CN113235076B - Preparation method and application of phosphorus-doped passivated foamed nickel - Google Patents

Preparation method and application of phosphorus-doped passivated foamed nickel Download PDF

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CN113235076B
CN113235076B CN202110206891.6A CN202110206891A CN113235076B CN 113235076 B CN113235076 B CN 113235076B CN 202110206891 A CN202110206891 A CN 202110206891A CN 113235076 B CN113235076 B CN 113235076B
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foamed nickel
phosphorus
passivated
nickel
doped
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CN113235076A (en
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叶宝华
张海波
薛洪
范鹏元
姜礼
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Dongguan Pulom Electronic Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/07—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/78—Pretreatment of the material to be coated
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/82—After-treatment
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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Abstract

The invention provides a preparation method and application of phosphorus-doped passivated foamed nickel, and relates to the fields of hydrogen energy and electrochemistry. The preparation method of the phosphorus-doped passivated foamed nickel mainly comprises the following steps: cleaning, passivating, treating mixed solution of sodium hypophosphite and hydrogen peroxide, passivating in a tubular furnace and the like. The invention overcomes the defects of the prior art, and the prepared phosphorus-doped passivated foamed nickel serving as a catalytic material has excellent electro-catalytic hydrogen evolution performance and initial potential (namely the current density is-1 mA-cm)‑2Potential of time) is shifted by 52mV positively compared with the original foam nickel and at a high current density (-100mA cm)‑2) When the nickel foam is used, the hydrogen evolution overpotential is 420mV, which is shifted to 172mV compared with the original nickel foam.

