Preparation method and application of vacancy coupling nano-tip material for electrochemically extracting uranium from seawater

Abstract

The invention discloses a preparation method of a vacancy coupled nano tip material for electrochemical seawater uranium extraction, which comprises the following steps: slicing foamed nickel, performing ultrasonic treatment in acetone, ethanol, pure water and a hydrochloric acid solution in sequence, thoroughly washing with pure water, and drying for later use; the preparation method comprises the following steps: dissolving a cobalt source, urea and ammonium fluoride in pure water, transferring the solution into a polytetrafluoroethylene lining, then adding treated foamed nickel, reacting in a high-pressure reactor, taking out a material, washing with pure water, and drying; and then calcining the dried flaky material, and treating with Ar plasma after calcining to obtain the vacancy-coupled nano tip material. The Co3O4 nano tip array rich in oxygen vacancies grows on the surface of the foamed nickel, an enhanced electric field on the nano tip induces OH <-> in a solution outside an electrode surface interface to be enriched, a local alkaline pH protection layer is formed, and attachment and deposition of metal salt on the surface of the electrode are reduced.

Description

Technical Field

[0001] The present invention belongs to the fields of uranium extraction from seawater and environmental protection. More specifically, the present invention relates to a preparation method and application of a vacancy-coupled nano-tip material for electrochemically extracting uranium from seawater. Background Art

[0002] Nuclear energy is considered an important energy form for changing the future energy structure due to its advantages of being green, clean, and having a high energy density. In recent years, with the strategic requirements of nuclear energy development, the exploitation and supply of uranium resources have become increasingly important. Since the total amount of uranium in seawater is abundant, uranium extraction from seawater is considered a very promising unconventional uranium resource exploitation method to ensure future nuclear energy development. The electrochemically uranium extraction from seawater technology induces the directional migration of U(VI) to the surface of the electrode material and its reduction by electrons through an externally applied electric field. This method has fast kinetics and high reduction efficiency for uranium extraction, and at the same time avoids the need for a large amount of subsequent tail treatment of solid waste and liquid waste, and is highly anticipated. In recent years, researchers have developed a variety of electrode materials for electrochemically extracting uranium from seawater, such as covalent organic frameworks (COFs), metal-organic frameworks (MOFs), amidoxime-based materials, metal sulfides, metal oxides, etc. Especially metal oxides, metal oxides have the advantages of stable structure, good conductivity, high structural tunability, and easy preparation. In addition, special uranium adsorption sites are easily constructed on the oxide surface and have received much attention in recent years. The extremely high concentration of metal salts in seawater has a relatively serious impact on the electrochemically uranium extraction process. The fouling of a large amount of metal salts on the electrode surface not only hinders the active sites but also affects the separation and purification of subsequent uranium products. This is a point that has not been considered in the current electrochemically uranium extraction technology. Summary of the Invention

[0003] An object of the present invention is to solve at least the above problems and / or defects and provide at least the advantages described hereinafter.

[0004] To achieve these objects and other advantages of the present invention, a preparation method of a vacancy-coupled nano-tip material for electrochemically extracting uranium from seawater is provided, including the following steps:

[0005] Step 1: Cut nickel foam (NF) into slices of different sizes, then ultrasonically treat it in acetone, ethanol, pure water, and hydrochloric acid solution in sequence, thoroughly rinse it with pure water, and then dry it in a vacuum drying oven for later use;

[0006] Step 2: Dissolve a cobalt source, urea, and ammonium fluoride in pure water, stir, transfer the solution to a polytetrafluoroethylene inner liner, then add the treated nickel foam, react in a high-pressure reactor for a period of time, after the reaction is completed, take out the material, rinse it with pure water, and then dry it in a vacuum drying oven;

[0007] Step 3: Calcinate the dried flaky material in a muffle furnace, and then put it into an Ar plasma cleaner for treatment with Ar plasma to obtain a vacancy-coupled nano-tip material.

[0008] Preferably, in Step 1, the size of the nickel foam is 2×2 cm or 2×3 cm, the concentration of the hydrochloric acid solution is 0.6 mol / L, and the ultrasonic treatment is carried out for 15 - 20 min.

[0009] Preferably, in Step 2, the dosage ratio of the cobalt source, urea, ammonium fluoride and water is 0.1 - 0.6 g: 0.1 - 0.6: 0 - 0.4 g: 10 - 20 mL. The cobalt source is cobalt nitrate or cobalt acetate, and the dosage ratio of the nickel foam to water is 1 - 2 g: 10 - 20 mL.

