CN109482218B - By using Ni2Method for enhancing photocatalysis by P nano crystal - Google Patents

By using Ni2Method for enhancing photocatalysis by P nano crystal Download PDF

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CN109482218B
CN109482218B CN201811469698.6A CN201811469698A CN109482218B CN 109482218 B CN109482218 B CN 109482218B CN 201811469698 A CN201811469698 A CN 201811469698A CN 109482218 B CN109482218 B CN 109482218B
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silicon wafer
solution
water
array
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CN109482218A (en
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江林
苏菲静
文鹏
梁志强
孙迎辉
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Suzhou University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24—Nitrogen compounds
    • B01J35/23—
    • B01J35/39—
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/024—Multiple impregnation or coating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • B01J37/10—Heat treatment in the presence of water, e.g. steam
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/02—Preparation of oxygen
    • C01B13/0203—Preparation of oxygen from inorganic compounds
    • C01B13/0207—Water
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
    • C01B3/042—Decomposition of water
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Abstract

The invention relates to a method for preparing Ni2The method for enhancing photocatalysis by P nano-crystal comprises the following steps: (a) loading TiO on the surface of a substrate by a hydrothermal method2An array; (b) in the TiO2At least one layer of polystyrene nano film is loaded on the surface of the array; (c) immersing the product of the step (b) into a titanium dioxide sol precursor solution, taking out, drying and calcining in an oxygen atmosphere; subsequently spin-coating Ni-containing layer on the surface2And (3) baking the n-hexane solution of the P nanocrystal in a glove box to remove organic matters. Thus, not only can the inverse structure of the opal fully carry out catalytic reaction, but also Ni2P will also be on TiO2Has good cocatalyst effect.

Description

By using Ni2Method for enhancing photocatalysis by P nano crystal
Technical Field
The invention belongs to the field of nano materials, relates to a photocatalyst, and particularly relates to a photocatalyst prepared from Ni2A method for enhancing photocatalysis by P nanocrystals.
Background
The use of fossil energy not only brings convenience and prosperity of life to people, but also causes environmental pollution, and the fossil energy belongs to renewable energy, so that people are forced to seek cleaner energy. The hydrogen is burnt to release a large amount of energy, and water is generated after burning, so that the hydrogen is clean and pollution-free. At present, there are three main ways of producing hydrogen, which are: the recombination and regeneration of fossil energy, electric catalysis and photocatalysis. But the re-generation of fossil energy still produces CO2And the like, without solving the air problem, electrocatalysis consumes a large amount of energy, and photocatalysis is attracting attention because it utilizes sunlight.
Currently, two systems are mainly adopted for photocatalytic hydrogen production: powder systems and Photoelectrochemical systems (PEC systems). The powder system is that the catalyst is put into water, hydrogen and oxygen are generated under the irradiation of sunlight, but the separation of hydrogen and oxygen is difficult because the hydrogen generation and the oxygen generation are carried out in one catalyst at the same time. The PEC system is in the form of an electrode, and the cathode generates oxygen and the anode generates hydrogen during the reaction, thereby facilitating the effective separation of hydrogen and oxygen. Therefore, a photocatalyst with high selection efficiency, low energy consumption and simple and convenient operation becomes a problem to be solved urgently.
The band position of the photocatalyst should be greater than 1.8eV or more, and thus most photocatalysts are mainly concentrated on metal oxides. Due to TiO2The photocatalyst is nontoxic and harmless, has good chemical stability, corrosion resistance and the like, and becomes the most classical metal oxide photocatalyst. But due to TiO2The forbidden band width of the electron-hole separator is 3.2eV, and larger energy is needed to separate the electron and the hole. Thus how to improve TiO2The photocatalytic performance of (2) has also been a problem of research.
Disclosure of Invention
The invention aims to overcome the defects of the prior artSufficient to provide the use of Ni2A method for enhancing photocatalysis by P nanocrystals.
