CN112144089A - Nickel-titanium alloy hydrophobic lead dioxide electrode and preparation method thereof - Google Patents
Nickel-titanium alloy hydrophobic lead dioxide electrode and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of electrocatalysis electrode preparation, and particularly discloses a nickel-titanium alloy hydrophobic lead dioxide electrode which is composed of a lead dioxide surface hydrophobic coating and a nickel-titanium alloy substrate with a nanotube structure. Also discloses a preparation method of the electrode. The invention changes the conductivity of the titanium dioxide nanotube and the hydrophilicity of the catalyst layer, thereby reducing the impedance of the electrode, improving the utilization rate of OH, simultaneously enhancing the electrocatalytic capacity of the electrode, and being beneficial to energy consumption control and efficiency guarantee in large-scale production.
Description
Technical Field
The invention relates to the field of electrocatalysis electrode preparation, in particular to a nickel-titanium alloy hydrophobic lead dioxide electrode and a preparation method thereof.
Background
Due to the rapid development of human society, a series of new refractory pollutants cause a plurality of problems, great challenges are brought to human health and ecological systems, and various advanced oxidation methods based on OH can effectively treat the refractory pollutants, wherein the electrochemical oxidation method has stronger oxidation capacity than the common chemical oxidation method, and other chemical agents are not added, so the electrochemical oxidation method has unique superiority. The electrocatalytic oxidation mainly realizes the oxidation capacity through an anode, so the development of a novel high-efficiency electrocatalytic electrode becomes a research hotspot.
In comparison, PbO2High electrode oxygen evolution potential and PbO2The cost is low, and the method is very suitable for decomposing organic pollutants by anodic oxidation. But it also has PbO2The coating has larger interface resistance, is easy to peel off from the substrate and has shorter service life due to PbO2The electrode is hydrophilic although PbO2The amount of. OH formed on the electrode is larger than that of the BDD electrode, but the oxidation efficiency is low, so improvement is needed. At present, the most studied is the microstructure design of the substrate because the microstructure design can effectively improve the comprehensive performance of the catalytic electrode, but the microstructure design is limited by the characteristics of the material and the existing electrode preparation process, and the research objects of the alternative electrode material and the microstructure design are only limited by TiO2-NTs. Although the performance of the electrode such as oxygen evolution potential and service life enhancement can be effectively improved, the electrode has the serious defect of poor conductivity. At present, research on electrode research and development mostly focuses on improvement of the catalyst layer and the intermediate layer, and research on the substrate and hydrophilicity is less, so the invention firstly provides the nickel-titanium alloy hydrophobic lead dioxide electrode and the preparation method thereof, and the conductivity of the substrate and the hydrophobicity of the catalyst layer on the surface of the electrode are improved.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a nickel-titanium alloy hydrophobic lead dioxide electrode and a preparation method thereof.
The technical purpose of the invention is realized by the following technical scheme: a nickel-titanium alloy hydrophobic lead dioxide electrode is composed of a lead dioxide surface hydrophobic plating layer and a nickel-titanium alloy substrate with a nanotube structure, wherein after the nickel-titanium alloy substrate is subjected to anodic oxidation, a nickel-doped titanium dioxide nanotube array is formed on the surface of the nickel-titanium alloy substrate, then high-temperature annealing is carried out, and then the lead dioxide surface hydrophobic plating layer is formed on a substrate through a direct-current electrodeposition method, wherein the lead dioxide surface hydrophobic plating layer is a lead dioxide hydrophobic catalytic layer.
The surface of the nickel-doped titanium dioxide nanotube array is composed of nanotubes with the average diameter of 100-120nm, and the length range of the nanotubes is 6 +/-1 mu m. . The oxide plating layer is lead oxide.
When the preparation is carried out, the following steps are carried out:
step 1, pretreatment of an alloy matrix: firstly, cutting by a wire to obtain a needed nickel-titanium alloy substrate, and polishing by abrasive paper to remove oxides on the surface; then, alkali liquor is used for removing oil from the alloy matrix at high temperature; then acid etching is carried out on the alloy matrix by acid liquor at the micro-boiling temperature; finally, ultrasonically cleaning the matrix by using deionized water, and sealing and storing the matrix in a 95% ethanol solution for later use.
In step 1, the mass ratio of the nickel-titanium alloy substrate is Ni: ti 1:99 with Ni: ti is 2: 98.
In the step 1, the alkali liquor is 5-10 wt% NaOH solution when alkali washing is carried out to remove oil, the alkali washing temperature is 90-94 ℃, the alkali washing time is 2-3h, the acid liquor is 10-15 wt% oxalic acid solution when acid etching is carried out, the acid etching temperature is 97-100 DEG C
Step 2, preparing the nanotube array: adopting anodic oxidation method, using pretreatment electrode as working electrode, using stainless steel electrode as counter electrode, using ethylene glycol and H2O、NH4The mixed solution F is electrolyte, is subjected to anodic oxidation under constant voltage, and is stirred continuously to be uniform. And oxidizing to obtain an initial amorphous nanotube, and finally annealing at high temperature to obtain a stable nanotube array.