[0010] Preferably, in Step 2, the reaction pressure is normal pressure, the reaction temperature is 100 - 150 °C, and the reaction time is 6 - 8 h.

[0011] Preferably, in Step 3, the calcination temperature is 300 - 500 °C, the calcination time is 2 - 3 h, and the Ar plasma treatment is carried out for 10 - 20 min.

[0012] Preferably, after the nickel foam is treated in Step 1, it is subjected to N and C doping modification. The method is as follows: Put the treated nickel foam into Tris buffer solution, add dopamine hydrochloride, adjust the pH to 8.0 - 9.0, stir and react for a certain time, and then take it out, wash and dry.

[0013] Preferably, the concentration of dopamine hydrochloride in the Tris buffer solution is 1 - 4 mg / mL, and the dosage ratio of the nickel foam to dopamine hydrochloride is 1: 0.25 - 0.5.

[0014] Preferably, when calcining the flaky material in Step 3, 3 - 5 Vol% of water vapor is introduced into the calcination gas.

[0015] The present invention also provides an application of the vacancy-coupled nano-tip material for electrochemically extracting uranium from seawater, using the vacancy-coupled nano-tip material as a working electrode for electrochemically extracting uranium from seawater.

[0016] The present invention has at least the following beneficial effects: By growing a nano-tip array of Co3O4 rich in oxygen vacancies on the surface of nickel foam, an electrode material for electrochemically extracting uranium from seawater with an anti-scaling effect is constructed (V O -NCCONF / NDCONF). The enhanced electric field on the nano-tips induces OH in the solution outside the electrode surface interface -Enrichment forms a "protective layer" with a local alkaline pH, reducing the attachment and deposition of metal salts on the electrode surface. At the same time, oxygen vacancies provide specific binding sites for U(VI), enabling U(VI) to undergo an adsorption-reduction-oxidation-crystallization reaction process on the electrode surface and ultimately deposit on the electrode. The synergistic effect of oxygen vacancies and tips promotes uranium separation and extraction. Therefore, V O -NCCONF exhibits a high extraction capacity of 1.93 mg g - 1 d -1 in natural seawater, which is superior to most reported electrode materials. The present invention also modifies nickel foam by N and C doping. First, polydopamine (PDA) is generated on its surface. After subsequent calcination of PDA, the remaining N and C are doped on the nickel foam, improving the O electron transfer efficiency of V O -NCCONF as the working electrode, thereby further enhancing the uranium extraction ability of the nanoscale tip material. By introducing low-concentration water vapor during calcination, H2O reacts with lattice oxygen at high temperature to generate hydroxyl groups (-OH), forming "oxygen vacancy-hydroxyl" dual active sites on the material surface: oxygen vacancies enhance the electron capture ability of uranyl ions, and hydroxyl groups improve the adsorption selectivity through hydrogen bonding.

[0017] Other advantages, objectives, and features of the present invention will be partially reflected in the following description and partially understood by those skilled in the art through the research and practice of the present invention. Description of the Drawings

[0018] Figure 1 SEM image of V O -NCCONF prepared in Example 1;

[0019] Figure 2 SEM image of V O -NDCONF prepared in Example 2;

[0020] Figure 3 HRTEM image of V O -NCCONF prepared in Example 1 and the corresponding lattice fringe spacing image and inverse fast Fourier transform (FFT) profile;

[0021] Figure 4 XPS spectrum (a) and Co 2p spectrum (b) of V O -NCCONF prepared in Example 1;

[0022] Figure 5 Electrochemical uranium extraction efficiency diagrams for Examples 1-2 and Comparative Examples 1-3;

[0023] Figure 6 Electrochemical uranium extraction efficiency diagrams for Examples 3-4 and Example 1;

[0024] Figure 7 For V in Application Example 2 O - The full XPS spectrum of the NCCONF electrode and V before and after the reaction O - Photos of the NCCONF electrode;

[0025] Figure 8 Schematic diagram of the working mechanism of the vacancy-coupled nano-tip material prepared by the present invention as a working electrode during electrochemically uranium extraction

[0026] Figure 9 For V prepared in Example 1 O - Uranium extraction amount diagrams of NCCONF and other electrochemically uranium extraction materials in the prior art Detailed implementation manners

[0027] The present invention will be further described in detail below with reference to the accompanying drawings, so that those skilled in the art can implement it according to the description in the specification.