In order to achieve the purpose, the invention adopts the technical scheme that: by using Ni2The method for enhancing photocatalysis by P nano-crystal comprises the following steps:
(a) loading TiO on the surface of a substrate by a hydrothermal method2An array;
(b) in the TiO2At least one layer of polystyrene nano film is loaded on the surface of the array;
(c) immersing the product of the step (b) into a titanium dioxide sol precursor solution, taking out, drying and calcining in an oxygen atmosphere; subsequently spin-coating Ni-containing layer on the surface2And (3) baking the n-hexane solution of the P nanocrystal in a glove box to remove organic matters.
Optimally, step (a) comprises the steps of:
(a1) adding tetrabutyl titanate into a hydrochloric acid aqueous solution, and stirring until the tetrabutyl titanate is colorless to obtain a first precursor solution;
(a2) immersing a substrate into the first precursor solution, heating the substrate in an oven to perform hydrothermal reaction, cooling and cleaning;
(a3) and (b) calcining the product of the step (a2) in a muffle furnace.
Further, the step (b) comprises the steps of:
(b1) cleaning a silicon wafer, soaking the silicon wafer into a mixed solution of water, hydrogen peroxide and ammonia water for cooking to obtain a hydrophilic surface, then washing the silicon wafer with deionized water and drying the silicon wafer under nitrogen airflow;
(b2) immersing part of the silicon slice treated in the step (b1) into water containing a surfactant, and transferring the polystyrene nanosphere solution to the water surface through the hydrophilic surface to form a polystyrene nanosphere membrane;
(b3) by supporting TiO2And extracting the polystyrene nanosphere film from the substrate of the array, and drying.
Preferably, in the step (c), the titania sol precursor solution is prepared by dissolving titanium isopropoxide in a mixed solution of ethanol and concentrated hydrochloric acid.
Further, in the step (c), the calcining temperature is 400-650 ℃, and the baking temperature is 250-350 ℃.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages: the invention adopts Ni2Method for enhancing photocatalysis by P nanocrystals on TiO2At least one layer of polystyrene nano film is loaded on the surface of the array, so that a titanium dioxide nano structure (namely an opal inverse structure) is constructed by taking the film as a template, and then TiO is coated with the nano film2Ni loading on array and titanium dioxide nanostructure2P nanocrystal, so that not only can the opal reverse structure fully perform catalytic reaction, but also Ni2P will also be on TiO2Has good cocatalyst effect.
Drawings
FIG. 1 shows the use of Ni in the present invention2A flow schematic diagram of a method for enhancing photocatalysis by P nanocrystals;
FIG. 2 is an SEM image of a sample of example 2: (a) TiO 22A front view of the inverse opal structure; (b) TiO 22A cross-sectional view of an opal inverse structure; (c) TiO 22/Ni2A front view of the inverse structure of P-opal; (d) TiO 22/Ni2A cross-sectional view of the inverse structure of P-opal;
FIG. 3 is a plot of the linear voltammogram scan of the sample of example 2;
FIG. 4 is a graph of time-dependent current density under intermittent simulated solar irradiation (external bias 1.23V vs. RHE) for the samples of example 2;
FIG. 5 is a graph of light conversion efficiency as a function of applied bias for the sample of example 2;
FIG. 6 is a graph of incident photon-current conversion efficiency for the sample of example 2;
FIG. 7 is a graph of data on hydrogen and oxygen evolution for the sample of example 2 under simulated solar radiation;
FIG. 8 is a graph of the stability of the sample of example 2 under simulated solar radiation over 24 hours.
Detailed Description
The invention adopts Ni2The method for enhancing photocatalysis by P nano-crystal comprises the following steps: (a) miningMethod for loading TiO on substrate surface by hydrothermal method2An array; (b) in the TiO2At least one layer of polystyrene nano film is loaded on the surface of the array; (c) immersing the product of the step (b) into a titanium dioxide sol precursor solution, taking out, drying and calcining in an oxygen atmosphere; subsequently spin-coating Ni-containing layer on the surface2And (3) baking the n-hexane solution of the P nanocrystal in a glove box to remove organic matters. By reaction on TiO2At least one layer of polystyrene nano film is loaded on the surface of the array, so that a titanium dioxide nano structure (namely an opal inverse structure) is constructed by taking the film as a template, and then TiO is coated with the nano film2Ni loading on array and titanium dioxide nanostructure2P nanocrystal, so that not only can the opal reverse structure fully perform catalytic reaction, but also Ni2P will also be on TiO2Has good cocatalyst effect.
