CN114752946A - Preparation method of electrocatalytic water electrolysis bipolar plate - Google Patents
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Abstract
The invention discloses a preparation method of an electrocatalytic water electrolysis bipolar plate. The invention takes an iron sheet or a stainless steel sheet as a current collector, and prepares the bipolar plate capable of simultaneously generating excellent hydrogen and oxygen in an alkaline electrolyte by adopting a mild electrochemical in-situ growth and surface modification method. The bipolar plate has excellent electrocatalytic activity and stable performance, and can be connected in series or in parallel as required in the water electrolysis process to form a water electrolysis hydrogen production system. The bipolar plate is prepared from iron sheets or stainless steel sheets as raw materials, the cost of the raw materials is low, and the preparation cost of the electrode in unit area is only 1/6-1/5 of the prior art (foamed nickel); in addition, the preparation process does not need high-temperature and high-pressure reaction conditions, and the used electrolyte does not contain any organic component, so that the preparation method is environment-friendly; therefore, the preparation method of the invention can obviously reduce the cost of the bipolar plate and reduce the environmental pollution, and has simple and convenient preparation process, mild reaction condition and easy industrial production.
Description
Technical Field
The invention relates to the technical field of electrochemistry, in particular to a preparation method of an electrocatalytic water electrolysis bipolar plate.
Background
Hydrogen is a clean renewable energy source, the combustion product of which is water, and the environment pollution and the greenhouse effect are not generated, and the hydrogen is considered as an ideal energy carrier after fossil fuel is exhausted. Hydrogen production by alkaline water electrolysis is one of the most attractive methods for generating renewable energy, and not only can high-purity hydrogen be produced on a large scale, but also a conversion path between electric energy (especially clean energy such as wind power, photoelectric energy, valley period hydroelectric energy and the like) and hydrogen energy can be established. At 25 ℃, the theoretical decomposition voltage of water is 1.23V, and the corresponding electric energy consumption is 32.9kWh kg-1H2. However, due to the high cathodic hydrogen evolution and anodic oxygen evolution overpotentials, the actual power consumption is up to 48-54 kWh kg-1H2. Therefore, the key issue in the production of hydrogen by water electrolysis is to reduce the overpotential for cathodic hydrogen evolution and/or anodic oxygen evolution in order to produce hydrogen efficiently with as low an energy input as possible.
Heretofore, Pt group metals and Ru, Ir based compounds have been considered as the best catalysts for HER and OER performance, respectively, when IrO2And Pt for OER and HER, respectively, up to 10mA cm with an applied external voltage of 1.5V-2However, the current density is high, and the large-scale industrial application of Pt, Ir, Ru, and the like is not possible due to the high price and resource scarcity characteristics of these materials. Over the past decade, great progress has been made in understanding some key electrochemical transformations, particularly those involving water, hydrogen, and oxygen. With the help of volcanic curve, researchers have developed a series of non-noble metal high-efficiency electrocatalysts such as transition metal sulfides, transition metal phosphides, monatomic electrocatalysts and the like in succession from the aspects of improving intrinsic activity, improving active site density, strengthening process mass transfer and charge transfer, enhancing desorption of hydrogen and oxygen and the like. Nevertheless, most of the oxygen evolution catalysts and hydrogen evolution catalysts expected to be used are up to 10mA cm -2High overpotential of 250-400 mV and-100 mV are still needed respectively, and 10mA cm is reached when water electrolysis of two electrodes is formed-2The cell voltage of (2) is about 1.75V. Thus developing the preparation of non-noble metal electrolytic water electrode with higher performanceThe technology becomes one of the international research hotspots at present. In addition, in an electrolytic water system, generally, an electrode material accounts for 30-60% of the total manufacturing cost, in order to reduce the preparation cost of an electrocatalytic electrode and simplify the complexity of the water electrolysis system, a low-cost conductive material is used as a current collector to prepare a bipolar plate (bipolar plate) with high-activity hydrogen evolution and high-activity oxygen evolution simultaneously, so that a series connection structure and a parallel connection structure can be flexibly adopted according to needs when the water electrolysis system is formed, and the method is one of important means for reducing the manufacturing cost of the electrolytic water system to realize large-scale application.
