CN113943945B - Preparation method of size-stable anode with high oxygen evolution catalytic porous coating - Google Patents
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Abstract
A preparation method of a dimension stable anode with a high oxygen evolution catalytic porous coating comprises the following steps: (1) Raw materials LiOH and H 2 IrCl 6 ·xH 2 Placing the O in an organic solvent, and carrying out ultrasonic treatment; (2) dripping a covering substrate, and drying; (3) Placing the mixture in a preheated muffle furnace for heat treatment and air cooling; (4) repeating the steps (2) and (3) for a plurality of times; (5) Dripping precursor solution to cover the substrate with the multilayer coating, drying, placing in a preheated muffle furnace for stabilization heat treatment, and air cooling; and (6) drying after washing. The method is simple and convenient to operate, easy to implement and capable of accurately controlling the proportion regulation and control components, the grain size and the porosity; the coating has a special micro-porous structure and high-efficiency oxygen evolution catalytic performance, and can be stably used under an acidic condition.
Description
Technical Field
The invention belongs to the technical field of electrochemical industrial electrode materials, and particularly relates to a preparation method of a dimensionally stable anode with a high oxygen evolution catalytic porous coating.
Background
In the hydrometallurgical production of metals such as copper, zinc and the like, the electrical energy consumption of the electrolytic deposition step is large, mainly because the oxygen evolution overpotential of the anode is high during the electrolytic deposition. At present, lead-based anodes are commonly used in the copper-zinc electrolytic deposition process, and have the defects of high oxygen evolution overpotential, easy pollution of cathode products, easy creep deformation in the electrolytic deposition process and the like. The Dimensionally Stable Anode (DSA) proposed in 1963 has the advantages of stable size, low oxygen evolution overpotential, no product pollution and the like. The oxygen evolution overpotential of DSA is mainly determined by the catalytic activity of the oxide catalytic coating coated on the surface of DSA, and the electrolytic deposition of metals such as copper, zinc and the like is generally carried out on DSASince the reaction is carried out in an acidic solution, a part of transition group metals and oxides thereof have good oxygen evolution electrocatalytic activity, but have poor stability under acidic high potential conditions. The active coating commonly used at present for DSA adopts IrO 2 +Ta 2 O 5 Although the electrode has higher oxygen evolution activity compared with the traditional lead electrode or graphite electrode, the performance of the electrode still has great promotion potential, and further promotion of the catalytic activity of the electrode has important significance for popularization and application of DSA.
The current methods for improving the electrical catalytic activity of DSA are divided into two types: one is to improve the electrocatalytic activity of the catalyst, such as preparing amorphous material with higher activity; and another method is to increase the active area and obtain more active sites, such as preparing a surface porous structure by a plurality of new processes. However, the amorphous material with high activity is generally in the problem of poor stability, and other novel processes for preparing the porous structure have high cost and complicated steps, so that technical innovation needs to be realized on the conventional method to obtain a novel DSA with high activity and large surface area.
The invention content is as follows:
the invention aims to provide a preparation method of a dimension stable anode of a high oxygen evolution porous catalytic porous coating, which adopts nanocrystalline IrO with a porous structure 2 The material is used as a DSA porous coating, improves the oxygen evolution capacity, and can ensure that the DSA can be stably used under the acidic condition.
The method of the invention comprises the following steps:
(1) Raw materials LiOH and H 2 IrCl 6 ·xH 2 Placing O in an organic solvent, and then carrying out ultrasonic treatment to dissolve the raw materials to obtain a precursor solution;
(2) Dropwise adding the precursor solution onto a substrate to enable the precursor solution to cover the substrate, then putting the substrate into a preheated oven, and drying to remove the organic solvent to obtain the substrate with the pretreated coating;
(3) Placing the substrate with the pretreatment coating in a preheated muffle furnace for heat treatment, taking out the substrate, and air-cooling the substrate to normal temperature to obtain a substrate with a single-layer coating;
(4) Repeating the steps (2) and (3) for a plurality of times on the substrate with the single-layer coating to obtain a substrate with a multi-layer coating;
(5) Dropwise adding the precursor solution onto a substrate with a multilayer coating to enable the precursor solution to cover the substrate with the multilayer coating, then putting the substrate into a preheated oven, drying to remove the organic solvent, then putting the substrate into a preheated muffle furnace, carrying out stabilization heat treatment, and carrying out air cooling to normal temperature to obtain the substrate with the stabilized porous coating;
(6) And washing the substrate with the stabilized porous coating to remove surface impurities, and drying to remove water to obtain the substrate with the high oxygen evolution catalytic porous coating on the surface, namely obtaining the dimension stable anode with the high oxygen evolution catalytic coating.