[0028] Example 1

[0029] A preparation method of a vacancy-coupled nano-tip material for electrochemically extracting uranium from seawater, comprising the following steps:

[0030] Step 1: Cut the nickel foam into 2×3 cm sheet-shaped nickel foam, then ultrasonically treat it in acetone, ethanol, pure water and 0.6 mol / L hydrochloric acid solution in sequence for 15 min. After thoroughly rinsing with pure water, dry it in a vacuum drying oven for later use;

[0031] Step 2: Dissolve 0.55 g of cobalt nitrate and 0.6 g of urea in 15 mL of pure water. After stirring for 30 min, transfer the solution to a 50 mL polytetrafluoroethylene inner liner, then add 2 g of the treated nickel foam, and react at 120 °C in a high-pressure reactor for 6 h. After the reaction is completed, take out the material, rinse it with pure water, and then dry it in a vacuum drying oven;

[0032] Step 3: Calcinate the dried sheet material in a muffle furnace at 300 °C for 2 h. After calcination, put it into an Ar plasma cleaner and treat it with Ar plasma for 10 min to obtain a vacancy-coupled nano-tip material (V O -NCCONF).

[0033] V O The SEM image of NCCONF is as Figure 1 shown. It can be seen that the V O -NCCONF nanorod structure grows on the nickel foam; Figure 3 For V prepared in Example 2 O- The HRTEM image of NCCONF shows that the lattice fringe spacing is 0.29 nm, and this lattice fringe belongs to Co3O4; Figure 4 V prepared in Example 2 O - The XPS spectrum (a) and Co2p spectrum (b) of NCCONF show that O - The surface elements of NCCONF include Ni, Co, and O. The Co2p spectrum indicates that the valence states of Co are +3 and +2, which is in good agreement with the results in Co3O4.

[0034] Example 2

[0035] A preparation method of a vacancy-coupled nano-tip material for electrochemically extracting uranium from seawater, comprising the following steps:

[0036] Step 1: Cut the nickel foam into 2×2 cm sheet-shaped nickel foam, then ultrasonically treat it in acetone, ethanol, pure water, and 0.6 mol / L hydrochloric acid solution in sequence for 15 min. After thoroughly rinsing with pure water, dry it in a vacuum drying oven for later use;

[0037] Step 2: Dissolve 0.134 g of cobalt acetate, 0.12 g of urea, and 0.4 g of ammonium fluoride in 20 mL of pure water. After stirring for 30 min, transfer the solution to a 50 mL polytetrafluoroethylene inner liner, then add 2 g of the treated nickel foam, and react at 120 °C in a high-pressure reactor for 8 h. After the reaction is completed, take out the material, rinse it with pure water, and then dry it in a vacuum drying oven;

[0038] Step 3: Calcinate the dried sheet-shaped material in a muffle furnace at 500 °C for 3 h, and then put it into an Ar plasma cleaner for Ar plasma treatment for 10 min to obtain a vacancy-coupled nano-tip material (V O - NDCONF), and its SEM image is as Figure 2 shown. It can be seen that O - NDCONF nanorod structures grow on the nickel foam.

[0039] Example 3

[0040] A preparation method of a vacancy-coupled nano-tip material for electrochemically extracting uranium from seawater, comprising the following steps:

[0041] Step 1: Cut the nickel foam into 2×3 cm sheet-shaped nickel foam, then ultrasonically treat it in acetone, ethanol, pure water, and 0.6 mol / L hydrochloric acid solution in sequence for 15 min. After thoroughly rinsing with pure water, dry it in a vacuum drying oven for later use;

[0042] Step 2. After the nickel foam is treated in Step 1, perform surface modification on it: Put 1 g of the treated nickel foam into 100 mL of Tris buffer solution, add 400 mg of dopamine hydrochloride, and prepare a Tris-dopamine hydrochloride solution with a concentration of 4 mg / mL. Adjust the pH to 8.0 with HCl or NaOH, stir and react for 4 h, then take it out, wash and dry it;

[0043] Step 3. Dissolve 0.55 g of cobalt nitrate and 0.6 g of urea in 15 mL of pure water, stir for 30 min, then transfer the solution to a 50 mL polytetrafluoroethylene inner liner, and then add 2 g of nickel foam with polydopamine on its surface. React in a high-pressure reactor at 120 °C for 6 h. After the reaction is completed, take out the material, wash it with pure water, and then dry it in a vacuum drying oven to obtain nickel foam with polydopamine on its surface;

[0044] Step 4. Calcinate the dried flaky material in a muffle furnace at 500 °C for 3 h. After calcination, put it into an Ar plasma cleaner and treat it with Ar plasma for 10 min to obtain a nano-tip material with N, C-doped vacancy coupling (V O -NCCONF-N-C).

