CN110923746A - Nano-porous Fe-P-C material, preparation method thereof and application thereof in hydrogen production by water electrolysis - Google Patents
Nano-porous Fe-P-C material, preparation method thereof and application thereof in hydrogen production by water electrolysis Download PDFInfo
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C25F3/00—Electrolytic etching or polishing
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- C25F3/06—Etching of iron or steel
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a nano porous Fe-P-C material, a preparation method thereof and application thereof in hydrogen production by water electrolysis, wherein a crystal strip of an alloy is prepared according to the following mass ratio: the mass percent of pure Fe is 22-64 percent, and Fe319 to 41 percent of P and Fe3The mass percent of C is 17% -37%, and the sum of the three components is 100%. Mixing and smelting metal raw materials to obtain an alloy ingot, melting and ejecting the alloy ingot to obtain an alloy strip, and performing ultrasonic vacuum drying. Using an electrochemical workstation three-electrode system, taking a calomel electrode as a reference electrode, a platinum net as a counter electrode, a Fe-P-C alloy strip as a working electrode, and H2SO4An aqueous solution as an electrolyte byElectrochemical corrosion is carried out at constant potential, the potential parameter is-0.1V to-0.5V, and the corrosion time is 600-1600 s. Compared with the noble metal catalyst in the market, the catalyst has higher price advantage, higher stability, simple and convenient preparation method, less flow and good market industrialization prospect.
Description
Technical Field
The invention relates to a nano-scale porous material, in particular to a nano-scale porous Fe-P-C material, a preparation method thereof and application thereof in hydrogen production by water electrolysis, which are mainly used as a cathode hydrogen production catalyst material in an electrolytic water system.
Background
With the large volume production of fossil fuels in recent years, the reserves of fossil fuels on earth have been decreasing. Fossil fuel combustion generates a large amount of greenhouse gases, which causes the global warming effect to be intensified, and then causes a series of ecological and environmental problems. With the increasing situation, hydrogen energy has attracted more and more attention in the field of new energy due to its high energy conversion efficiency and cleanness without pollution. However, anode catalyst activity and cost issues have been limiting the large scale application of direct fuel cells. Pt and Pt-based alloys are used as hydrogen production catalysts for electrolysis with the best performance, and the price and the reserves limit the commercial application of the hydrogen production catalysts. The P, C doped Fe-based nano-porous catalyst is prepared by an electrochemical dealloying method, and the mechanism of improving the performance of P, C doped materials in the field of hydrogen production by water electrolysis has been demonstrated by material characterization and electrochemical tests. The significance of the invention is that the doping of nonmetal P, C, S is a research hotspot in the field of water electrolysis in recent years, and the preparation process of the conventional multi-element nonmetal compound is complicated, so that the invention utilizes the alloying of nonmetal elements such as Fe3P and Fe3And C, the simple multi-element doped metal compound material is prepared, so that the preparation process is greatly simplified, and a thought is provided for the preparation of a novel multi-element non-metal element compound. The nanoporous material prepared by the electrochemical dealloying method is a catalyst that does not require a support. In the conventional carbon-supported nanoparticle catalyst, a serious coarse-term phenomenon occurs in a long-range catalysis process, so that the contact area between the nanoparticles and the carbon material is reduced. Therefore, the use of nanoporous materials to replace carbon-supported noble metal catalysts is a promising research direction.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a nano-porous Fe-P-C material, a preparation method thereof and application thereof in hydrogen production by water electrolysis, namely a method for preparing a nano-porous Fe-P-C cathode hydrogen production catalyst material for water electrolysis by using an electrochemical dealloying method.
The technical purpose of the invention is realized by the following technical scheme.
A nano porous Fe-P-C material and a preparation method thereof are carried out according to the following steps:
step 1, preparing Fe-P-C alloy strip
Mixing pure Fe and Fe3P、Fe3C is prepared according to the proportion, then is melted in an argon arc furnace to form an alloy ingot, and then a melt-spun machine is used for melting the alloy ingot, spraying the alloy ingot and rapidly cooling the alloy ingot to form an alloy strip, wherein the mass percent of pure Fe is 22-64 percent, and Fe319 to 41 percent of P and Fe3The mass percent of C is 17% -37%, and the sum of the three components is 100%.