Description

Preparation method and application of phosphorus-doped passivated foamed nickel
Technical Field
The invention relates to the technical field of hydrogen energy and electrochemistry, in particular to a preparation method and application of phosphorus-doped passivated foamed nickel.
Background
Global environmental pollution and energy crisis have prompted the rapid research on renewable energy sources. Hydrogen energy is widely favored because of its cleanliness, environmental friendliness, and high combustion value. Currently, a green process for hydrogen production is electrocatalytic water splitting. However, the large overpotential of the electrode surface makes it necessary to find a catalyst having low cost and high performance. Especially for the alkaline hydrogen release reaction (HER), it involves an additional process of water dissociation.
Recently, great efforts have been made to develop non-noble metal based catalysts, including transition metal sulfides, phosphates, carbides, alloys and many other non-metallic compounds. Among these, metal phosphates, in particular bimetallic phosphates, are known for their high intrinsic activity (e.g. CoP, Ni)2P) and exhibit excellent HER performance in alkaline media. The patent No. 202010556343.1 discloses "a preparation method and application of a foam nickel loaded amorphous phosphorus-doped nickel molybdate bifunctional electrocatalytic electrode", which uses foam nickel loaded amorphous phosphorus-doped nickel molybdate to realize the catalytic action of electrolytic hydrogen production, but the process of electrolytic hydrogen production usually requires urea assistance, and it can be seen from the relevant examples of the patent that the range of its use is mostly small current density (a)<100mA·cm-2) And is not suitable for actual large-scale industrial production.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method and application of phosphorus-doped passivated foamed nickel, and the preparation process of the phosphorus-doped passivated foamed nickel is low in cost, simple in process and environment-friendly, so that the phosphorus-doped passivated foamed nickel can be subjected to electrocatalytic hydrogen evolution in an alkaline solution and at a low voltage, and has a good industrial application value.
In order to achieve the above purpose, the technical scheme of the invention is realized by the following technical scheme:
a preparation method of phosphorus-doped passivated foamed nickel comprises the following steps:
(1) cleaning foamed nickel: sequentially placing foamed nickel in acetone, acid liquor, distilled water and ethanol for treating for 10min, and removing surface grease and metal oxide;
(2) and (3) drying the foamed nickel: putting the foamed nickel obtained in the step (1) into an oven for drying treatment to obtain dried foamed nickel for later use;
(3) putting the foam nickel dried in the step (2) into a muffle furnace for passivation treatment to obtain passivated foam nickel for later use;
(4) dissolving sodium hypophosphite in deionized water, magnetically stirring for 5-20min until the sodium hypophosphite is dissolved to obtain a sodium hypophosphite solution, adding hydrogen peroxide, and uniformly stirring to obtain a solution A for later use;
(5) adding the passivated foamed nickel in the step (3) into the solution A, standing for reaction for a period of time to obtain a phosphorus-doped passivated foamed nickel precursor for later use;
(6) and (4) putting the phosphorus-doped passivated foamed nickel precursor in the step (5) into a tubular furnace, and reacting in an argon atmosphere to obtain the phosphorus-doped passivated foamed nickel compound.
Preferably, the specification of the foamed nickel in the step (1) is 20X 30X 1 mm; the acid solution is hydrochloric acid aqueous solution with concentration of 3 mol/L.
Preferably, the drying temperature of the foamed nickel in the step (2) is 60 ℃, and the drying time is 3 h.
Preferably, the passivation process of the nickel foam in the step (3) is to heat up to 500 ℃ at a heating rate of 3 ℃/min and then to preserve heat for 3 h.
Preferably, the concentration of the sodium hypophosphite solution prepared in the step (4) is 5mol/L, and the amount of hydrogen peroxide is 2 ml.
Preferably, the reaction condition in the step (5) is that the temperature is raised to 500 ℃ at the temperature raising rate of 2 ℃/min, and then the temperature is maintained for 3 h.
Preferably, the phosphorus-doped passivated foamed nickel is applied as an electrocatalytic hydrogen evolution electrode material.
The invention provides a preparation method and application of phosphorus-doped passivated foamed nickel, which have the following advantages compared with the prior art:
the phosphorus-doped passivated foamed nickel provided by the invention has a three-dimensional structure, is firm in structure, has corrosion resistance and bears large current (more than 100 mA-cm)-2) The use of a binder is avoided, so that the impedance of an electrolytic system is reduced and the overall efficiency is improved, and phosphorus (P) doping can effectively change the electronic structure, improve the polarity, catalytic activity and stability of metal compounds, so that the method has great potential in industrial application.
Description of the drawings:
FIG. 1 is an X-ray powder diffraction pattern (XRD) of example 1(60-NF), example 2(500-NF), example 3(60-NF/P) and example 4 (500-NF/P);
FIG. 2 is a Scanning Electron Micrograph (SEM) and an X-ray energy spectrum analysis (EDS) of example 1; (wherein a in FIG. 2 is SEM picture, b is EDS picture)
FIG. 3 is a Scanning Electron Micrograph (SEM) and an X-ray energy spectrum analysis (EDS) of example 2; (wherein a in FIG. 3 is SEM picture, b is EDS picture);
FIG. 4 is a Scanning Electron Micrograph (SEM) and an X-ray energy spectrum analysis (EDS) of example 3; (wherein in FIG. 4, a is SEM picture and b is EDS picture)