[0045] Example 4

[0046] A preparation method of a nano-tip material with vacancy coupling for electrochemically extracting uranium from seawater, comprising the following steps:

[0047] Step 1. Cut the nickel foam into 2×3 cm flaky nickel foam, then ultrasonically treat it in acetone, ethanol, pure water and 0.6 mol / L hydrochloric acid solution in sequence for 15 min. After thoroughly rinsing with pure water, dry it in a vacuum drying oven for standby;

[0048] Step 2. After the nickel foam is treated in Step 1, perform surface modification on it: Put 1 g of the treated nickel foam into 100 mL of Tris buffer solution, add 400 mg of dopamine hydrochloride, and prepare a Tris-dopamine hydrochloride solution with a concentration of 4 mg / mL. Adjust the pH to 8.0 with HCl or NaOH, stir and react for 4 h, then take it out, wash and dry it to obtain nickel foam with polydopamine on its surface;

[0049] Step 3. Dissolve 0.55 g of cobalt nitrate and 0.6 g of urea in 15 mL of pure water, stir for 30 min, then transfer the solution to a 50 mL polytetrafluoroethylene inner liner, and then add 2 g of nickel foam with polydopamine on its surface. React in a high-pressure reactor at 120 °C for 6 h. After the reaction is completed, take out the material, wash it with pure water, and then dry it in a vacuum drying oven;

[0050] Step 4: Calcinate the dried flaky material in a muffle furnace at 500 °C, introduce 4 Vol% water vapor into the calcination gas, calcinate for 3 h, and then put it into an Ar plasma cleaner for Ar plasma treatment for 10 min to obtain a surface-hydroxylated N, C-doped vacancy-coupled nano-tip material (V O -NCCONF-N-C-OH).

[0051] Comparative Example 1

[0052] Step 1: Cut the nickel foam into 2×3 cm flaky nickel foam, then ultrasonically treat it in acetone, ethanol, pure water, and 0.6 mol / L hydrochloric acid solution in sequence for 15 min. After thoroughly rinsing with pure water, dry it in a vacuum drying oven for later use;

[0053] Step 2: Put the treated nickel foam into an Ar plasma cleaner for Ar plasma treatment for 10 min.

[0054] Comparative Example 2

[0055] Step 1: Cut the nickel foam into 2×3 cm flaky nickel foam, then ultrasonically treat it in acetone, ethanol, pure water, and 0.6 mol / L hydrochloric acid solution in sequence for 15 min. After thoroughly rinsing with pure water, dry it in a vacuum drying oven for later use;

[0056] Step 2: Dissolve 0.55 g of cobalt nitrate and 0.6 g of urea in 15 mL of pure water. After stirring for 30 min, transfer the solution to a 50 mL polytetrafluoroethylene inner liner, then add 2 g of the treated nickel foam, and react in a high-pressure reactor at 120 °C for 6 h. After the reaction is completed, take out the material, rinse it with pure water, and then dry it in a vacuum drying oven;

[0057] Step 3: Calcinate the dried flaky material in a muffle furnace at 300 °C for 2 h to obtain NCCONF after calcination.

[0058] Comparative Example 3

[0059] Step 1: Cut the nickel foam into 2×2 cm flaky nickel foam, then ultrasonically treat it in acetone, ethanol, pure water, and 0.6 mol / L hydrochloric acid solution in sequence for 15 min. After thoroughly rinsing with pure water, dry it in a vacuum drying oven for later use;

[0060] Step 2: Dissolve 0.134 g of cobalt acetate, 0.12 g of urea, and 0.4 ammonium fluoride in 20 mL of pure water. After stirring for 30 min, transfer the solution to a 50 mL polytetrafluoroethylene inner liner, then add 2 g of the treated nickel foam, and react in a high-pressure reactor at 120 °C for 8 h. After the reaction is completed, take out the material, rinse it with pure water, and then dry it in a vacuum drying oven;

[0061] Step 3: Calcinate the dried flaky material in a muffle furnace at 500 °C for 3 h to obtain NDCONF after calcination.