In the step 1, cutting the prepared Fe-P-C (amorphous) alloy strip into small sections, putting the cut strip into a beaker, ultrasonically cleaning the strip in absolute ethyl alcohol, and then drying the strip in a vacuum drying oven at room temperature of 20-25 ℃ in vacuum.
In step 1, the mass percent of pure Fe is 30% -60%, and Fe325 to 40 percent of P and Fe3The mass percent of C is 20-30%.
In step 1, the raw materials are pure Fe and Fe3P、Fe3And C, mixing the raw materials according to a certain proportion, putting the mixture into an argon arc melting furnace, and starting to melt for 4-5 times to ensure that the alloy components are mixed more uniformly. Then taking out the alloy ingot to be crushed, taking the crushed blocks, putting the crushed blocks into a clean quartz tube after being cleaned by absolute ethyl alcohol through ultrasonic wave, placing the crushed blocks into a ribbon throwing machine, and spraying the melted liquid alloy onto a copper roller rotating at high speed after high vacuum is pumped so that the liquid is rapidly cooled to form a crystal ribbon instantly.
In step 1, the melt spinning machine needs to be pumped to 1 × 10-3Pa～1×10-2Pa, the rotating speed of the copper roller needs to be controlled within 3000-4000 revolutions per minute, and the pressure difference between the quartz tube and the interior of the furnace body needs to be controlled within 0.1-0.5 Pa.
In step 1, the prepared Fe-P-C alloy strip has the atomic content (mol percent) of Fe of 80-90%, the content of P of 5-10%, the content of C of 5-10%, and the three atomic ratios are added to be one hundred percent, has an iron crystal structure, and the elements P and C exist in a sample in the form of solid solution defects.
Step 2, preparing the nano porous Fe-P-C material by adopting an electrochemical dealloying method
Carrying out electrochemical corrosion on the Fe-P-C alloy strip prepared in the step 1 under constant potential, taking the Fe-P-C alloy strip as a working electrode, setting the potential parameter to be-0.5V-0.1V, the corrosion time to be 600-1600s and the electrolyte to be 0.1-1M sulfuric acid aqueous solution; and after the electrochemical corrosion is finished, taking out the sample, cleaning, and drying at room temperature in vacuum to obtain the nano porous Fe-P-C material.
In the step 2, the calomel electrode is used as a reference electrode, the platinum net is used as a counter electrode, and the alloy strip is used as a working electrode to carry out constant potential electrochemical corrosion.
In step 2, setting the corrosion potential to-0.3V-0.1V, the time to 1000-1500s, and the electrolyte to be 0.5-1M sulfuric acid water solution.
In the step 2, after the Fe-P-C alloy strip prepared in the step 1 is subjected to electrochemical dealloying, element atoms are not diffused synchronously in the dealloying process, so that partial amorphous and nanocrystalline are generated, a short-range ordered and long-range disordered structure is formed, and partial Fe atoms are corroded under constant potential corrosion to form a nanoporous morphology structure.
In the step 2, the sample is taken out and washed with deionized water and absolute ethyl alcohol for five times respectively, and then dried at the room temperature of 20-25 ℃ in vacuum to prevent oxidation, and finally the nano-porous structure nanocrystalline material is obtained.
The application of the nano porous Fe-P-C material in the water electrolysis cathode catalysis hydrogen production (namely the application in the water electrolysis hydrogen production) is that the current density is 10mA/cm2The overpotential in the case of time is 120-125 mV.