Step (a) preferably comprises the steps of: (a1) adding tetrabutyl titanate into a hydrochloric acid aqueous solution, and stirring until the tetrabutyl titanate is colorless to obtain a first precursor solution; (a2) immersing a substrate into the first precursor solution, heating the substrate in an oven to perform hydrothermal reaction, cooling and cleaning; (a3) and (b) calcining the product of the step (a2) in a muffle furnace. Step (b) preferably comprises the steps of: (b1) cleaning a silicon wafer, soaking the silicon wafer into a mixed solution of water, hydrogen peroxide and ammonia water for cooking to obtain a hydrophilic surface, then washing the silicon wafer with deionized water and drying the silicon wafer under nitrogen airflow; (b2) immersing part of the silicon slice treated in the step (b1) into water containing a surfactant, and transferring the polystyrene nanosphere solution to the water surface through the hydrophilic surface to form a polystyrene nanosphere membrane; (b3) by supporting TiO2And extracting the polystyrene nanosphere film from the substrate of the array, and drying. In the step (c), the titania sol precursor solution is prepared by dissolving titanium isopropoxide in a mixed solution of ethanol and concentrated hydrochloric acid. In the step (c), the calcining temperature is 400-650 ℃, and the baking temperature is 250-350 ℃.
The present invention will be further illustrated with reference to the following examples.
Example 1
This example provides a method of using Ni2P-nanocrystal enhanced photocatalysisThe method, as shown in fig. 1, comprises the following steps:
(a) loading TiO on the surface of a substrate (FTO) by a hydrothermal method2An array; the method specifically comprises the following steps:
(a1) adding 50mL of water and 50mL of concentrated hydrochloric acid (the concentration is 30 wt%) into a 150mL beaker, fully and uniformly stirring to obtain a hydrochloric acid solution, and then adding 2mL of tetrabutyl titanate, and stirring until the solution is colorless to obtain a first precursor solution;
(a2) ultrasonically cleaning fluorine-doped tin oxide (FTO) conductive glass (with the size of 1.0 multiplied by 4.0cm) in acetone, ethanol and deionized water for 10 minutes in sequence, and then drying under nitrogen flow; then leaning against a 25mL polyvinyl fluoride bottle (with the front face facing downwards), taking 10mL of the first precursor solution and adding the first precursor solution into the polyvinyl fluoride bottle, so that the conductive glass is partially immersed in the first precursor solution; putting a polyvinyl fluoride bottle into a reaction kettle, keeping the temperature of the reaction kettle in an oven at 160 ℃ for 1h, and cooling the reaction kettle to room temperature;
(a3) taking out the FTO, repeatedly washing with a large amount of deionized water and ethanol, and naturally drying; placing the dried FTO in a muffle furnace, calcining for 2h at 450 ℃ (the heating and cooling speeds are about 5 ℃/min), cooling to room temperature, and recording to obtain the loaded TiO2FTO of the array;
(b) in the above TiO2At least one layer of polystyrene nano film is loaded on the surface of the array; the method specifically comprises the following steps:
(b1) cutting a silicon wafer of 6cm multiplied by 3cm, sequentially carrying out ultrasonic treatment on the silicon wafer for 5min by using acetone, ethanol and deionized water, and boiling the silicon wafer for half an hour at the temperature of 150 ℃ by using a mixed solution of water, hydrogen peroxide and ammonia water according to the volume ratio of 1:1:4 (the volumes are respectively 20mL, 20mL and 80mL), so that the surface of the silicon wafer achieves a hydrophilic effect; finally, washing with a large amount of deionized water and drying under a nitrogen flow for later use;