In the step (1), the precursor solution contains LiOH to H according to the molar ratio 2 IrCl 6 ·xH 2 O＝(1～5):1。
In the above step (4), the steps (2) and (3) are repeated 9 to 15 times.
The component of the high oxygen evolution catalytic porous coating is IrO 2 The crystal form is nanocrystalline rutile, and the grain size is 2-5 nm.
The thickness of the high oxygen evolution catalytic porous coating is 15-25 μm.
In the step (1), the organic solvent is a mixture of ethanol and isopropanol.
In the above step (1), liOH and H 2 IrCl 6 ·xH 2 The mass ratio of the total amount of O to the organic solvent is (3-5) to 1.
In the steps (2), (5) and (6), the drying is carried out at the temperature of 120 +/-2 ℃ for 10-15 min.
In the step (2), the substrate is made of Ti.
In the steps (2) and (5), the temperature of the oven after preheating is 120 +/-2 ℃.
In the steps (3), (4) and (5), the temperature of the preheated muffle furnace is 450 +/-5 ℃, and the heat treatment is carried out for 5-15 min at the temperature of 450 +/-5 ℃; the temperature of the stabilizing heat treatment is 450 +/-5 ℃, and the time is 100-150 min.
The reaction formula of the method is as follows:
LiOH+H 2 IrCl 6 →Li 2 [Ir(OH) 4 Cl 2 ]+H 2 O (1)、
Li[Ir(OH) 4 Cl 2 ]→LiCl+Ir(OH) 4 (2)
and
Ir(OH) 4 →IrO 2 +H 2 O (3)。
the principle of the invention is as follows: after addition of LiOH, liOH reacts with H 2 IrCl 6 Reacting to generate Li first 2 [Ir(OH) 4 Cl 2 ]And then decomposed into Ir (OH) 4 Finally, irO is generated 2 (ii) a And conventional H 2 IrCl 6 First decomposed into IrCl 4 Reoxidized to IrO 2 Compared with the process, the method can form a porous structure coating with larger specific surface area, is a nanocrystalline material with rutile crystal form, and is more amorphous material rutile IrO than the amorphous material obtained by the traditional method 2 Compared with the prior art, the method has higher oxygen evolution activity and higher electron transfer efficiency.
The traditional thermal deposition method adopted by the invention is simple and convenient to operate and easy to implement, can accurately control the proportion and the dosage of reactants, and regulates and controls the components, the grain size and the porosity of the high oxygen evolution catalytic porous coating; the method has no complex or high-cost method, and can realize the great improvement of the oxygen evolution performance and the effective improvement of the electrolysis efficiency of the high oxygen evolution catalytic porous coating; the additive is low in price and easy to obtain; and conventional IrO 2 Compared with the coating, the coating has a special micro porous structure and high-efficiency oxygen evolution catalytic performance, can be stably used under an acidic condition, effectively reduces the energy consumption in the electrodeposition process, saves energy, and has industrial application value.
Description of the drawings:
FIG. 1 is a low magnification SEM image of a high oxygen evolution catalytic porous coating of example 1 of the present invention;
FIG. 2 is a high magnification SEM image of a high oxygen evolution catalytic porous coating of example 1 of the present invention;
FIG. 3 is a TEM image of the high oxygen evolution catalytic porous coating of example 1 of the present invention;
FIG. 4 is a diffraction diagram of the high oxygen evolution catalytic porous coating of example 1 of the present invention;
FIG. 5 shows the high oxygen evolution catalytic porous coating of example 1 of the present invention and conventional IrO 2 XRD pattern of the coating; in the figure,: "conventional IrO 2 Coating, namely diamond solid is a high oxygen evolution catalytic porous coating;
FIG. 6 is a graph of the high oxygen evolution catalytic porous coating and a conventional IrO of example 1 of the present invention 2 Polarization profile of the coating; in the figure, the solid curve is the conventional IrO 2 The dotted curve is a high oxygen evolution catalytic porous coating;
FIG. 7 shows a high oxygen evolution catalytic porous coating of example 1 of the present invention and a conventional IrO 2 Coating Tafel slope plot; in the figure, □ is a conventional IrO 2 Coating,. Smallcircle.is a high oxygen evolution catalytic porous coating.
The specific implementation mode is as follows:
the load capacity of Ir element on the surface of the substrate in the embodiment of the invention is 1-2 mg/cm 2 。
LiOH and H used in the examples of the present invention 2 IrCl 6 ·xH 2 O is a commercially available analytical pure reagent.
The ethanol and isopropanol used in the examples of the present invention are commercially available analytical reagents.
The volume ratio of ethanol to isopropanol in the organic solvent in the examples of the present invention was 1:1.
In the embodiment of the invention, the mass content of Ti in the substrate is more than 99%.
