CN109930147B - Lead bipolar plate and preparation method thereof - Google Patents
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Abstract
The invention belongs to the technical field of surface engineering treatment, and particularly relates to a lead bipolar plate and a preparation method thereof, wherein the lead bipolar plate is prepared by a cold spraying process, a layer of compact lead or lead alloy coating with the thickness of 50 mu m-5mm is deposited on the surface of a substrate with excellent mechanical strength, bonding strength and deformation resistance through cold spraying, and the prepared lead bipolar plate can be directly used as an anode and can also form PbO through anodic oxidation2As an anode of an electrolytic system, the porosity of a lead coating is lower than 1%, the oxygen evolution potential is more than +1.5V (VS.SCE), the electrode reinforced electrolysis service life reaches more than 2000h, the problems of insufficient strength and passivation falling of a lead electrode can be solved, the assembly performance is better, the manufacturing and using cost of the lead electrode is greatly saved, the lead electrode can be widely applied to various industries such as electrolytic zinc, electrolytic copper, organic synthesis, advanced oxidation, ozone preparation, sewage treatment and the like, and the lead electrode has great economic benefits.
Description
The technical field is as follows:
the invention belongs to the technical field of surface engineering treatment, and particularly relates to a lead bipolar plate and a preparation method thereof.
Background art:
the lead alloy electrode has the advantages of high oxygen evolution potential, good corrosion resistance, excellent conductivity, low price and stable neutral property in various salt and acid solutions, so that the lead alloy electrode is widely applied to various industries such as electro-galvanizing, electrolytic copper, organic synthesis, advanced oxidation, ozone preparation, sewage treatment and the like. The oxide on the surface of the lead enables the lead alloy electrode to have the quality, the early lead electrode is used after metal lead is subjected to anodic oxidation or is directly used, however, even if the lead electrode is subjected to anodic polarization, the surface of the lead electrode is corroded to generate the lead oxide, the lead oxide is mostly conductive, the conductivity of the lead electrode is not reduced, and the expansion coefficients are all similar. However, lead anodes can creep during use due to the metal itselfOr residual stress of machining, and bending may occur during packaging or transportation. After the polar plate is deformed or bent, the cathode and the anode are easy to physically contact to form a short circuit when the electrode is used, the current efficiency of the electrode is greatly reduced, the anode plate and the cathode plate are easy to burn, the anode plate and the cathode plate are damaged, the production cost is increased, and the waste is more waste. The traditional method for treating the deformed anode plate is to use a punching hole or install an insulator to prevent the contact of the electrode plate, for example, when the electrode plate is bent or deformed too much, the cathode plate and the anode plate are in hard contact with each other along with the deposition of cathode copper on the cathode plate, and the groove and the storage tank of the electrode plate are influenced, so that the continuous deformation of the cathode plate can be caused after long-term use, and the adverse influence is brought to production, management and cost control. In the prior art, the common method for overcoming the deformation of the polar plate is to directly deposit PbO on the surface of the valve metal2By virtue of the excellent mechanical properties of the metal and PbO2The outstanding electrochemical performance solves the problems of insufficient structural strength and short service life of the electrode, typical valve metals comprise titanium, zirconium, tantalum and the like, and titanium is a widely-used lead electrode substrate supporting material at present due to relatively low price. But due to PbO2The medium is easy to permeate into the matrix to react with the titanium matrix, so that titanium is corroded and passivated, the bath pressure of an electrolytic cell is greatly increased, the electrochemical reaction cannot be carried out, and meanwhile, the problems of volume expansion and stress increase caused by corrosion products of titanium are solved, so that the active component PbO is prepared2The layers fall off. Improvement of active component PbO by coating intermediate layer of tantalum, tin-tellurium alloy and the like2The method for layer peeling has multiple working procedures and is extremely complex, and the active component PbO is improved by the intermediate layer formed by the methods of electroplating and the like2The layer-dropping method cannot ensure complete isolation of the substrate, so that the risk of substrate passivation failure exists, and the defect of high cost for manufacturing the electrode also exists. Coating a lead alloy on the surface of metal to form a compact lead layer, and directly using or forming PbO by anodic oxidation2Layer reuse, i.e. passing the medium through PbO2The penetration into the substrate causes corrosion of the substrate and the formation of electrochemically active lead compounds, a process which is very promising in terms of application potential.