Disclosure of Invention
The invention aims to solve the problems of high price of electrode materials, harsh reaction conditions and discharge of a large amount of waste in the production process in the prior art, and provides a preparation method of an electrocatalytic water electrolysis bipolar plate.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a preparation method of an electrocatalytic water electrolysis bipolar plate comprises the following steps:
S1, pretreating an electrode, wherein the electrode is an iron sheet or a stainless steel sheet;
s2, taking the electrode pretreated in S1 as a cathode, taking a graphite sheet or a stainless steel sheet as an anode, and taking transition metal sulfate and (NH)4)2SO4Performing electrodeposition with constant current as electrolyte, washing cathode, and drying to obtain electrode after constant current electrodeposition;
s3, taking the electrode after constant current electrodeposition in S2 as a cathode, taking a graphite sheet or a stainless steel sheet as an anode, and taking NaH as a cathode2PO2And alkaline solution is electrolyte, carry on the electrodeposition with the constant potential, dry after washing the negative pole, make the electrode after the electrodeposition of constant potential;
and S4, taking the electrode subjected to constant potential electrodeposition in S3 as a working electrode, a graphite sheet or a stainless steel sheet as an auxiliary electrode, a saturated Ag/AgCl electrode as a reference electrode, and scanning for 50-500 circles in alkaline electrolyte by adopting a cyclic voltammetry method at a rate of 50-300 mV/S within a range of-1.0V, wherein the scanned working electrode is the bipolar plate.
Preferably, the pretreatment in S1 is to remove rust and polish the electrode for 10-30 seconds by using 3mol/L HCl, then ultrasonically treat the electrode for 5-15 minutes by using ultrapure water, and blow the electrode by cold air.
Preferably, the constant current in S2 is 50-250 mA/cm 2The electrodeposition time is 5 to 20 minutes.
Preferably, the transition metal sulfate in S2 is CoSO4Or NiSO4Said CoSO4Or NiSO40.05 to 0.5 mol/L; said (NH)4)2SO40.1 to 0.5 mol/L.
More preferably, the constant potential in S3 is-0.5V to-1.2V (relative to a saturated Ag/AgCl electrode), and the electrodeposition time is 50-300 seconds.
Further preferably, the alkaline solution in S3 is NaOH or KOH, and the NaOH or KOH is 0.5 mol/L; the NaH2PO20.01 to 0.1 mol/L.
More preferably, the alkaline electrolyte in S4 is 1.0mol/L KOH.
The invention has the following beneficial effects:
firstly), an iron sheet or a stainless steel sheet is used as a current collector, and a mild electrochemical in-situ growth and surface modification method is adopted to prepare the bipolar plate which can simultaneously generate hydrogen and oxygen in an alkaline electrolyte, the bipolar plate has excellent electrocatalytic activity and stable performance, and can be connected in series or in parallel as required in the water electrolysis process to form an electrolyzed water hydrogen production system;
secondly) the bipolar plate prepared by the method forms a two-electrode electrolytic water system, takes 1mol/L KOH as electrolyte and has the cathode current density of 10mA/cm at room temperature2The cell voltage of (1) is about 1.60V; at the cathode current density of 100mA/cm 2The cell voltage of (2) is about 1.90V; the bipolar plate assembly prepared by the method of the invention has a two-electrode system with a cathode current density of 40mA/cm2The voltage fluctuation of the cell is only 5-10 mV after the cell is continuously operated for 48 hours at room temperature;
thirdly), the bipolar plate prepared in the invention is made of iron sheets or stainless steel sheets, the cost of the raw materials is low, and the preparation cost of the electrode in unit area is only 1/6-1/5 of the prior art (foamed nickel); in addition, the preparation process does not need high-temperature and high-pressure reaction conditions, and the used electrolyte does not contain any organic component, so that the preparation method is environment-friendly; therefore, the preparation method of the invention can obviously reduce the cost of the bipolar plate and reduce the environmental pollution, and has simple and convenient preparation process, mild reaction condition and easy industrial production.
