CN110203964B - Preparation of laser-induced metal sulfide/three-dimensional porous graphene composite photoelectrode - Google Patents
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Abstract
A preparation method of a laser-induced metal sulfide/three-dimensional porous graphene composite photoelectrode adopts a laser-induced preparation mode. Dissolving a metal ion complex into a polysulfone polymer solution, spin-coating the obtained viscous solution on the surface of indium tin oxide conductive glass, heating to volatilize the solvent, forming a metal ion-doped polysulfone polymer film on the surface of the indium tin oxide conductive glass, and utilizing CO 2 And scanning the surface of the metal ion doped polysulfone polymer film by laser to prepare the metal sulfide/three-dimensional porous graphene composite photoelectrode.
Description
Technical Field
The invention relates to a novel laser-induced in-situ and synchronous preparation method of a metal sulfide/three-dimensional porous graphene composite photoelectrode.
Background
Photo-electrochemical sensing is an analytical technique with great development prospect, and due to the different energy forms of an excitation source (light) and an output signal (current), background signals can be greatly reduced, the sensitivity can be remarkably improved, and the photo-electrochemical sensing attracts wide attention in the field of analytical chemistry. During the past decade, researchers have been working on the construction of photo-electrochemical sensing platforms using various metal sulfides as the photoactive material of the photoelectrode, such as cadmium sulfide, lead sulfide, bismuth sulfide, and silver sulfide. In order to further improve the photocurrent conversion efficiency, researchers combine metal sulfides with binary metal oxide semiconductors, ternary metal oxide semiconductors and carbonitrides to prepare various metal sulfide composite materials, and the sensitivity of the metal sulfide-based photoinduced electrochemical sensor is greatly improved. Graphene, as an excellent carrier transfer carrier, has been widely used for constructing heterojunction composite materials of metal sulfides, and can effectively inhibit the recombination of electrons and holes in the metal sulfides, thereby improving the photocurrent conversion efficiency of the metal sulfides. However, the conventional method for preparing the metal sulfide/graphene composite photoelectrode generally includes a plurality of tedious steps, such as: the preparation method comprises the following steps of graphene preparation, metal sulfide preparation, graphene and metal sulfide assembly, modification and protection of a metal sulfide/graphene composite material on the surface of an electrode and the like. Therefore, the patent develops a novel method for preparing the metal sulfide/three-dimensional porous graphene composite photoelectrode aiming at the problem, and the polysulfone polymer is simultaneously used as a carbon source and a sulfur source to convert the metal complex doped polysulfone polymer film on the surface of the indium tin oxide conductive glass into the metal sulfide/three-dimensional porous graphene composite material in situ and synchronously so as to form the composite photoelectrode with excellent photo-induced electrochemical performance. The method is simple, stable and strong in universality, and can realize mass preparation.
Disclosure of Invention
The invention aims to provide a preparation method of a laser-induced metal sulfide/three-dimensional porous graphene composite photo-electrode based on a polysulfone polymer film.
The technical scheme of the invention is as follows
A preparation method of a laser-induced metal sulfide/three-dimensional porous graphene composite photoelectrode is shown in figure 1 and adopts a laser-induced preparation mode. Dissolving a metal ion complex into a polysulfone polymer solution, spin-coating the obtained viscous solution on the surface of indium tin oxide conductive glass, heating to volatilize the solvent, forming a metal ion-doped polysulfone polymer film on the surface of the indium tin oxide conductive glass, and utilizing CO 2 And scanning the surface of the metal ion doped polysulfone polymer film by laser to prepare the metal sulfide/three-dimensional porous graphene composite photoelectrode.
The metal ion complex is cadmium acetylacetonate, cadmium porphyrin, cadmium acetate, lead acetylacetonate, lead porphyrin and lead acetate.
The polysulfone polymer is polysulfone, polyethersulfone or polyphenylsulfone.
The preparation method of the laser-induced metal sulfide/three-dimensional porous graphene composite photoelectrode comprises the following steps:
step 1, adding 0.8-1.2 g of metal ion complex into 20-30 mL of N, N-dimethylformamide solution, and magnetically stirring to completely dissolve the metal ion complex;
step 2, adding 2.0-3.0 g of polysulfone polymer into the solution obtained in the step 1 for 3-5 times (with the time interval of 20-30 minutes), and continuously stirring to form a solution containing the metal ion polysulfone polymer with certain viscosity;
step 3, spin-coating the solution containing the metal ion polysulfone polymer synthesized in the step 2 on the surface of the indium tin oxide conductive glass which is cleaned, and forming a uniform film containing the metal ion polysulfone polymer solution on the surface of the indium tin oxide conductive glass, wherein the spin-coating speed is 2000-3000 r/min, and the spin-coating time is 80-100 s;
step 4, carrying out vacuum heat preservation on the indium tin oxide conductive glass modified by the metal ion-containing polysulfone polymer solution film obtained in the step 3 at the temperature of 75-100 ℃ for 1-3 h, so that a solvent is volatilized, and thus the metal ion-doped polysulfone polymer film is prepared on the surface of the indium tin oxide conductive glass;
step 5, cooling the metal ion doped polysulfone polymer film obtained in the step 4 to room temperature, and adding CO 2 Laser cutting carving machine working platform using CO 2 The method comprises the steps of scanning the surface of a metal ion doped polysulfone polymer film by laser, and directly converting the metal ion doped polysulfone polymer film on the surface of indium tin oxide conductive glass into metal sulfide/three-dimensional porous graphene in situ. The laser engraving parameters are as follows: the laser power is 4.0-4.8 w, the laser engraving speed is 166-250 mm/s, the laser engraving resolution is 600-1200, and the laser defocusing distance is 0.2-0.4 cm.