The lead anode plate for electrolytic deposition disclosed in the chinese patent 201210480109.0 comprises an anode plate and an electrolytic lead raw material arranged on the anode plate, wherein a pure lead plate is arranged on the anode plate, the lead plate is in the shape of a thin sheet, the lead plate is welded with a raw material tank, a plurality of through holes are uniformly distributed on the surface of the lead plate, the problem of gas stress is solved through gas guide holes, and the problems of poor reliability of a welded part and large resistance exist, which affects the service life and reliability of the electrode; the lead peroxide electrode disclosed by the Chinese patent 201810294315.X comprises a lead sheet with a surface containing a lead oxide layer or a lead sheet with a surface containing a lead oxide layer, which is prepared by electrolyzing the lead sheet with the surface containing the lead oxide layer, has good electrochemical performance, but does not solve the problem of insufficient mechanical strength of the electrode; the device for correcting the deformed insoluble lead anode plate disclosed in the Chinese patent 201720811668.3 comprises an integral steel frame, a hydraulic station, a hydraulic piston cylinder, a plate surface correcting support plate, a plate surface correcting pressure plate, a hydraulic station support and a conductive cross beam correcting fastening bolt; the integral steel frame is fixed on the front side of the plate surface correction support plate and is used for supporting the plate surface correction support plate; two side ends of the plate surface correcting support plate are connected with two side ends of the plate surface correcting pressure plate through half-tooth bolts; the hydraulic station provides hydraulic pressure for the hydraulic piston cylinder, the movable end of the hydraulic piston cylinder is positioned in front of the plate surface correcting pressure plate, the movable end moves forwards and then presses the plate surface correcting pressure plate, the fixed end of the hydraulic piston cylinder is connected with the plate surface correcting support plate through a hydraulic station support, namely, the fixed end of the hydraulic piston cylinder is fixed with the hydraulic station support, and two ends of the hydraulic station support are fixed at two side ends of the plate surface correcting support plate; the conductive cross beam correction fastening bolt is positioned at the upper section of the plate surface correction pressing plate; the front end of the conductive cross beam correction fastening bolt extends out of the plate surface correction pressing plate, so that the problem of short circuit of an electrode can be solved, and the problem of falling failure of effective components caused by electrode deformation can not be solved; the titanium-based lead dioxide electrode modified by strontium chromium-doped titanate disclosed in Chinese patent 201510863863.6 comprises a substrate and a plating layer, wherein the substrate is a titanium substrate, the plating layer is composed of lead dioxide modified by strontium chromium-doped titanate, the content of the strontium chromium-doped titanate in the plating layer is 5-12 wt%, the thickness of the plating layer is 0.2-1mm, and the lead dioxide is beta-PbO2China specialityThe utility model 201711146830.5 discloses a titanium-based lanthanum-doped lead dioxide electrode, the body of which is a titanium plate substrate, the titanium plate substrate is wrapped with a nafion film coated with a modified carbon nano tube as a bottom layer, and a lanthanum-doped lead dioxide intermediate layer and a surface active layer are generated on the bottom layer through electrodeposition, and a preparation method of the nano lead dioxide electrode disclosed in the Chinese patent 201110008379.7 comprises the following steps: (1) preparing a titanium dioxide nanotube array substrate; (2) preparing lead dioxide electrodeposition liquid; (3) the preparation of the nano lead dioxide electrode on the titanium dioxide nanotube array substrate by electrodeposition and the novel gradient composite lead dioxide anode plate disclosed in the Chinese patent 201710964712.9 comprise an iron substrate, a ferrite transition layer coated on the iron substrate, and a composite alpha-PbO coated on the transition layer2Intermediate layer and composite alpha-PbO coated thereon2Composite beta-PbO on intermediate layer2An active layer; the ferrite transition layer is nickel oxide, copper oxide, iron oxide, zinc oxide and CaCO3One or more than two of Si, graphite and PbS powder are mixed in a wet way and calcined, then crushed, added with CaS and polyvinyl alcohol solution and sprayed on an iron substrate after being stirred; the complex alpha-PbO2The intermediate layer material is alpha-PbO2-ZrO2(ii) a The complex beta-PbO2The active layer material is beta-PbO2-ZrO2-carbon nanotubes-MnO2；The service life of the titanium-based lead dioxide electrode is prolonged by doping, intermediate layer and nanocrystallization, which can be greatly improved, but the failure mechanism of the electrode cannot be fundamentally changed, the reliability of the service life cannot be ensured, and the failure is still fast under the condition of large current. Therefore, a bipolar plate electrode material system is researched and designed, a compact lead or lead alloy layer is prepared on a substrate through a cold spraying method, a medium and the substrate are completely and physically isolated to form a double-electrode system, the problem of low mechanical strength of lead is solved, and the preparation cost of the lead electrode material is reduced.