In step 2, the electrolyte is 96-98 vol% of ethylene glycol and 2-4 vol% of H2O，0.5-1wt％NH4And F, mixed solution.
In step 2, the voltage is 40-50V, the anodic oxidation time is 2.5-3h, the annealing temperature is 450-550 ℃, and the annealing time is 2-3 h.
Step 3, loading the lead dioxide surface hydrophobic coating by a direct current deposition method: taking a pretreatment electrode as an anode, a stainless steel electrode as a cathode, taking a mixed solution of lead nitrate, sodium fluoride, dilute nitric acid and polytetrafluoroethylene resin as a precursor solution, performing electrodeposition at 80 ℃, cleaning and drying to obtain a final electrode;
in step 3, the precursor solution is 0.4-0.6mol/L Pb (NO)3)2、0.05-0.15mol/L HNO30.04-0.06mol/L NaF and 4-5mL/L PTFE resin;
in the step 3, the current density is 40-60mA/cm during electrodeposition2The electrodeposition time is 50-70 min.
Compared with the prior art, the method has the advantages that the nickel-doped titanium dioxide nanotube array is generated on the nickel-titanium alloy substrate through an anodic oxidation method, and the hydrophobic coating on the surface of the lead dioxide is loaded through a direct-current deposition method, so that the hydrophobic lead dioxide electrode is prepared, the conductivity of the titanium dioxide nanotube and the hydrophilicity of the catalyst layer are changed, the impedance of the electrode is reduced, the utilization rate of OH is improved, the electrocatalytic capacity of the electrode is enhanced, and the method is favorable for energy consumption control and efficiency guarantee in large-scale production.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
Example 1
The preparation method of the nickel-titanium alloy hydrophobic lead dioxide electrode comprises the following steps:
(1) pretreatment of an alloy matrix: firstly, obtaining a nickel-titanium alloy substrate with the mass ratio of nickel to titanium of 20 multiplied by 20mm being 1:99 by linear cutting, sequentially polishing the nickel-titanium alloy substrate by 150-mesh, 600-mesh and 1000-mesh abrasive paper until the surface is smooth, and removing oxides on the surface; then, degreasing the alloy matrix for 2 hours by using 5 wt% NaOH solution in a water bath at 90 ℃; then, performing acid etching on the alloy matrix for 3 hours by using 10 wt% of oxalic acid solution in a water bath at the temperature of 98 ℃; finally, ultrasonically cleaning the substrate by using deionized water, and sealing and storing the substrate in a 95% ethanol solution for later use;
(2) preparing a nanotube array: adopting an anodic oxidation method, taking a pretreatment electrode as a working electrode, taking a stainless steel electrode as a counter electrode, and taking 98 vol% of ethylene glycol and 2 vol% of H2O、0.5wt％NH4The mixed solution of F is electrolyte, is subjected to anodic oxidation for 3 hours under the constant voltage of 45V, and is continuously stirredThe solution was homogenized. And (3) oxidizing to obtain an initial amorphous nanotube, and finally annealing at 450 ℃ for 3h to obtain the stable nickel-doped titanium dioxide nanotube array.
(3) Loading a lead dioxide surface hydrophobic coating by a direct current deposition method: by adopting a direct current deposition method, a pretreatment electrode is taken as a cathode, a stainless steel electrode is taken as an anode, and 0.5mol/L Pb (NO) is used3)2、0.10mol/L HNO30.05mol/L NaF and 4.5mL/L PTFE resin solution as precursor solution at 50mA/cm2Performing electrodeposition at 80 ℃ for 60min under current density, cleaning and drying to obtain the final electrode.
Example 2
The preparation method of the nickel-titanium alloy hydrophobic lead dioxide electrode comprises the following steps:
(1) pretreatment of an alloy matrix: firstly, obtaining a nickel-titanium alloy substrate with the mass ratio of nickel to titanium of 20 multiplied by 20mm being 1:98.5 by linear cutting, sequentially polishing the nickel-titanium alloy substrate by using 150-mesh, 600-mesh and 1000-mesh sandpaper until the surface is smooth, and removing oxides on the surface; then, degreasing the alloy matrix for 2 hours by using 5 wt% NaOH solution in a water bath at 90 ℃; then, performing acid etching on the alloy matrix for 3 hours by using 10 wt% of oxalic acid solution in a water bath at the temperature of 98 ℃; finally, ultrasonically cleaning the substrate by using deionized water, and sealing and storing the substrate in a 95% ethanol solution for later use;
(2) preparing a nanotube array: by adopting an anodic oxidation method, a pretreatment electrode is used as a working electrode, a stainless steel electrode is used as a counter electrode, and 96 vol% of ethylene glycol, 4 vol% of H2O and 1.5% of wtNH are used4And the mixed solution F is electrolyte, is subjected to anodic oxidation for 2.5 hours under the constant voltage of 40V, and is stirred continuously to be uniform. And (3) oxidizing to obtain an initial amorphous nanotube, and finally annealing at the high temperature of 400 ℃ for 2.5h to obtain the stable nickel-doped titanium dioxide nanotube array.