Compared with the prior art, the carbon-supported nanoparticle catalyst commonly used can generate serious coarse-term phenomenon in the long-range catalysis process, so that the contact area between the nanoparticles and the carbon material is reduced. The nanoparticles are easy to fall off during the catalytic reactionAnd dissolution, poor stability. The three-dimensional bicontinuous nano porous structure is prepared by a dealloying method, so that the stability of the material is improved, the specific surface area of the material is greatly increased, the material transmission is promoted, and the integral catalytic effect of the catalyst is finally improved. Compared with the prior art, the introduction of C and P increases the number of active sites of the material and improves the intrinsic catalytic activity of the material. The performance of the material in the field of hydrogen production by electrolyzing water is improved by doping P, C. And the raw material used by Fe-P-C is cheaper than the conventional commercial noble metal catalyst, and Fe3P and Fe3P is an industrial raw material, has higher price advantage and higher stability compared with the noble metal catalyst on the market, has simple and convenient preparation method and less flow, is beneficial to realizing industrial production and has good market industrialization prospect.
Drawings
FIG. 1 is an SEM photograph of the surface nano-porous structure of the Fe-P-C nanocrystalline material prepared in example 1.
FIG. 2 is an XRD spectrum of a Fe-P-C alloy strip prepared in example 1 before electrochemical etching.
FIG. 3 is an XRD spectrum of a Fe-P-C alloy strip prepared in example 1 after electrochemical etching.
FIG. 4 is a LSV curve diagram of Fe-P-C nano-porous material prepared in example 1 as a cathode material during hydrogen evolution by electrolysis of water.
FIG. 5 is a graph of current density versus time for electrochemical dealloying of Fe-P-C alloy strips prepared in example 1.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
Example 1
1. 5.1075g of pure iron (Fe) and iron phosphide (Fe) are weighed3P)1.517g, iron carbide (Fe)3C)1.375 g. The total sample was 8 g.
2. And (3) putting 8g of sample into an argon smelting furnace, pumping high vacuum by a molecular pump, introducing high-purity argon protective atmosphere, and smelting for 4 times to ensure that the internal components of the alloy are uniform. To obtain Fe90P5C5And (3) alloy ingots.
3. Then taking out the alloy ingot to be crushed, taking the fragments, ultrasonically cleaning the fragments by absolute ethyl alcohol, placing the fragments into a clean quartz tube, placing the fragments into a ribbon throwing machine, pumping high vacuum, and then spraying the melted liquid alloy onto a copper roller rotating at high speed to ensure that the liquid is rapidly cooled to form an amorphous ribbon instantly. The melt-spun machine needs to be drawn to 7 multiplied by 10-3Pa. The rotation speed of the copper roller needs to be controlled at 4000 revolutions per minute. The pressure difference between the quartz tube and the interior of the furnace body needs to be controlled at 0.4 Pa. To obtain Fe90P5C5A strip of crystalline alloy.
4. Mixing Fe90P5C5The amorphous alloy strip is cut into small sections, the width of the strip is 8mm, and the length of the strip is 20 mm. The cut strips were put into a beaker, sonicated in absolute ethanol for 20min, then washed with absolute ethanol, and then placed in a vacuum drying oven at room temperature for 12 hours.
5. Preparing an electrochemical workstation and a three-electrode system, taking a calomel electrode as a reference electrode, taking a platinum net as a counter electrode, taking an alloy strip as a working electrode, carrying out electrochemical corrosion on the Fe-P-C strip under constant potential, using 0.5M dilute sulfuric acid aqueous solution as electrolyte, sequentially washing the electrolyte with deionized water and absolute ethyl alcohol after taking out a sample, and then drying the sample at room temperature in vacuum to obtain the nano-crystalline material with the nano-porous structure.