Drawings
FIG. 1 is a schematic flow chart of the technique for preparing bipolar plate according to the present invention;
FIG. 2 is NiOOH @ Ni in example 1xThe current density-voltage curve of the two electrode systems of the P/FF bipolar plate;
FIG. 3 is NiOOH @ Ni in example 1xP/FF bipolar plate two electrode system with constant current of 40mA/cm2Time voltage-time curve;
FIG. 4 shows Ni in example 2y(Co)1-yOOH@NiCo1-xThe current density-voltage curve of the two electrode systems of the P/SF bipolar plate;
FIG. 5 shows Ni in example 2y(Co)1-yOOH@NiCo1-xP/SF bipolar plate two electrode system with constant current of 40mA/cm 2Voltage-time curve of time;
FIG. 6 is the CoOOH @ Co example 3xThe voltage-current density curve of two electrode systems of the P/SF bipolar plate;
FIG. 7 is the CoOOH @ Co example 3xThe two electrode bodies of the P/SF bipolar plate system have a current density of 10mA/cm2、40mA/cm2Voltage-time electrical curve of time.
Detailed Description
The invention is further described with reference to the following figures and specific examples.
Example 1
The method comprises the following steps: and (4) derusting and polishing pretreatment of the iron sheet. Polishing the iron sheet with the thickness of 0.3mm in 3mol/L HCl for 15s, taking out, repeatedly washing the iron sheet with ultrapure water, then cleaning the iron sheet with the ultrapure water for 10 minutes, taking out, and drying the iron sheet with cold air for later use.
Step two: electrodepositing nickel hydride. Taking the polished iron sheet as a cathode and 0.1mol/L NiSO4+0.5mol/L(NH4)2SO4Is used as electrolyte and the high-purity graphite plate isAnode with electrode distance of 5cm at room temperature of 150mA/cm2Taking out after electrodeposition is carried out for 10 minutes under constant current, washing with ultrapure water, and drying with cold air for later use.
Step three: the electrode prepared in the second step is used as a cathode, the stainless steel sheet is used as an auxiliary electrode, and 0.5mol/L KOH +0.05mol/L NaH is used2PO2Taking out the electrolyte after electrodeposition for 150 seconds at-1.0V (relative to a saturated Ag/AgCl electrode), washing the electrolyte clean by ultrapure water, and drying the electrolyte by cold air for later use.
Step four: and (3) taking the electrode prepared in the third step as a working electrode, a high-purity graphite plate as an auxiliary electrode and a saturated Ag/AgCl electrode as a reference electrode, and scanning for 150 circles by a cyclic voltammetry method at a rate of 100mV/s within a range of-1.0V. The prepared electrode is formed by growing NiOOH @ Ni in situ by taking an iron sheet as a current collectorxP bipolar plate NiOOH @ NixP/FF (FF represents iron sheet).
NiOOH @ Ni prepared by the fourth stepxThe P/FF bipolar plate is used as a cathode and an anode, 1.0mol/L KOH is used as electrolyte, the temperature is room temperature, non-woven fabric is used as a diaphragm to form a two-electrode electrolytic water system, and the current density of the cathode is measured to be 10mA/cm2The cell voltage of (2) is 1.603V, and the cathode current density is 100mA/cm2The cell voltage of (a) is 1.893V (as shown in fig. 2). The two-electrode system has a cathode current density of 40mA/cm2And the voltage fluctuation of the cell is less than 10mV (shown in figure 3) after the cell is continuously operated for 48h at room temperature.
Example 2
The method comprises the following steps: rust removing and polishing pretreatment of the stainless steel sheet. Polishing a stainless steel sheet with the thickness of 0.3mm in 3mol/L HCl for 30s, taking out, repeatedly washing the stainless steel sheet with ultrapure water, cleaning the stainless steel sheet with the ultrapure water for 15 minutes, taking out, and drying the stainless steel sheet with cold air for later use.
Step two: electrodepositing nickel cobalt hydride. Taking the polished iron sheet as a cathode and 0.05mol/L NiSO 4+0.05mol/L CoSO4+0.5mol/L(NH4)2SO4Is used as electrolyte, high-purity graphite plate is used as anode, the electrode distance is 5cm, the temperature is room temperature, and the temperature is 200mA/cm2Taking out the film after electrodeposition for 15 minutes under constant current, washing the film with ultrapure water, and drying the film with cold air for later use.