The preparation principle of the laser-induced metal sulfide/three-dimensional porous graphene composite photoelectrode based on the polysulfone polymer film is as follows:
during the laser engraving process, due to CO 2 The photo-thermal effect of the laser can increase the local instantaneous temperature of the metal ion doped polysulfone polymer film to nearly 3000 ℃, and sp in the polysulfone polymer film 3 Conversion of hybrid carbon to sp 2 And hybridizing carbon, and finally highly graphitizing the polysulfone polymer film containing a large number of benzene ring structures to generate the graphene. The vigorous graphitization process is accompanied by the release of gases such as water vapor and nitrogen to form a porous structure. Meanwhile, sulfur elements in the polysulfone polymer are subjected to carbothermic reduction in the presence of metal ions to form metal sulfide nano particles which are uniformly attached to the three-dimensional porous graphene, so that the metal sulfide/three-dimensional porous graphene composite photoelectrode is prepared.
Compared with the prior art, the invention has the following characteristics:
the invention provides a novel laser-induced in-situ and synchronous preparation method of a metal sulfide/three-dimensional porous graphene composite photoelectrode, which has the following characteristics compared with the traditional preparation method of a metal sulfide/graphene composite material:
(1) The novel laser-induced preparation method can directly, in-situ and synchronously generate the metal sulfide/three-dimensional porous graphene composite photoelectric material on the surface of the indium tin oxide conductive glass, has the characteristics of simple and rapid operation steps, accurate and controllable electrode area and strong universality, and can realize mass preparation;
(2) The metal sulfide/three-dimensional porous graphene composite photoelectrode prepared by laser induction has high stability and good repeatability, can be repeatedly used for more than 30 times, and can be stably stored for more than 10 months at room temperature.
Drawings
FIG. 1 is a schematic diagram of a preparation process of a metal sulfide/three-dimensional porous graphene composite photoelectrode.
Detailed Description
Example 1 preparation of a cadmium sulfide/three-dimensional porous graphene composite photoelectrode:
preparing a polyether sulfone solution containing cadmium ions: adding 0.8 g of acetylacetone cadmium into 20 mL of N, N-dimethylformamide, magnetically stirring to completely dissolve the acetylacetone cadmium, then adding 2.5 g of polyethersulfone for 5 times (time interval is 2 hours), and continuously stirring to form a polyethersulfone solution containing cadmium ions and having certain viscosity;
preparing the indium tin oxide conductive glass modified by the polyether sulfone film containing cadmium ions: spin-coating the solution containing the cadmium ions to the surface of the indium tin oxide conductive glass which is cleaned, wherein the spin-coating speed is 1000 r/min, the spin-coating time is 60 s, forming a uniform film containing the cadmium ions on the surface of the indium tin oxide conductive glass, and carrying out vacuum heat preservation on the obtained film containing the cadmium ions at the temperature of 100 ℃ for 2 h to volatilize the solvent, so that the cadmium ion-doped polyether sulfone film is prepared on the surface of the indium tin oxide conductive glass;
preparing a cadmium sulfide/three-dimensional porous graphene composite photo-electrode by laser induction: modifying the obtained cadmium ion doped polyether sulfone film with indium oxideCooling the tin conductive glass to room temperature, adding CO 2 Laser cutting carving machine working platform using CO 2 The method comprises the steps of scanning the surface of a cadmium ion doped polyether sulfone film by laser, and directly converting the cadmium ion doped polyether sulfone film on the surface of indium tin oxide conductive glass into a cadmium sulfide/three-dimensional porous graphene composite photoelectrode in situ. The laser engraving parameters were as follows: the laser power is 4.0W, the laser engraving speed is 166 mm/s, the laser engraving resolution is 1200, and the laser defocusing distance is 0.3 cm.