The SEM observation equipment FEI Quanta250FEG scanning electron microscope in the embodiment of the invention.
The observation device of the TEM in the embodiment of the invention is a JEOL JEM-ARM200F spherical aberration transmission electron microscope.
In the embodiment of the invention, the diffraction ring is in a form after Fourier transformation of a transmission electron microscope picture.
In the embodiment of the invention, the XRD observation equipment is a SmartLabX-ray diffractometer.
In the embodiment of the invention, a VersasTAT 4 electrochemical workstation is adopted for polarization curve test and Tafel slope test; the method carries out a polarization curve test according to an OER performance evaluation method (Zhao Dandan and the like, the latest development of a non-noble metal electro-catalysis oxygen evolution catalyst, electrochemistry, 2018,24 (05): 455-465.).
The frequency of the ultrasonic treatment in the embodiment of the present invention was 20kHz.
In the embodiment of the invention, the temperature of the oven after preheating is 120 +/-2 ℃.
In the embodiment of the invention, the drying is carried out at the temperature of 120 +/-2 ℃ for 10-15 min.
Example 1
Raw materials LiOH and H 2 IrCl 6 ·xH 2 Placing O in an organic solvent, and then carrying out ultrasonic treatment to dissolve the raw materials to obtain a precursor solution; the molar ratio of LiOH to H in the precursor solution 2 IrCl 6 ·xH 2 O =4:1; liOH and H 2 IrCl 6 ·xH 2 The mass ratio of the total amount of O to the organic solvent is 3:1;
dropwise adding the precursor solution onto a substrate to enable the precursor solution to cover the substrate, then putting the substrate into a preheated oven, and drying to remove the organic solvent to obtain the substrate with the pretreated coating; the substrate is made of Ti;
placing the substrate with the pretreatment coating in a preheated muffle furnace for heat treatment, taking out the substrate and air-cooling the substrate to normal temperature to obtain a substrate with a single-layer coating; the heat treatment is carried out at 450 +/-5 ℃ for 5min;
repeating the precursor solution covering step and the heat treatment step in a muffle furnace on the substrate with the single-layer coating for 14 times to obtain the substrate with the multi-layer coating;
dropwise adding the precursor solution onto a substrate with a multilayer coating to enable the precursor solution to cover the substrate with the multilayer coating, then putting the substrate into a preheated oven, drying to remove the organic solvent, then putting the substrate into a preheated muffle furnace, carrying out stabilization heat treatment, and air-cooling to normal temperature to obtain the substrate with the stabilized porous coating; the temperature of the stabilizing heat treatment is 450 +/-5 ℃, and the time is 120min;
washing the substrate with the stabilized porous coating with water to remove surface impurities, and drying to remove water to obtain a substrate with a high oxygen evolution catalytic porous coating on the surface, namely obtaining a dimension stable anode of the high oxygen evolution catalytic porous coating;
wherein the temperature of the preheated muffle furnace is 450 +/-5 ℃;
the component of the high oxygen evolution catalytic porous coating is IrO 2 The crystal form is nanocrystalline rutile, and the grain size is 2-5 nm; the thickness of the high oxygen evolution catalytic porous coating is 20 μm;
the low-magnification SEM image of the high oxygen evolution catalytic porous coating is shown in figure 1, the high-magnification SEM image is shown in figure 2, the TEM image is shown in figure 3, the diffraction ring image is shown in figure 4, the XRD image is shown in the lower curve of figure 5, the polarization curve diagram is shown in the dotted line of figure 6, and the Tafel slope is shown in the lower curve of figure 7; the current density is 10mA/cm 2 And 100mA/cm 2 When the voltage is equal to 1.432V vsRhHE and 1.473V vs RHE; as seen from SEM and TEM images, the high oxygen evolution catalytic porous coating is of a porous structure, and the size of the crystal structure is 1-10 nm; as can be seen from the graph, the coating has high oxygen evolution capacity and can be stably used under acidic conditions;
adopting conventional method, adding no LiOH, and the rest is the same as above method to obtain IrO with surface 2 An anode of the coating; the XRD pattern is shown as the upper curve of FIG. 5, the polarization curve is shown as the solid line of FIG. 6, and the Tafel slope is shown as the upper curve of FIG. 7; the current density is 10mA/cm 2 And 100mA/cm 2 The potentials were 1.474V vs RHE and 1.535V vs RHE, respectively.
Example 2
The method is the same as example 1, except that:
(1) The molar ratio of LiOH to H in the precursor solution 2 IrCl 6 ·xH 2 O =2:1; liOH and H 2 IrCl 6 ·xH 2 The mass ratio of the total amount of O to the organic solvent is 3.5;
(2) Preserving heat for 8min during heat treatment;
(3) The current density is 10mA/cm 2 And 100mA/cm 2 The potentials were 1.446V vs RHE and 1.490V vsRhHE, respectively.