(b2) about 300mL of water was added to a clean petri dish with a diameter of 14cm, and about 10 drops of a 2wt% aqueous solution of sodium dodecyl sulfate (SDS, surfactant) was added using a 50mL syringe; placing the silicon wafer processed in step (b1) against the edge of a watch glass, so that part of the silicon wafer is immersed in water and the other part of the silicon wafer is exposed in air; absorbing a Polystyrene (PS) nanosphere solution (with the concentration of 7.5 percent, sold in the market and sigma) with the diameter of 200nm by using a microsyringe, and slowly adding the solution through the surface of a silicon wafer so as to enter the water surface and form a hexagonal close-packed polystyrene nanosphere monolayer; after the dripping is finished, adding 2wt% SDS aqueous solution into a 50mL syringe to stabilize the single-layer membrane;
(b3) by supporting TiO2Extracting a polystyrene nanosphere membrane by using the FTO of the array, and placing the membrane until the moisture is fully dissipated;
(c) vertically immersing the product (i.e. the sample) in the step (b) into a titanium dioxide sol precursor solution (20 mL of ethanol, 0.1mL of commercially available concentrated hydrochloric acid and 0.4mL of titanium isopropoxide are added into a 30mL beaker and ultrasonically mixed) for 1min, and taking out and naturally drying at room temperature; calcining the sample in a muffle furnace at 550 ℃ for 3h (the heating rate and the cooling rate are both about 3/min) to obtain TiO2-an opal inverse structure; using a 100. mu.L pipette to pipette 50. mu.L of Ni2Putting n-hexane solution (with concentration of 2g/L) of P nanocrystal into TiO2Spin coating at 3000r/s speed in the middle of the inverse opal structure; repeating for five times, baking the FTO in a glove box at 320 deg.C to remove organic substances to obtain TiO2/Ni2P opal reverse structure electrode.
Example 2
This example provides a method of using Ni2A method of enhancing photocatalysis by P nanocrystals, substantially in accordance with example 1, except that: repeating the steps (b2) and (b3) once, thereby forming a film on the TiO2Two layers of styrene nanosphere films are attached to the surface of the array; the resulting TiO2The inverse structure of opal is shown in fig. 2(a) -2 (b); TiO finally obtained2/Ni2The inverse structure of P-opal is shown in FIGS. 2(c) -2 (d). As can be seen from FIG. 2(a), the upper and lower layers of the structure using PS beads as templates are staggered, which is favorable for Ni2P nanocrystal is smoothly loaded on TiO2Thereby achieving better catalytic effect; from FIG. 2(b), TiO can be seen2Vertically on the FTO substrate and on the TiO2The structure of the inverse opal structure prepared by taking the PS pellets as a template is just above; from FIGS. 2(c) to 2(d), Ni can be seen2The P nanocrystalline is loaded on the inverse structure of the opal and also on the TiO2Upper loadThis is advantageous in that not only the inverse opal structure is sufficiently reacted in the catalytic process, but also Ni2P to TiO2Also has very good cocatalyst effect.
Example 3
This example provides a method of using Ni2A method of enhancing photocatalysis by P nanocrystals, substantially in accordance with example 1, except that: repeating the steps (b2) and (b3) twice, thereby obtaining a mixture of TiO and TiO2Three layers of styrene nanosphere films are attached to the surface of the array.
Comparative example 1
This example provides only one type of TiO2A method of preparing an array, which is in accordance with step (a) of example 1.