[0062] Application Example 1

[0063] The materials prepared in Examples 1-4 and Comparative Example 1 were used for electrochemically uranium extraction tests. All the electrochemically uranium extraction tests were carried out using a CHI660E electrochemical workstation. The specific steps are as follows: The test was carried out using a three-electrode system, in which the silver / silver chloride electrode was used as the reference electrode and the platinum wire electrode was used as the counter electrode. The materials prepared in Examples 1-4 and Comparative Example 1 were cut into a size of 2×2 cm as the working electrode. Figure 8 It is a schematic diagram of the working mechanism of the vacancy-coupled nano-tip material as the working electrode during electrochemically uranium extraction. The electrochemically uranium extraction performance test was carried out in simulated seawater. A 100 mL of 0.5 M Na2SO4 solution containing 100 mg / L of uranium was used. The uranium concentration in the solution before and after the reaction was measured by ICP-MS.

[0064] The surface element ratios of the electrode materials in Examples 1, 2 and Comparative Example 1 after 3-hour electrochemical reaction are shown in Table 1.

[0065] Table 1

[0066]

[0067] Figure 5 It is the electrochemically uranium extraction efficiency diagram of Examples 1-2 and Comparative Examples 1-3 in Application Example 1. The electric field formed by the high-curvature tip electron enrichment of V O -NCCONF prepared in Example 1 is stronger, and the uranium extraction rate is the highest. The V O -NDCONF prepared in Example 2 has a low curvature and no obvious electron enrichment, and the uranium extraction rate is slightly lower. The uranium extraction effect of Comparative Example 1 using only NF as the working electrode is the worst. After growing Co3O4 nanorods on the surface of NF in Comparative Examples 2-3, the uranium extraction efficiency is improved. Compared with Comparative Examples 2-3, the vacancy-coupled nano-tip materials V O -NCCONF and V O -NDCONF treated by Ar plasma in Examples 1-2 have significantly improved uranium extraction efficiency; at the same time, combined with Table 1 and Figure 5 it can be seen that after the electrochemical reaction of the materials prepared in Examples 1 and 2, V O -NDCONF prepared in Example 2 has the worst anti-scaling performance because there is no tip and the conductivity is a little worse, while NF has better conductivity so the anti-scaling performance is medium. The tip of V O -NCCONF prepared in Example 1 endows an enhanced electric field to overcome the deficiency of conductivity, and the tip has an effect on OH -The repulsive effect is the strongest, so the best effect is that the content of metal salt deposited on the electrode surface is significantly less than that on the electrode material surface in Comparative Example 1, and its anti-scaling performance is the best.

[0068] Figure 6 For the electrochemical uranium extraction efficiency diagrams of Examples 3-4 and Example 1 in Application Example 1, it can be seen that on the basis of Example 1, in Example 3, by calcining the polydopamine on the surface of NF, N and C are doped on NF. After doping N and C, V O -NCCONF can effectively improve the electron transfer efficiency and enhance the electrode performance when used as an electrochemical working electrode, thereby improving the uranium extraction rate; on the basis of Example 3, the uranium extraction efficiency in Example 4 is further improved. This is because "oxygen vacancy-hydroxyl" dual active sites are formed on the material surface: oxygen vacancies enhance the electron capture ability of uranyl ions, and hydroxyl groups improve the adsorption selectivity through hydrogen bonding.

[0069] Application Example 2

[0070] The material prepared in Example 1 was used for electrochemical uranium extraction testing in real seawater. The testing method was the same as that in Application Example 1, except that after adding 500 mg / L uranium to the real seawater, electrochemical uranium extraction was carried out for 6 h. After 6 hours of electrochemical uranium extraction, the full XPS spectrum of the V O -NCCONF electrode is as Figure 7 shown, Figure 7 and the photos of the V O -NCCONF electrode before and after the reaction are respectively shown in O . It can be seen that two new main peaks are detected in the XPS spectrum of V O -NCCONF after electrochemical uranium extraction, which are respectively attributed to U and Na. In addition, no other obvious metal element peaks are detected, indicating that V

[0071] Application Example 3

[0072] The V O -NCCONF prepared in Example 1 of the present invention and other electrochemical uranium extraction materials in the prior art were respectively tested for the amount of electrochemical uranium extraction. The results are as Figure 9 shown. It can be seen that the amount of electrochemical uranium extraction of V O -NCCONF prepared in Example 1 of the present invention (the abscissa 1 in Figure 9 ) reaches 1.93 mg g -1 d -1 , which is significantly better than the amount of arc electrochemical uranium extraction of other materials in the prior art (the abscissa 2-11 in Figure 9 ).