Example 3
The method is the same as example 1, except that:
(1) Precursor bodyIn solution according to the molar ratio of LiOH to H 2 IrCl 6 ·xH 2 O =3:1; liOH and H 2 IrCl 6 ·xH 2 The mass ratio of the total amount of O to the organic solvent is 4:1;
(2) Preserving heat for 10min during heat treatment;
(3) The current density is 10mA/cm 2 And 100mA/cm 2 The potential was 1.437V vs RHE and 1.479V vsRhHE, respectively.
Example 4
The method is the same as example 1, except that:
(1) The molar ratio of LiOH to H in the precursor solution 2 IrCl 6 ·xH 2 O =1:1; liOH and H 2 IrCl 6 ·xH 2 The mass ratio of the total amount of O to the organic solvent is 4.5;
(2) Preserving heat for 12min during heat treatment;
(3) The current density is 10mA/cm 2 And 100mA/cm 2 The potentials are 1.436V vs RHE and 1.473V vsHE, respectively.
Example 5
The method is the same as example 1, except that:
(1) The molar ratio of LiOH to H in the precursor solution 2 IrCl 6 ·xH 2 O =5:1; liOH and H 2 IrCl 6 ·xH 2 The mass ratio of the total amount of O to the organic solvent is 5:1;
(2) Preserving heat for 15min during heat treatment;
(3) The current density is 10mA/cm 2 And 100mA/cm 2 The potentials were 1.446V vs RHE and 1.491V vsRHE, respectively.
Claims (7)
1. A preparation method of a dimension stable anode with a high oxygen evolution catalytic porous coating is characterized by comprising the following steps:
(1) According to the molar ratio of LiOH to H 2 IrCl 6 ·xH 2 O = (1-5): 1, raw materials LiOH and H 2 IrCl 6 ·xH 2 Placing O in an organic solvent, and then carrying out ultrasonic treatment to dissolve the raw materials to obtain a precursor solution;
(2) Dropwise adding the precursor solution onto a substrate to enable the precursor solution to cover the substrate, then putting the substrate into a preheated oven, and drying to remove the organic solvent to obtain the substrate with the pretreatment coating;
(3) Placing the substrate with the pretreatment coating in a preheated muffle furnace for heat treatment, taking out the substrate and air-cooling the substrate to normal temperature to obtain a substrate with a single-layer coating;
(4) Repeating the steps (2) and (3) for a plurality of times on the substrate with the single-layer coating to obtain a substrate with a multi-layer coating;
(5) Dropwise adding the precursor solution onto a substrate with a multilayer coating to enable the precursor solution to cover the substrate with the multilayer coating, then putting the substrate into a preheated oven, drying to remove the organic solvent, then putting the substrate into a preheated muffle furnace, carrying out stabilization heat treatment, and air-cooling to normal temperature to obtain the substrate with the stabilized coating;
(6) Washing the substrate with the stabilizing coating with water to remove surface impurities, and drying to remove water to obtain a substrate with a high oxygen evolution catalytic coating on the surface, namely obtaining a size-stable anode of the high oxygen evolution catalytic coating; the component of the high oxygen evolution catalytic coating is IrO 2 The crystal form is nanocrystalline rutile, and the grain size is 2-5 nm;
in the steps (3), (4) and (5), the temperature of the preheated muffle furnace is 450 +/-5 ℃, and the heat treatment is carried out for 5 to 15min at the temperature of 450 +/-5 ℃; the temperature of the stabilizing heat treatment is 450 +/-5 ℃, and the time is 100 to 150min.
2. The method for preparing a dimensionally stable anode with a high oxygen evolution catalytic porous coating according to claim 1, characterized in that in step (4), steps (2) and (3) are repeated 9 to 15 times.
3. The method of claim 1 wherein the high oxygen evolution catalytic coating has a thickness of 15 to 25 μm.
4. The method of claim 1, wherein in step (1), the organic solvent is a mixture of ethanol and isopropanol.
5. The method of claim 1 wherein in step (1), liOH and H are added to the anode in a dimensionally stable form 2 IrCl 6 ·xH 2 The mass ratio of the total amount of O to the organic solvent is (3-5): 1.
6. The method of claim 1, wherein in step (2), the substrate is made of Ti.
7. The method of claim 1, wherein the heat treatment and the stabilizing heat treatment are performed according to the following reaction formula:
LiOH + H 2 IrCl 6 →Li 2 [Ir(OH) 4 Cl 2 ] + H 2 O （1）、
Li[Ir(OH) 4 Cl 2 ] →LiCl +Ir(OH) 4 （2）
and
Ir(OH) 4 → IrO 2 + H 2 O（3）。
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