(3) Loading a lead dioxide surface hydrophobic coating by a direct current deposition method: by adopting a direct current deposition method, a pretreatment electrode is taken as a cathode, a stainless steel electrode is taken as an anode, and 0.6mol/L Pb (NO) is taken3)2、0.15mol/L HNO30.06mol/L NaF and 5mL/L PTFE resin solution as precursor solution at 60mA/cm2Electrodepositing at 80 deg.C for 70min under current density, cleaning, and oven drying to obtain final electrode。
Comparative example 1
(1) Pretreatment of the titanium substrate: firstly, cutting by a wire to obtain a titanium substrate with the size of 20 multiplied by 20mm, sequentially polishing by 150-mesh, 600-mesh and 1000-mesh sand paper until the surface is smooth, and removing oxides on the surface; then, degreasing the alloy matrix for 2 hours by using 5 wt% NaOH solution in a water bath at 90 ℃; then, performing acid etching on the alloy matrix for 3 hours by using 10 wt% of oxalic acid solution in a water bath at the temperature of 98 ℃; finally, ultrasonically cleaning the substrate by using deionized water, and sealing and storing the substrate in a 95% ethanol solution for later use;
(2) preparing a nanotube array: adopting an anodic oxidation method, taking a pretreatment electrode as a working electrode, taking a stainless steel electrode as a counter electrode, and taking 98 vol% of ethylene glycol and 2 vol% of H2O、0.5wt％NH4And the mixed solution F is electrolyte, is subjected to anodic oxidation for 3 hours under the constant voltage of 45V, and is stirred continuously to be uniform. And (3) oxidizing to obtain an initial amorphous nanotube, and finally annealing at 450 ℃ for 3h to obtain the stable nickel-doped titanium dioxide nanotube array.
(3) Loading a lead dioxide surface coating by a direct current deposition method: by adopting a direct current deposition method, a pretreatment electrode is taken as a cathode, a stainless steel electrode is taken as an anode, and 0.5mol/L Pb (NO) is used3)2、0.10mol/L HNO30.05mol/L NaF solution is used as precursor solution at 50mA/cm2Performing electrodeposition at 80 ℃ for 60min under current density, cleaning and drying to obtain the final electrode.
Comparative example 2
(1) Pretreatment of the titanium substrate: firstly, cutting by a wire to obtain a titanium substrate with the size of 20 multiplied by 20mm, sequentially polishing by 150-mesh, 600-mesh and 1000-mesh sandpaper until the surface is smooth, and removing oxides on the surface; then, degreasing the alloy matrix for 2 hours by using 5 wt% NaOH solution in a water bath at 90 ℃; then, performing acid etching on the alloy matrix for 3 hours by using 10 wt% of oxalic acid solution in a water bath at the temperature of 98 ℃; finally, ultrasonically cleaning the substrate by using deionized water, and sealing and storing the substrate in a 95% ethanol solution for later use;
(2) preparing a nanotube array: by adopting an anodic oxidation method, a pretreatment electrode is used as a working electrode, a stainless steel electrode is used as a counter electrode, and 96 vol% of ethylene glycol and 4 vol% of H are used2O、1.5％wtNH4And the mixed solution F is electrolyte, is subjected to anodic oxidation for 2.5 hours under the constant voltage of 40V, and is stirred continuously to be uniform. And (3) oxidizing to obtain an initial amorphous nanotube, and finally annealing at the high temperature of 400 ℃ for 2.5h to obtain the stable nickel-doped titanium dioxide nanotube array.
(3) Loading a lead dioxide surface coating by a direct current deposition method: by adopting a direct current deposition method, a pretreatment electrode is taken as a cathode, a stainless steel electrode is taken as an anode, and 0.6mol/L Pb (NO) is taken3)2、0.15mol/L HNO30.06mol/L NaF solution is used as precursor solution at 60mA/cm2Electrodepositing at 80 deg.C for 70min under current density, cleaning, and oven drying to obtain final electrode.