Step three: taking the electrode prepared in the second step as a cathode, a stainless steel sheet as an auxiliary electrode, and 0.5mol/L NaOH +0.1mol/L NaH2PO2Taking out the electrolyte after electrodeposition for 300 seconds at-1.2V (relative to a saturated Ag/AgCl electrode), washing the electrolyte clean with ultrapure water, and drying the electrolyte with cold air for later use.
Step four: and (3) scanning for 300 circles by a cyclic voltammetry method at a rate of 150mV/s within the range of-1.0V by taking the electrode prepared in the third step as a working electrode, a high-purity graphite plate as an auxiliary electrode and a saturated Ag/AgCl electrode as a reference electrode. The prepared electrode takes an iron sheet as a current collector to grow Ni in situy(Co)1-yOOH@NiCo1-xP bipolar plate Niy(Co)1-yOOH@NiCo1-xP/SF (SF means stainless steel sheet).
Ni prepared by the fourth stepy(Co)1-yOOH@NiCo1-xThe P/SF bipolar plate is used as a cathode and an anode, 1.0mol/LKOH is used as electrolyte, the temperature is room temperature, non-woven fabric is used as a diaphragm to form a two-electrode electrolytic water system, and the current density of the cathode is measured to be 10mA/cm2The cell voltage of (2) is 1.574V, and the cathode current density is 100mA/cm2The cell voltage of (a) is 1.829V (as shown in fig. 4). The two-electrode system has a cathode current density of 40mA/cm 2The voltage fluctuation of the cell is about 6mV (shown in figure 5) when the cell is continuously operated for 48 hours at room temperature.
Example 3
The method comprises the following steps: rust removing and polishing pretreatment of the stainless steel sheet. Polishing a stainless steel sheet with the thickness of 0.3mm in 3mol/L HCl for 30s, taking out, repeatedly washing the stainless steel sheet with ultrapure water, then cleaning the stainless steel sheet in the ultrapure water for 15 minutes, taking out, and drying the stainless steel sheet with cold air for later use.
Step two: cobalt hydroxide was electrodeposited. Using polished stainless steel as cathode, 0.1mol/L CoSO4+0.25mol/L(NH4)2SO4The electrolyte is high-purity graphite flake as anode, the electrode distance is 5cm, the temperature is room temperature, and the temperature is 50mA/cm2Taking out after electrodeposition is carried out for 20 minutes under constant current, washing with ultrapure water, and drying with cold air for later use.
Step three: the electrode prepared in the second step is used as a cathode, the stainless steel sheet is used as an auxiliary electrode, and 0.5mol/L KOH +0.05mol/LNaH2PO2Taking out the electrolyte after electrodeposition is carried out for 200 seconds at-1.0V (relative to a saturated Ag/AgCl electrode), washing the electrolyte by using ultrapure water, and blowing the electrolyte by using cold air for later use.
Step four: and (3) scanning for 300 circles by using the electrode prepared in the third step as a working electrode, a high-purity graphite sheet as an auxiliary electrode and a saturated Ag/AgCl electrode as a reference electrode in a cyclic voltammetry method at a rate of 250mV/s within the range of-1.0V. The prepared electrode takes a stainless steel sheet as a current collector to grow CoOOH @ Co in situ xP bipolar plate CoOOH @ CoxP/SF (SF means stainless steel sheet).
CoOOH @ Co prepared in the fourth stepxThe P/SF bipolar plate is used as a cathode and an anode, 1.0mol/L KOH is used as electrolyte, the temperature is room temperature, non-woven fabric is used as a diaphragm to form a two-electrode electrolytic water system, and the current density of the cathode is measured to be 10mA/cm2The cell voltage of (2) is 1.620V, and the cathode current density is 100mA/cm2The cell voltage of (a) is 1.911V (as shown in fig. 6). The two-electrode system has a cathode current density of 10mA/cm2And 40mA/cm2The voltage fluctuation of the cell continuously running for 12h at room temperature is about 5mV (as shown in figure 7).