The invention content is as follows:
the invention aims to overcome the defects in the prior art, and designs a lead bipolar plate and a preparation method thereof, which simplify the preparation process of an electrode material, improve the service performance of the electrode material, reduce the preparation cost of the electrode material and solve the problem of passivation failure of a lead electrode matrix.
In order to achieve the purpose, the main structure of the lead bipolar plate comprises a substrate and a coating, wherein the coating with the thickness of 50-5mm is sprayed on the surface of the substrate; the shape of the basal body is flat plate, tubular or reticular, the material of the basal body is iron, copper, steel, titanium, ceramic or plastic, the basal body has no blind hole, chamfer angle less than 1.5mm and sharp part; the surface roughness of the coating is less than or equal to 1.5 mu m, the raw material of the coating is pure lead, bi-component lead alloy or multi-component lead alloy powder, the component for improving the lead electrode can be added into the powder, the percentage of the pores of the coating in the volume is less than or equal to 1 percent, no bluing points exist by adopting the national standard test method of the iron reagent, and no penetrating pores exist.
The preparation method of the lead bipolar plate comprises three steps of matrix pretreatment, coating raw material selection and coating cold spraying:
firstly, pretreatment of a substrate: according to the material, size and thickness of the base body required by setting, checking and cleaning the bulges, sharp corners and welding slag on the surface of the base body, cleaning the base body, carrying out sand blasting treatment on the spraying coating surface of the base body on a sand blasting machine, wherein the sand blasting angle is 50-90 degrees, and the sand blasting distance is 40-90mm, and finishing the pretreatment of the base body;
the substrate after sand blasting can not be polluted again, the surface of the substrate can be fully cleaned and coarsened, the rust removal grade meets the Sa2.5 grade and above specified in the Standard of Steel surface Corrosion grade and Rust removal grade before coating, the surface roughness of the substrate reaches Rz40-150 mu m, and the test requirement of a probe measurement method in the Steel surface roughness characteristic after steel surface treatment and spray cleaning before coating is met;
selecting raw materials of a coating layer: according to the requirements of spraying and use, selecting pure lead, bi-component lead alloy or multi-component lead alloy powder as a coating raw material, according to the performance requirements of a polar plate, the production process of the powder comprises ion atomization, smelting deposition and electrolysis, according to the spraying requirements, the particle size of the powder is 1-200 mu m, the powder is spherical, quasi-spherical, irregular strip or irregular, a component for improving a lead electrode is added into the powder, according to the performance requirements of the polar plate electrode, the content of an oxide in the bi-component lead alloy or multi-component lead alloy powder is less than or equal to 50%, and the component of the oxide is not limited to lead protoxide, lead oxide, lead peroxide or non-quantitative compounds;
(III) cold spraying of the coating: according to the requirements of the set electrode bonding strength and compactness, the cold spraying equipment, the power air spraying equipment, the cold air power spraying equipment, the low-pressure cold spraying equipment, the supersonic speed power spraying equipment, the warm spraying equipment, the choking type pressure pipeline device or the device for continuously accelerating the powder to the critical speed at low temperature is adopted to spray the powder on the surface of the substrate to form a coating, the structure of the nozzle is a typical supersonic nozzle which is scaled, a choking nozzle which is only shrunk, a straight