As shown in the attached figure 1, SEM pictures of samples with the magnification of 2.5k, 30k and 100k show that the three-dimensional bicontinuous sponge-like nano-porous structure has large specific surface area and thus exposes more active sites, and the pore diameter and ligament size are about 100 +/-10 nm clearly shown in the pictures. As shown in FIGS. 2 and 3, the XRD pattern of the sample before dealloying, i.e., the XRD pattern of the bands, corresponds to iron crystals (Im-3m) for three peaks. 2 theta is 44.673 for (110), 65.021 for (200), and 82.333 for (211). P and C exist in the sample in the form of solid solution defects; compared with the XRD pattern before dealloying, the XRD pattern after dealloying of the sample has reduced peak intensity, which is caused by that the diffusion of element atoms is asynchronous in the dealloying process, so that partial amorphous and nanocrystalline are generated, and a short-range ordered and long-range disordered structure is formed. Use ofThe three-electrode system, calomel electrode as reference electrode, platinum net as counter electrode, nanocrystalline material as working electrode (as cathode), and electrolyte as 0.5M dilute sulfuric acid aqueous solution, as shown in figure 4. By LSV it can be found that the sample has a current density of 10mA/cm2The overpotential is 125mV, and for cheap metal element Fe, the overpotential of the current commercial platinum-carbon electrode is 30mV (AlfaAesar). The self-corrosion potential of the prepared nanocrystalline material component is measured to be-0.4225V, the corrosion time is 1520s when the potential parameter is set to be-0.3V (constant voltage is-0.3V), the nanocrystalline material is corroded until the current density is less than 50 mu A, the current density is increased and then reduced along with the prolonging of the time, the soluble components are less and less, and the corrosion reaction can be considered to stop when the current density is less than 50 mu A when the time is 1520 s.
Example 2
Weighing pure iron, iron phosphide and iron carbide, and smelting to obtain Fe80P10C10And (3) alloy ingots. Then taking out the alloy ingot to be crushed, taking the fragments, ultrasonically cleaning the fragments by absolute ethyl alcohol, placing the fragments into a clean quartz tube, placing the fragments into a ribbon throwing machine, pumping high vacuum, and then spraying the melted liquid alloy onto a copper roller rotating at high speed to ensure that the liquid is rapidly cooled to form an amorphous ribbon instantly. The melt-spun machine needs to be drawn to 7 multiplied by 10-3Pa. The rotation speed of the copper roller needs to be controlled at 4000 revolutions per minute. The pressure difference between the quartz tube and the interior of the furnace body needs to be controlled at 0.4 Pa. To obtain Fe80P10C10A strip of crystalline alloy. Cutting into small segments, wherein the width of the strip is 8mm, and the length of the strip is 20 mm. The cut strips were put into a beaker, sonicated in absolute ethanol for 20min, then washed with absolute ethanol, and then placed in a vacuum drying oven at room temperature for 12 hours.
Preparing an electrochemical workstation and a three-electrode system, taking a calomel electrode as a reference electrode, taking a platinum net as a counter electrode, taking an alloy strip as a working electrode, carrying out electrochemical corrosion on an Fe-P-C strip under constant potential, using 1M dilute sulfuric acid aqueous solution as electrolyte, sequentially washing the electrolyte with deionized water and absolute ethyl alcohol after taking out a sample, and then drying the sample at room temperature in vacuum to finally obtain the nano-crystalline material with the nano-porous structure.
Example 3
Weighing pure iron, iron phosphide and iron carbide, and smelting to obtain Fe85P10C5And (3) alloy ingots. Then taking out the alloy ingot to be crushed, taking the fragments, ultrasonically cleaning the fragments by absolute ethyl alcohol, placing the fragments into a clean quartz tube, placing the fragments into a ribbon throwing machine, pumping high vacuum, and then spraying the melted liquid alloy onto a copper roller rotating at high speed to ensure that the liquid is rapidly cooled to form an amorphous ribbon instantly. The melt-spun machine needs to be drawn to 7 multiplied by 10-3Pa. The rotation speed of the copper roller needs to be controlled at 4000 revolutions per minute. The pressure difference between the quartz tube and the interior of the furnace body needs to be controlled at 0.4 Pa. To obtain Fe80P10C10A strip of crystalline alloy. Cutting into small segments, wherein the width of the strip is 8mm, and the length of the strip is 20 mm. The cut strips were put into a beaker, sonicated in absolute ethanol for 20min, then washed with absolute ethanol, and then placed in a vacuum drying oven at room temperature for 12 hours.
Preparing an electrochemical workstation and a three-electrode system, taking a calomel electrode as a reference electrode, taking a platinum net as a counter electrode, taking an alloy strip as a working electrode, carrying out electrochemical corrosion on an Fe-P-C strip under constant potential, using 0.1M dilute sulfuric acid aqueous solution as electrolyte, sequentially washing the electrolyte with deionized water and absolute ethyl alcohol, and then drying the electrolyte at room temperature in vacuum to obtain the nano-crystalline material with the nano-porous structure.