Example 2. Preparation of a lead sulfide/three-dimensional porous graphene composite photoelectrode:
preparing a polysulfone solution containing lead ions: adding 1.0 g of acetylacetone lead into 20 mL of N, N-dimethylformamide, carrying out magnetic stirring to completely dissolve the acetylacetone lead, then adding 2.5 g of polysulfone into the solution for 5 times (with the time interval of 2 hours), and continuously stirring to form a lead ion polysulfone solution with certain viscosity;
preparing lead ion-containing polysulfone film modified indium tin oxide conductive glass: spin-coating the lead ion-containing polysulfone solution on the surface of the cleaned indium tin oxide conductive glass at the spin-coating speed of 800 r/min for 80 s to form a uniform lead ion-containing polysulfone solution film on the surface of the indium tin oxide conductive glass, and carrying out vacuum heat preservation on the obtained lead ion-containing polysulfone solution film at the temperature of 100 ℃ for 2 h to volatilize the solvent, thereby preparing a lead ion-doped polysulfone film on the surface of the indium tin oxide conductive glass;
preparing a leaded sulfur three-dimensional porous graphene composite photo-electrode by laser induction: cooling the obtained lead ion doped polysulfone membrane to room temperature, and adding CO 2 Laser cutting carving machine working platform using CO 2 The method comprises the steps of scanning the surface of a lead ion doped polysulfone membrane by laser, and directly converting the lead ion doped polysulfone membrane on the surface of indium tin oxide conductive glass into a lead sulfide/three-dimensional porous graphene composite photoelectrode in situ. The laser engraving parameters were as follows: the laser power is 4.5W, the laser engraving speed is 196 mm/s, the laser engraving resolution is 1200, and the laser defocusing distance is 0.3 cm.
Claims (3)
1. Preparation of laser-induced metal sulfide/three-dimensional porous graphene composite photoelectrodeThe preparation method adopts a laser-induced preparation mode. Dissolving a metal ion complex into a polysulfone polymer solution, spin-coating the obtained viscous solution on the surface of indium tin oxide conductive glass, heating to volatilize the solvent, forming a metal ion-doped polysulfone polymer film on the surface of the indium tin oxide conductive glass, and utilizing CO 2 And scanning the surface of the metal ion doped polysulfone polymer film by laser to prepare the metal sulfide/three-dimensional porous graphene composite photoelectrode. The metal ion complex is cadmium acetylacetonate, cadmium porphyrin, cadmium acetate, lead acetylacetonate, lead porphyrin and lead acetate; the polysulfone polymer is polysulfone, polyethersulfone and polyphenylsulfone.
2. The method for preparing the laser-induced metal sulfide/three-dimensional porous graphene composite photoelectrode according to claim 1, which is characterized by comprising the following steps:
step 1, adding 0.8-1.2 g of metal ion complex into 20-30 mL of N, N-dimethylformamide solution, and magnetically stirring to completely dissolve the metal ion complex;
step 2, adding 2.0-3.0 g of polysulfone polymer into the solution obtained in the step 1 for 3-5 times at the time interval of 20-30 minutes, and continuously stirring to form a solution of the polysulfone polymer containing metal ions and having a certain viscosity;
step 3, spin-coating the metal ion-containing polysulfone polymer solution synthesized in the step 2 on the surface of the indium tin oxide conductive glass which is cleaned, and forming a uniform metal ion-containing polysulfone polymer solution film on the surface of the indium tin oxide conductive glass, wherein the spin-coating speed is 2000-3000 r/min, and the spin-coating time is 80-100 s;
step 4, carrying out vacuum heat preservation on the indium tin oxide conductive glass modified by the metal ion-containing polysulfone polymer solution film obtained in the step 3 at the temperature of 75-100 ℃ for 1-3 h, so that a solvent is volatilized, and thus the metal ion-doped polysulfone polymer film is prepared on the surface of the indium tin oxide conductive glass;
step 5, cooling the metal ion doped polysulfone polymer film obtained in the step 4 to room temperature, and adding CO 2 Laser cutting carving machine working platform using CO 2 The method comprises the steps of scanning the surface of a metal ion doped polysulfone polymer film by laser, and directly converting the metal ion doped polysulfone polymer film on the surface of indium tin oxide conductive glass into metal sulfide/three-dimensional porous graphene in situ.
3. The method for preparing the laser-induced metal sulfide/three-dimensional porous graphene composite photoelectrode according to claim 1, wherein the method comprises the following steps: the laser power is 4.0-4.8W, the laser engraving speed is 166-250 mm/s, the laser engraving resolution is 600-1200, and the laser defocusing distance is 0.2-0.4 cm.
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| CN112779561A (en) * | 2019-11-10 | 2021-05-11 | 青岛农业大学 | Preparation of laser-induced electrocatalyst-semiconductor-three-dimensional porous graphene ternary composite photoelectrode |
| CN111923438B (en) * | 2020-06-16 | 2021-09-14 | 北京航空航天大学 | Preparation method of self-converted multifunctional graphene composite material |
| CN113809199A (en) * | 2020-06-17 | 2021-12-17 | 青岛农业大学 | Laser-induced preparation of nano bismuth surface plasma enhanced composite photoelectrode |
| CN113758975A (en) * | 2021-09-10 | 2021-12-07 | 华东师范大学 | Laser-induced graphene/metal oxide sensitive material and preparation method thereof |
| CN115161624B (en) * | 2022-07-19 | 2023-04-28 | 广东工业大学 | Coating method based on laser-induced zirconium-doped graphene |
| CN115420393B (en) * | 2022-09-06 | 2024-03-15 | 河北工业大学 | Preparation method of gas-temperature sensor |
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