pipe type nozzle or a nozzle which accelerates the lead to the critical deposition speed by high-pressure gas according to the spraying requirements, the spraying temperature is-40-220 ℃ according to the spraying requirements according to the process requirements, the spraying pressure is 0.4-5MPa, and compressed air, nitrogen, helium or the mixture of any of the gases is adopted as a carrier gas in the spraying process, the spraying distance is 0.5-10cm, the spraying angle is 30-90 degrees, the powder feeding speed and the nozzle walking speed are coordinated, the thickness of the coating is controlled to be 50-5mm, according to the use requirement, the tensile bonding strength of the coating is more than 7MPa so as to resist falling caused by stress in the use process and ensure the electric conductivity between the coating and the substrate, the coating is subjected to constant temperature heat treatment for 1-3h to eliminate the stress in the spraying process, and the cold spraying of the coating is completed.
The lead bipolar plate prepared by the invention has the oxygen evolution potential of more than 1.5V and the oxygen evolution potential of more than 1.55V after anodic oxidation.
The lead bipolar plate prepared by the invention has the characteristic of compactness, and can be used for NaCl solution and NaSO4Solution, H2SO4The solution electrolyzes domestic sewage, industrial sewage and medical sewage.
The lead bipolar plate prepared by the invention can be directly used or oxidized by adopting an anodic oxidation process to generate PbO2And then used, the anodic oxidation process comprises the following steps: by using lead salt solutionsAnodizing to obtain lead dioxide, oxidizing divalent lead salt with chlorine, bromine or hypochlorous acid in alkaline solution to obtain lead dioxide, and reacting sodium peroxide or peroxodisulfate as oxidant with suspension of lead tetraoxide to obtain lead dioxide, wherein the anodizing time is 15-60min to ensure the service life of the electrode.
The lead bipolar plate prepared by the invention is processed into alpha-PbO with an intermediate layer2Surface of beta-PbO2The layered structure of (2) can improve service life and efficiency.
Compared with the prior art, the invention deposits a layer of compact lead or lead alloy coating with the thickness of 50 mu m-5mm on the surface of a substrate with excellent mechanical strength, bonding strength and deformation resistance through cold spraying, and the prepared lead bipolar plate can be directly used as an anode and can also form PbO through anodic oxidation2As an anode of an electrolytic system, the porosity of a lead coating is lower than 1%, the oxygen evolution potential is more than +1.5V (VS.SCE), the electrode reinforced electrolysis service life reaches more than 2000h, the problems of insufficient strength and passivation falling of a lead electrode can be solved, the assembly performance is better, the manufacturing and using cost of the lead electrode is greatly saved, the lead electrode can be widely applied to various industries such as electrolytic zinc, electrolytic copper, organic synthesis, advanced oxidation, ozone preparation, sewage treatment and the like, and the lead electrode has great economic benefits.
Description of the drawings:
FIG. 1 is a block diagram of the process flow of the present invention.
Fig. 2 is a schematic view of the principal structural principle of a lead bipolar plate according to embodiment 1 of the present invention.
And (3) a macro morphology graph of the aluminum-based boron carbide composite coating.
Fig. 3 is a schematic view of the principal structural principle of a lead bipolar plate according to embodiment 2 of the present invention.
FIG. 4 is a macroscopic surface topography map of the coating prepared in example 3 of the present invention.
FIG. 5 is a microscopic surface topography of the coating prepared in example 3 of the present invention.
FIG. 6 is a microscopic cross-sectional profile of the coating prepared in example 3 of the present invention.