The nano-crystalline material with the nano-porous structure has a three-dimensional bicontinuous spongy nano-porous structure, the pore diameter and the ligament size are about 100 +/-10 nm, element atoms are not diffused synchronously in the dealloying process, partial amorphous and nano-crystalline are caused to appear, a short-range ordered and long-range disordered structure is formed, and the current density is 10mA/cm2The overpotential in the case of time is 120-125 mV.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (10)
1. A nano-porous Fe-P-C material is characterized by comprising the following steps:
step 1, preparing Fe-P-C alloy strip
Mixing pure Fe and Fe3P、Fe3C is prepared according to the proportion, then is melted in an argon arc furnace to form an alloy ingot, and then a melt-spun machine is used for melting the alloy ingot, spraying the alloy ingot and rapidly cooling the alloy ingot to form an alloy strip, wherein the mass percent of pure Fe is 22-64 percent, and Fe319 to 41 percent of P and Fe3The mass percent of C is 17% -37%, and the sum of the three components is 100%; the prepared Fe-P-C alloy strip has the atomic content (mol percent) of Fe of 80-90 percent, the content of P of 5-10 percent and the content of C of 5-10 percent, and the sum of the three atomic ratios is one hundred percent;
step 2, preparing the nano porous Fe-P-C material by adopting an electrochemical dealloying method
Carrying out electrochemical corrosion on the Fe-P-C alloy strip prepared in the step 1 under constant potential, taking the Fe-P-C alloy strip as a working electrode, setting the potential parameter to be-0.5V-0.1V, the corrosion time to be 600-1600s and the electrolyte to be 0.1-1M sulfuric acid aqueous solution; and after the electrochemical corrosion is finished, taking out the sample, cleaning, and drying at room temperature in vacuum to obtain the nano porous Fe-P-C material.
2. The nanoporous Fe-P-C material of claim 1, wherein in step 1, the percentage by mass of pure Fe is 30% -60%, Fe325 to 40 percent of P and Fe3The mass percent of C is 20-30%.
3. The nano-porous Fe-P-C material as claimed in claim 1, wherein in step 1, the melt spinning machine needs to pump to 1 x 10-3Pa～1×10-2Pa, the rotating speed of the copper roller needs to be controlled within 3000-4000 revolutions per minute, and the pressure difference between the quartz tube and the interior of the furnace body needs to be controlled within 0.1-0.5 Pa.
4. The nanoporous Fe-P-C material as claimed in claim 1, wherein in step 2, a calomel electrode is used as a reference electrode, a platinum mesh is used as a counter electrode, and an alloy strip is used as a working electrode for constant potential electrochemical corrosion.
5. The nano-porous Fe-P-C material as claimed in claim 1, wherein in step 2, the corrosion potential is set to-0.3V to-0.1V, the time is set to 1000-.
6. A preparation method of a nano-porous Fe-P-C material is characterized by comprising the following steps:
step 1, preparing Fe-P-C alloy strip
Mixing pure Fe and Fe3P、Fe3C is prepared according to the proportion, then is melted in an argon arc furnace to form an alloy ingot, and then a melt-spun machine is used for melting the alloy ingot, spraying the alloy ingot and rapidly cooling the alloy ingot to form an alloy strip, wherein the mass percent of pure Fe is 22-64 percent, and Fe319 to 41 percent of P and Fe3The mass percent of C is 17% -37%, and the sum of the three components is 100%;
step 2, preparing the nano porous Fe-P-C material by adopting an electrochemical dealloying method
Carrying out electrochemical corrosion on the Fe-P-C alloy strip prepared in the step 1 under constant potential, taking the Fe-P-C alloy strip as a working electrode, setting the potential parameter to be-0.5V-0.1V, the corrosion time to be 600-1600s and the electrolyte to be 0.1-1M sulfuric acid aqueous solution; and after the electrochemical corrosion is finished, taking out the sample, cleaning, and drying at room temperature in vacuum to obtain the nano porous Fe-P-C material.
