12 hours at the temperature of 95-100 ℃;
s3, preparing a lead zirconate titanate precursor solution, wherein the solute of the precursor solution is prepared by mixing lead acetate trihydrate, n-butyl zirconium and tetrabutyl titanate according to the molar ratio of 1.1: x (1-x), x is more than or equal to 0.1 and less than or equal to 0.4, and the solvent is methanol or ethylene glycol monomethyl ether;
s4, spin-coating the precursor solution prepared in the step S3 on the conductive substrate processed in the step S2; the spin coating is completed in two steps, wherein the first step is maintained at 500-1000rpm for 5-10 s; the second step is maintained at 3000-4000rpm for 25-35 s, and the first step and the second step are repeated for 2-3 times;
s5, calcining the conductive substrate subjected to spin coating in the step S4 at 550-750 ℃ for 120-300 min.
2. The method for preparing the lead zirconate titanate-modified hematite nanorod array photoanode as claimed in claim 1, wherein in the step S3, x = 0.2.
3. The method for preparing the lead zirconate titanate modified hematite nanorod array photoanode as claimed in claim 1, wherein the step S5 comprises raising the temperature to 550-750 ℃ by a temperature raising rate of 5 ℃/min.
4. The method for preparing the lead zirconate titanate modified hematite nanorod array photoanode as claimed in claim 1, wherein the conductive substrate is conductive glass, a silicon wafer, a titanium foil or a copper foil.
5. The method for preparing the lead zirconate titanate modified hematite nanorod array photoanode as claimed in claim 1, wherein the growth solution in the step S1 adopts water as a solvent.
6. The method for preparing the lead zirconate titanate modified hematite nanorod array photoanode as claimed in claim 1, wherein in step S2, a stainless steel reaction kettle lined with polytetrafluoroethylene is used to immerse a conductive substrate into the growth solution for reaction through a hydrothermal synthesis method.
7. A photoanode prepared by the method for preparing a lead zirconate titanate-modified hematite nanorod array photoanode according to claim 1.
8. The use of the photoanode of claim 7 in the photoelectrocatalytic decomposition of water to produce hydrogen.
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