Claims (10)
1. The nickel-titanium alloy hydrophobic lead dioxide electrode is characterized by comprising a lead dioxide surface hydrophobic plating layer and a nickel-titanium alloy substrate with a nanotube structure, wherein the nickel-titanium alloy substrate is subjected to anodic oxidation, a nickel-doped titanium dioxide nanotube array is formed on the surface of the nickel-titanium alloy substrate, then the nickel-doped titanium dioxide nanotube array is subjected to high-temperature annealing, and then the lead dioxide surface hydrophobic plating layer is formed on a substrate through a direct-current deposition method, wherein the lead dioxide surface hydrophobic plating layer is a lead dioxide hydrophobic catalysis layer.
2. The hydrophobic lead dioxide electrode of NiTi alloy as claimed in claim 1, wherein the surface of the Ni-doped Titania nanotube array is composed of nanotubes with an average diameter of 100-120nm, the length of the nanotubes is within a range of 6 ± 1 μm, and the oxide coating is an oxide of lead.
3. The method for preparing the hydrophobic lead dioxide electrode made of nickel-titanium alloy according to claim 1 or 2, which is characterized by comprising the following steps:
1) pretreatment of an alloy matrix: firstly, cutting by a wire to obtain a needed nickel-titanium alloy substrate, and polishing by abrasive paper to remove oxides on the surface;
2) then, alkali liquor is used for removing oil from the alloy matrix at high temperature; then acid etching is carried out on the alloy matrix by acid liquor at the micro-boiling temperature;
3) finally, ultrasonically cleaning the matrix by using deionized water, and sealing and storing the matrix in a 95% ethanol solution for later use.
4. The method for preparing the hydrophobic lead dioxide electrode made of nickel-titanium alloy according to claim 3, wherein in the step 1), the ratio of the alloy Ni: the mass ratio of Ti is 2:98 to 1: 99.
5. the method for preparing the hydrophobic lead dioxide nickel-titanium alloy electrode according to claim 3, wherein in the step 1), alkali solution is 5-10 wt% NaOH solution when oil is washed with alkali, the alkali washing temperature is 90-94 ℃, the alkali washing time is 2-3h, acid solution is 10-15 wt% oxalic acid solution when acid etching is carried out, and the acid etching temperature is 97-100 ℃.
6. The method for preparing the hydrophobic lead dioxide electrode made of nickel-titanium alloy according to claim 3, wherein the step 2) is to prepare the nanotube array: adopting anodic oxidation method, using pretreatment electrode as working electrode, using stainless steel electrode as counter electrode, using ethylene glycol and H2O、NH4And the mixed solution F is an electrolyte, is subjected to anodic oxidation under constant voltage, is continuously stirred to be uniform, is oxidized to obtain an initial amorphous nanotube, and is finally annealed at high temperature to obtain a stable nanotube array.
7. The method for preparing hydrophobic lead dioxide electrode of nickel-titanium alloy according to claim 3, wherein the electrolyte of step 2) is 96-98 vol% ethylene glycol and 2-4 vol% H2O，0.5-1wt％NH4And F, mixed solution.
8. The method for preparing hydrophobic lead dioxide electrode of nickel titanium alloy according to claim 3, wherein the voltage of step 2) is 40-50V, the anodic oxidation time is 2.5-3h, the annealing temperature is 450-550 ℃, and the annealing time is 2-3 h.
9. The preparation method of the hydrophobic lead dioxide electrode made of nickel-titanium alloy according to claim 3, wherein the step 3) of loading the hydrophobic plating layer on the surface of the lead dioxide by a direct current deposition method comprises the following steps: and (3) performing electrodeposition at the temperature of 80 ℃, cleaning and drying to obtain the final electrode by taking the pretreatment electrode as an anode, the stainless steel electrode as a cathode and a mixed solution of lead nitrate, sodium fluoride, dilute nitric acid and polytetrafluoroethylene resin as a precursor solution.
10. The method for preparing hydrophobic lead dioxide electrode of nickel titanium alloy according to claim 3, wherein the precursor solution of step 3) is 0.4-0.6mol/L Pb (NO)3)2、0.05-0.15mol/L HNO30.04-0.06mol/L NaF and 4-5mL/L PTFE resin;
during electrodeposition, the current density is 40-60mA/cm2The electrodeposition time is 50-70 min.
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| CN114927705A (en) * | 2022-05-16 | 2022-08-19 | 内蒙古鄂尔多斯电力冶金集团股份有限公司 | Preparation method of self-supporting bubble-free suspension electrode for oxygen precipitation reaction |
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| CN114927705A (en) * | 2022-05-16 | 2022-08-19 | 内蒙古鄂尔多斯电力冶金集团股份有限公司 | Preparation method of self-supporting bubble-free suspension electrode for oxygen precipitation reaction |
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