7. The method for preparing a nano-porous Fe-P-C material according to claim 6, wherein in step 1, the mass percent of pure Fe is 30% -60%, and Fe325 to 40 percent of P and Fe3The mass percent of C is 20-30%.
8. The method for preparing a nano-porous Fe-P-C material as claimed in claim 6, wherein in step 1, the melt spinning machine needs to pump to 1 x 10-3Pa～1×10-2Pa, the rotating speed of the copper roller needs to be controlled within 3000-4000 revolutions per minute, and the pressure difference between the quartz tube and the interior of the furnace body needs to be controlled within 0.1-0.5 Pa.
9. The preparation method of the nano-porous Fe-P-C material as claimed in claim 6, wherein in the step 2, a calomel electrode is taken as a reference electrode, a platinum net is taken as a counter electrode, and an alloy strip is taken as a working electrode to carry out constant potential electrochemical corrosion; setting the corrosion potential at-0.3V to-0.1V, the time at 1000-1500s and the electrolyte at 0.5-1M sulfuric acid solution.
10. Use of a nanoporous Fe-P-C material according to any one of claims 1 to 5 for the electrolysis of water to produce hydrogen.
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| CN111485182A (en) * | 2020-04-07 | 2020-08-04 | 天津师范大学 | Iron-based amorphous nanocrystalline alloy prepared by using positive mixing heat among elements and preparation method and application thereof |
| CN112981442A (en) * | 2021-02-08 | 2021-06-18 | 东南大学 | FeCoMoPC amorphous alloy for alkaline full-hydrolysis and preparation method thereof |
| CN113896315A (en) * | 2021-11-11 | 2022-01-07 | 山东大学 | Application of FePC strip in degradation of methylene blue dye wastewater |
| CN115000420A (en) * | 2022-05-17 | 2022-09-02 | 一汽解放汽车有限公司 | Cathode catalytic membrane, membrane electrode, preparation methods of cathode catalytic membrane and membrane electrode, and fuel cell |
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| DONG YOUNG CHUNG等: ""Large-Scale Synthesis of Carbon-Shell-Coated FeP Nanoparticles for Robust Hydrogen Evolution Reaction Electrocatalyst"", 《J. AM. CHEM. SOC.》 * |
| JIANG, RUI 等: ""Highly efficient amorphous np-PdFePC catalyst for hydrogen evolution reaction "", 《ELECTROCHIMICA ACTA》 * |
| WANG, QIANQIAN等: ""Investigation of FePC amorphous alloys with self-renewing behaviour for highly efficient decolorization of methylene blue"", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
| XU, WENCE等: ""A highly efficient electrocatalyst based on amorphous Pd-Cu-S material for hydrogen evolution"", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
| XU, WENCE等: ""Nanoporous metal phosphide catalyst for bifunctional water splitting"", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
| 冯贺 等: ""过渡金属碳化物/B、N掺杂纳米碳的制备及其电催化性能"", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
| 郑继波 等: ""脱合金法制备Fe基纳米多孔材料及其催化性能"", 《材料导报》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111485182A (en) * | 2020-04-07 | 2020-08-04 | 天津师范大学 | Iron-based amorphous nanocrystalline alloy prepared by using positive mixing heat among elements and preparation method and application thereof |
| CN111485182B (en) * | 2020-04-07 | 2022-01-11 | 天津师范大学 | Iron-based amorphous nanocrystalline alloy prepared by using positive mixing heat among elements and preparation method and application thereof |
| CN112981442A (en) * | 2021-02-08 | 2021-06-18 | 东南大学 | FeCoMoPC amorphous alloy for alkaline full-hydrolysis and preparation method thereof |
| CN113896315A (en) * | 2021-11-11 | 2022-01-07 | 山东大学 | Application of FePC strip in degradation of methylene blue dye wastewater |
| CN115000420A (en) * | 2022-05-17 | 2022-09-02 | 一汽解放汽车有限公司 | Cathode catalytic membrane, membrane electrode, preparation methods of cathode catalytic membrane and membrane electrode, and fuel cell |
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