The TiO prepared in example 22Opal reverse structure, TiO2/Ni2Inverse structure of P-opal and TiO in comparative example 12The arrays were subjected to performance testing, the results of which are shown in fig. 3-8. FIG. 3 shows that TiO2、TiO2Inverse opal structure and TiO2/Ni2A group of volt-ampere linear scanning data of the three photoelectrode with P opal reverse structure under illumination condition, and the starting potential of the three photoelectrode under illumination condition is about 0.3V (relative to RHE); when the applied potential exceeds 0.3V, the current density increases rapidly and saturation is reached quickly, indicating that these photoelectrodes have very good photogenerated carrier separation and absorption. Fig. 4 shows the time-varying photoelectric density under intermittent illumination conditions, which is a test to show the photoelectric response behavior under continuous visible light irradiation, consistent with the incident photon-current conversion efficiency of fig. 6. In FIG. 6 TiO2、TiO2The opal reverse structure electrode does not show considerable photoelectric response under continuous visible light irradiation, while TiO2/Ni2The inverse P-opal structure electrode shows transient and significantly photo-responsive behavior. This is probably because of Ni2The P nanocrystal can rapidly capture TiO2Holes are generated under light conditions. FIG. 5 shows the photoelectric conversion efficiency, and it can be seen from the graph that TiO is used as the material for the photoelectric conversion element2、 TiO2Inverse structure of opalWith TiO2/Ni2The maximum photoelectric conversion efficiency of the three electrodes with the P opal inverse structure is 0.2%, 0.3% and 0.86% respectively. Fig. 7 shows the precipitation data of hydrogen and oxygen generated by the crystal form photoelectrochemistry synergistic decomposition of water under the illumination condition of four photoelectrodes. For all electrodes, hydrogen and oxygen were deposited at a stoichiometry of 2:1 on the platinum counter and working electrodes, respectively. From the evolution data in the figure, it can be seen that the quantities of photoelectrochemically evolved hydrogen of the three photoelectrodes are in the order from the largest: TiO 22(3.1μmol)<TiO2Opal inverse structure (5.9 mu mol)<TiO2/Ni2P opal inverse structure (27.6. mu. mol). FIG. 8 shows the TiO content in 24 hours2、TiO2Inverse opal structure and TiO2/Ni2The three electrodes with P opal inverse structures have stability under the illumination condition, and the current density of the three electrodes is not changed greatly before and after 24 hours of reaction, which indicates that the three electrodes have good stability.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.

Claims (3)

1. By using Ni2The method for enhancing photocatalysis by using P nanocrystals is characterized by comprising the following steps of:
(a) loading TiO on the surface of a substrate by a hydrothermal method2An array;
(b) in the TiO2At least one layer of polystyrene nano film is loaded on the surface of the array; the step (b) comprises the steps of:
(b1) cleaning a silicon wafer, soaking the silicon wafer into a mixed solution of water, hydrogen peroxide and ammonia water for cooking to obtain a hydrophilic surface, then washing the silicon wafer with deionized water and drying the silicon wafer under nitrogen airflow;
(b2) adding 300mL of water into a clean surface dish with the diameter of 14cm, and adding 10 drops of 2wt% aqueous solution of sodium dodecyl sulfate into the clean surface dish by using a 50mL syringe; placing the silicon wafer processed in step (b1) against the edge of a watch glass, so that part of the silicon wafer is immersed in water and the other part of the silicon wafer is exposed in air; absorbing a Polystyrene (PS) nanosphere solution with the diameter of 200nm and the concentration of 7.5% by using a microsyringe, slowly adding the solution through the surface of a silicon wafer, and then enabling the solution to enter the water surface to form a hexagonal close-packed polystyrene nanosphere monolayer; after the dripping is finished, adding 2wt% SDS aqueous solution into a 50mL syringe to stabilize the single-layer membrane;
(b3) by supporting TiO2Extracting the polystyrene nanosphere film from the substrate of the array, and drying;
(c) immersing the product of the step (b) into a titanium dioxide sol precursor solution, taking out, drying and calcining in an oxygen atmosphere; subsequently spin-coating Ni-containing layer on the surface2Baking the n-hexane solution of the P nanocrystal in a glove box to remove organic matters; the titanium dioxide sol precursor solution is prepared by dissolving titanium isopropoxide in a mixed solution of ethanol and concentrated hydrochloric acid.
2. The use of Ni as claimed in claim 12The method for enhancing photocatalysis by P nanocrystals is characterized in that the step (a) comprises the following steps:
(a1) adding tetrabutyl titanate into a hydrochloric acid aqueous solution, and stirring until the tetrabutyl titanate is colorless to obtain a first precursor solution;
(a2) immersing a substrate into the first precursor solution, heating the substrate in an oven to perform hydrothermal reaction, cooling and cleaning;
(a3) and (b) calcining the product of the step (a2) in a muffle furnace.
3. The use of Ni as claimed in claim 12The method for enhancing photocatalysis by using P nanocrystals is characterized by comprising the following steps: in the step (c), the calcining temperature is 400-650 ℃, and the baking temperature is 250-350 ℃.
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CN110681403A (en) * 2019-10-24 2020-01-14 吉林师范大学 Preparation method of defective titanium dioxide/nickel phosphide heterojunction visible-light-induced photocatalyst
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