The flow chart of the preparation process of the bipolar plate in the invention is shown in the attached figure 1. The bipolar plate which is prepared by the method and takes the iron sheet or the stainless steel sheet as the current collector and the nickel or the cobalt hydroxide @ nickel or the cobalt phosphide as the active component can be used as a cathode hydrogen evolution electrode and an anode oxygen evolution electrode in alkaline electrolyte such as KOH. When the two-electrode electrolytic water system is formed, a series system or a parallel system can be assembled according to requirements, and when the series system is adopted, one surface of each of two surfaces of the electrode is used for hydrogen evolution, and the other surface of each of the two surfaces of the electrode is used for oxygen evolution; when a parallel system is used, both sides of the electrode either evolve oxygen or hydrogen simultaneously. The data of examples 1-3 fully illustrate that bipolar plates prepared according to the present invention constitute a two-electrode electrolytic water system with 1mol/L KOH as the electrolyte and a cathodic current density of 10mA/cm at room temperature 2The cell voltage of (2) is about 1.60V; at a cathode current density of 100mA/cm2The cell voltage of (2) is about 1.90V. Two-electrode system assembled by bipolar plates prepared by the invention has the cathode current density of 40mA/cm2Continuous operation for 48h at room temperatureThe concentration is only 5-10 mV.
In conclusion, the preparation method of the bipolar plate is simple, no organic reagent is introduced into the electrolyte, the reaction condition is mild, the bipolar plate is environment-friendly, the bonding force between the active component and the substrate is strong, the contact resistance is low, the electrocatalytic activity is high, the bipolar plate is not easy to fall off under the cavitation action of oxygen evolution or hydrogen evolution, and the performance is stable.
The present specification and figures are to be regarded as illustrative rather than restrictive, and it is intended that all such alterations and modifications that fall within the true spirit and scope of the invention, and that all such modifications and variations are included within the scope of the invention as determined by the appended claims without the use of inventive faculty.
Claims (7)
1. The preparation method of the electrocatalytic water electrolysis bipolar plate is characterized by comprising the following steps of:
s1, preprocessing an electrode, wherein the electrode is an iron sheet or a stainless steel sheet;
s2, taking the electrode pretreated in S1 as a cathode, taking a graphite sheet or a stainless steel sheet as an anode, and taking transition metal sulfate and (NH) 4)2SO4Performing electrodeposition with constant current as electrolyte, washing cathode, and drying to obtain electrode after constant current electrodeposition;
s3, taking the electrode after constant current electrodeposition in S2 as a cathode, taking a graphite sheet or a stainless steel sheet as an anode, and taking NaH as a cathode2PO2And alkaline solution is electrolyte, carry on the electrodeposition with the constant potential, dry after washing the negative pole, make the electrode after the electrodeposition of constant potential;
and S4, taking the electrode subjected to constant potential electrodeposition in S3 as a working electrode, a graphite sheet or a stainless steel sheet as an auxiliary electrode, a saturated Ag/AgCl electrode as a reference electrode, and scanning for 50-500 circles in alkaline electrolyte by adopting a cyclic voltammetry method at a rate of 50-300 mV/S within a range of-1.0V, wherein the scanned working electrode is the bipolar plate.
2. The preparation method according to claim 1, wherein the pretreatment in S1 is to derust and polish the electrode with 3mol/L HCl for 10 to 30 seconds, then ultrasonically treat the electrode with ultra pure water for 5 to 15 minutes, and blow the electrode with cold air.
3. The method according to claim 1, wherein the constant current in S2 is 50-250 mA/cm2The electrodeposition time is 5 to 20 minutes.
4. The method according to claim 1, wherein the transition metal sulfate in S2 is CoSO 4Or NiSO4Said CoSO4Or NiSO40.05 to 0.5 mol/L; said (NH)4)2SO40.1 to 0.5 mol/L.
5. The method according to claim 1, wherein the constant potential in S3 is-0.5V to-1.2V (relative to a saturated Ag/AgCl electrode), and the electrodeposition time is 50-300 seconds.
6. The preparation method of claim 1, wherein the basic solution in S3 is NaOH or KOH, and the NaOH or KOH is 0.5 mol/L; the NaH2PO20.01 to 0.1 mol/L.
7. The preparation method according to claim 1, wherein the alkaline electrolyte in S4 is 1.0mol/L KOH.
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