FIG. 7 is a microscopic energy spectrum of the coating prepared in example 3 of the present invention.
FIG. 8 is a graph showing the linear relationship between the cell pressure and the electrolysis time in the coating strengthening electrolysis prepared in example 3 of the present invention.
The specific implementation mode is as follows:
the following is a further description by way of example and with reference to the accompanying drawings.
Example 1:
the main structure of the lead bipolar plate related to the embodiment comprises a substrate 1 and a coating 2, wherein the coating 2 with the thickness of 50 μm is sprayed on one side surface of the substrate 1 with a flat structure; the material of the substrate 1 is iron.
Example 2:
the main structure of the lead bipolar plate related to the embodiment comprises a substrate 1 and a coating 2, wherein the coating 2 with the thickness of 50 μm is sprayed on the two side surfaces of the substrate 1 with a flat structure; the material of the substrate 1 is iron.
The lead bipolar plate according to the present embodiment is applied to an electrochemical system.
Example 3:
the technical process of the lead polar plate preparation method related by the embodiment is as follows: spraying lead powder with the particle size of 10-50 mu m on the surface of a substrate 1 under the conditions that the powder feeding rate is 1.5g/s, the spraying distance is not 25mm, the spraying temperature is 20 ℃, the spraying pressure is 0.5MPa and the traveling speed is 20mm/s to obtain a coating 2 with the thickness of 500 mu m and the porosity of less than 0.5 percent, as shown in figure 4, the surface of the coating 2 has a compact structure, and after being pulled off, the surface has a large number of tough vortexes, as shown in figures 5-7, the coating 2 is sprayed on the surface of the substrate 1 at the speed of 1A/cm in a sulfuric acid solution2The electrolyte does not fail after 1460h of intensified electrolysis under the electrolysis current, as shown in FIG. 8.
Claims (4)
1. The preparation method of the lead bipolar plate is characterized in that the process comprises three steps of matrix pretreatment, coating raw material selection and coating cold spraying:
firstly, pretreatment of a substrate: according to the material, size and thickness of the base body required by setting, checking and cleaning the bulges, sharp corners and welding slag on the surface of the base body, cleaning the base body, carrying out sand blasting treatment on the spraying coating surface of the base body on a sand blasting machine, wherein the sand blasting angle is 50-90 degrees, and the sand blasting distance is 40-90mm, and finishing the pretreatment of the base body;
the substrate after sand blasting can not be polluted again, the surface of the substrate can be fully cleaned and coarsened, the rust removal grade meets the Sa2.5 grade and above specified in the Standard of Steel surface Corrosion grade and Rust removal grade before coating, the surface roughness of the substrate reaches Rz40-150 mu m, and the test requirement of a probe measurement method in the Steel surface roughness characteristic after steel surface treatment and spray cleaning before coating is met;
selecting raw materials of a coating layer: according to the requirements of spraying and use, pure lead, a two-component lead alloy or a multi-component lead alloy powder is selected as a coating raw material, according to the performance requirements of a polar plate, the production process of the powder comprises ion atomization, smelting deposition and electrolysis, according to the spraying requirements, the particle size of the powder is 1-200 mu m, the powder is spherical, quasi-spherical, irregular strip or irregular, according to the performance requirements of a polar plate electrode, the content of an oxide in the two-component lead alloy or the multi-component lead alloy powder is less than or equal to 50%, and the components of the oxide are not limited to lead protoxide, lead oxide and lead peroxide;
(III) cold spraying of the coating: according to the requirements of the set electrode bonding strength and compactness, the cold spraying equipment, the power air spraying equipment, the cold air power spraying equipment, the low-pressure cold spraying equipment, the supersonic speed power spraying equipment, the warm spraying equipment, the choking type pressure pipeline device or the device for continuously accelerating the powder to the critical speed at low temperature is adopted to spray the powder on the surface of the substrate to form a coating, the structure of the nozzle is a typical supersonic nozzle which is scaled, a choking nozzle which is only shrunk, a straight pipe type nozzle or a nozzle which accelerates the lead to the critical deposition speed by high-pressure gas according to the spraying requirements, the spraying temperature is-40-220 ℃ according to the spraying requirements according to the process requirements, the spraying pressure is 0.4-5MPa, and compressed air, nitrogen, helium or the mixture of any of the gases is adopted as a carrier gas in the spraying process, the spraying distance is 0.5-10cm, the spraying angle is 30-90 degrees, the powder feeding speed and the nozzle walking speed are coordinated, the thickness of the coating is controlled to be 50-5mm, according to the use requirement, the tensile bonding strength of the coating is more than 7MPa so as to resist falling caused by stress in the use process and ensure the electric conductivity between the coating and the matrix, the constant temperature heat treatment is carried out on the coating for 1-3h, the stress in the spraying process is eliminated, and the cold spraying of the coating is completed.