[0073] Although the embodiments of the present invention have been disclosed as above, they are not limited to the applications listed in the specification and embodiments. It can be fully applied to various fields suitable for the present invention. For those skilled in the art, additional modifications can be easily made. Therefore, without departing from the general concept defined by the claims and their equivalents, the present invention is not limited to the specific details and the examples shown and described herein.

Claims

1. A preparation method of a vacancy-coupled nano-tip material for electrochemically extracting uranium from seawater, characterized in that It includes the following steps: Step 1: Cut nickel foam into slices of different sizes, then ultrasonically treat it in acetone, ethanol, pure water, and hydrochloric acid solution in sequence. After thoroughly rinsing with pure water, dry it in a vacuum drying oven for later use; Step 2: Dissolve cobalt source, urea, and ammonium fluoride in pure water. After stirring, transfer the solution to a polytetrafluoroethylene liner, then add the treated nickel foam, and react in a high-pressure reactor for a period of time. After the reaction is completed, take out the material, rinse it with pure water, and then dry it in a vacuum drying oven; Step 3: Calcinate the dried sheet material in a muffle furnace, and then treat it with Ar plasma in an Ar plasma cleaner to obtain a vacancy-coupled nano-tip material.

2. The preparation method of the vacancy-coupled nano-tip material for electrochemically extracting uranium from seawater according to claim 1, wherein, In Step 1, the size of the nickel foam is 2×2 cm or 2×3 cm, the concentration of the hydrochloric acid solution is 0.6 mol / L, and the ultrasonic treatment is for 15 - 20 min.

3. The preparation method of the vacancy-coupled nano-tip material for electrochemically extracting uranium from seawater according to claim 1, characterized in that, In Step 2, the dosage ratio of cobalt source, urea, ammonium fluoride, and water is 0.1 - 0.6 g:0.1 - 0.6:0 - 0.4 g:10 - 20 mL. The cobalt source is cobalt nitrate or cobalt acetate, and the dosage ratio of nickel foam to water is 1 - 2 g:10 - 20 mL.

4. The preparation method of the vacancy-coupled nano-tip material for electrochemically extracting uranium from seawater according to claim 1, characterized in that, In Step 2, the reaction pressure is atmospheric pressure, the reaction temperature is 100 - 150 °C, and the reaction time is 6 - 8 h.

5. The preparation method of the vacancy-coupled nano-tip material for electrochemically extracting uranium from seawater according to claim 1, characterized in that, In Step 3, the calcination temperature is 300 - 500 °C, the calcination time is 2 - 3 h, and the Ar plasma treatment is for 10 - 20 min.

6. The preparation method of the vacancy-coupled nano-tip material for electrochemically extracting uranium from seawater according to claim 1, characterized in that, After treating the nickel foam in Step 1, perform N and C doping modification on it. The method is: put the treated nickel foam into Tris buffer solution, add hydrochloric acid dopamine, adjust the pH to 8.0 - 9.0, stir and react for a certain time, then take it out, wash, and dry.

7. The preparation method of the vacancy-coupled nano-tip material for electrochemically extracting uranium from seawater according to claim 6, characterized in that, The concentration of hydrochloric acid dopamine in the Tris buffer solution is 1 - 4 mg / mL, the dosage ratio of nickel foam to hydrochloric acid dopamine is 1:0.25 - 0.5, and the stirring reaction is for 3 - 6 h.

8. The preparation method of the vacancy-coupled nano-tip material for electrochemically extracting uranium from seawater according to claim 1, characterized in that, When calcining the sheet material in Step 3, introduce 3 - 5 Vol% of water vapor into the calcination gas.

9. Use of a vacancy-coupled nano-tip material for electrochemically extracting uranium from seawater prepared by the preparation method according to any one of claims 1 to 8, characterized in that, Use the obtained vacancy-coupled nano-tip material as the working electrode for electrochemically extracting uranium from seawater.

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