2. The method for preparing a lead bipolar plate according to claim 1, wherein the prepared lead bipolar plate has compactness characteristic and can be used for NaCl solution and Na2SO4Solution, H2SO4The solution electrolyzes domestic sewage, industrial sewage and medical sewage.
3. The method of claim 1, wherein the prepared lead bipolar plate can be directly used or oxidized by an anodic oxidation process to form PbO2And then used, the anodic oxidation process comprises the following steps: and (3) carrying out anodic oxidation by adopting a lead salt solution to prepare lead dioxide, wherein the anodic oxidation time is 15-60min, so as to ensure the service life of the electrode.
4. The method for preparing a lead bipolar plate according to claim 3, wherein the prepared lead bipolar plate has an oxygen evolution potential of 1.5V or more and an oxygen evolution potential of 1.55V or more through anodic oxidation.
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| CN110303236A (en) * | 2019-08-02 | 2019-10-08 | 中国兵器工业第五九研究所 | It is a kind of for tungsten or the hot isostatic pressing diffusion connection method of tungsten alloy and high strength steel |
| CN110760875A (en) * | 2019-10-30 | 2020-02-07 | 广东省新材料研究所 | All-solid-state rapid preparation method of alkaline electrolytic water electrode |
| CN112226785A (en) * | 2020-09-03 | 2021-01-15 | 广东臻鼎环境科技有限公司 | Foam copper-based composite lead electrode and preparation method thereof |
| CN112226786A (en) * | 2020-09-03 | 2021-01-15 | 广东臻鼎环境科技有限公司 | Composite lead dioxide electrode and preparation method thereof |
| CN112159987A (en) * | 2020-09-03 | 2021-01-01 | 广东臻鼎环境科技有限公司 | Sandwich structure composite lead electrode and preparation method thereof |
| CN113088957B (en) * | 2021-02-20 | 2022-09-02 | 景德镇明兴航空锻压有限公司 | Method for preparing wear-resistant and high-temperature-resistant coating on surface of titanium alloy through laser cladding |
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| US9168546B2 (en) * | 2008-12-12 | 2015-10-27 | National Research Council Of Canada | Cold gas dynamic spray apparatus, system and method |
| CN101736390B (en) * | 2009-12-24 | 2011-09-07 | 北京有色金属研究总院 | Lead dioxide electrode plate and preparation method thereof |
| CN102534654A (en) * | 2010-12-17 | 2012-07-04 | 北京有色金属研究总院 | Method for manufacturing lead dioxide electrode plate on metal substrate |
| CN108998790B (en) * | 2018-08-21 | 2020-06-19 | 中国船舶重工集团公司第七二五研究所 | Preparation method of aluminum-based boron carbide composite coating |
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| US5143806A (en) * | 1989-05-02 | 1992-09-01 | Globe-Union Inc. | Process for forming barium metaplumbate |
| CN203637271U (en) * | 2013-11-01 | 2014-06-11 | 昆明理工大学 | Light conductive core reinforced type lead-based double-metal laminated plate |
| DE102014105000A1 (en) * | 2014-04-08 | 2015-10-08 | Infineon Technologies Ag | Method for producing and assembling a circuit carrier |
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