FIG. 5 is a Scanning Electron Micrograph (SEM) and an X-ray energy spectrum analysis (EDS) of example 4; (wherein in FIG. 5, a is SEM picture and b is EDS picture)
FIG. 6 is a graph of the hydrogen evolution Linear Scan (LSV) for examples 1-4.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention.
Example 1:
preparation of non-passivated and non-phosphorus-doped foamed Nickel (60-NF)
(1) Sequentially placing 20X 30X 1mm foamed nickel in acetone, 3mol/L hydrochloric acid aqueous solution, distilled water and ethanol for treatment for 10min to remove surface grease and metal oxide;
(2) putting the foamed nickel obtained in the step (1) into a drying oven, and drying for 6 hours at the temperature of 60 ℃;
60-NF was obtained.
Example 2:
preparation of passivated and non-phosphorus doped foamed Nickel (500-NF)
(1) Sequentially placing 20X 30X 1mm foamed nickel in acetone, 3mol/L hydrochloric acid aqueous solution, distilled water and ethanol for treatment for 10min to remove surface grease and metal oxide;
(2) putting the foamed nickel in the step (1) into an oven, and drying for 3h at the temperature of 60 ℃;
(3) putting the foamed nickel in the step (2) into a muffle furnace, heating to 500 ℃ at a heating rate of 3 ℃/min, and then preserving heat and passivating for 3 h;
500-NF is obtained.
Example 3:
preparation of non-passivated and phosphorus-doped foamed nickel (60-NF/P)
(1) Sequentially placing 20X 30X 1mm foamed nickel in acetone, 3mol/L hydrochloric acid aqueous solution, distilled water and ethanol for treatment for 10min to remove surface grease and metal oxide;
(2) putting the foamed nickel in the step (1) into an oven, and drying for 3h at the temperature of 60 ℃;
(3) adding 2mL of hydrogen peroxide into 5mol/L sodium hypophosphite solution, uniformly mixing, adding the foamed nickel obtained in the step (2), and reacting for 12 hours;
(4) putting the foamed nickel in the step (2) into a muffle furnace, heating to 500 ℃ at a heating rate of 3 ℃/min, and then preserving heat and passivating for 3 h;
60-NF/P was obtained.
Example 4
Preparation of passivated and phosphorus-doped foamed Nickel (500-NF/P)
(1) Sequentially placing 20X 30X 1mm foamed nickel in acetone, 3mol/L hydrochloric acid aqueous solution, distilled water and ethanol for treatment for 10min to remove surface grease and metal oxide;
(2) putting the foamed nickel in the step (1) into an oven, and drying for 3h at the temperature of 60 ℃;
(3) putting the foamed nickel in the step (2) into a muffle furnace, heating to 500 ℃ at a heating rate of 3 ℃/min, and then preserving heat and passivating for 3 h;
(4) adding 2mL of hydrogen peroxide into 5mol/L sodium hypophosphite solution, uniformly mixing, adding the foamed nickel obtained in the step (3), and reacting for 12 hours;
(5) taking out the foamed nickel in the step (4), placing the foamed nickel in a tubular furnace in an argon atmosphere, heating to 350 ℃ at the heating rate of 2 ℃/min, then preserving heat for 3 hours, and cooling along with the furnace;
500-NF/P is obtained.
Detection 1:
combining the above examples 1-4:
(1) x-ray powder diffraction analysis is carried out on 500-NF/P, 60-NF, 500-NF and 60-NF/P, as shown in figure 1, wherein the peak value of 500-NF/P corresponds to JCPDS 04-0850 and 18-0883, and is the peak value of foam nickel and nickel phosphide, which indicates that the new phase is synthesized by successfully doping phosphorus; the peak value of 60-NF corresponds to JCPDS 04-0850 and is the peak of foam nickel; 500-NF corresponds to JCPDS 04-0850 and is the peak of foam nickel; 60-NF/P corresponds to JCPDS 04-0850 and JCPDS 18-0883, and is the peak of foam nickel and nickel phosphide, which indicates that the new phase is successfully synthesized by doping phosphorus;
(2) for 500-NF/P, 60-NF, 500-NF, 60-NF/P electron microscope and X-ray energy spectrum analysis: wherein 500-NF/P is shown as a and b in FIG. 5, the 500-NF/P surface has a large amount of nano-particles and nano-sheets, which shows that phosphorus is successfully doped and a new phase is formed, and elemental analysis contains phosphorus element; the 60-NF is shown as a and b in figure 2, the 60-NF surface is relatively smooth and has no etching trace, which shows that the surface is cleaned and the elemental analysis is single and has no other metal oxide; 500-NF is shown as a and b in FIG. 3, the 500-NF surface has a large number of holes and etching traces, which shows that the passivation is successful and the elemental analysis is single and no other metal oxide exists; 60-NF/P As shown in a and b in FIG. 4, the surface of 60-NF/P has a large amount of nano-particles and nano-sheets, which shows that phosphorus is successfully doped and a new phase is formed, and the elemental analysis contains phosphorus element.
And (3) detection 2:
the materials prepared in the above examples 1 to 4 were subjected to an electrochemical HER performance test using an electrochemical workstation of the type shanghai chen CHI-760E.
In a 1mol/L KOH solution, Ag/AgCl is used as a reference electrode, a carbon rod is used as a counter electrode, and the materials in example 1 and comparative examples 1 to 3 are used as working electrodes. Polarization curves of HER as shown in fig. 6, the HER performance of the catalytic material is ranked in the following order: 500-NF/P is more than 60-NF/P is more than 500-NF is more than 60-NF.
Specifically, catalytic materials (500-NF/P, 60-NF/P,500-NF and 60-NF) at an initial potential (i.e., a current density of-1 mA cm-2Potential of (ii) 26mV, 30mV, 50mV and 78mV, respectively; and under the condition of large current density (-100mA cm)-2) The overpotentials of (1) are 420mV, 442mV, 529mV and 592mV, respectively.
In conclusion, the material in example 4 of the present application is excellent in hydrogen evolution performance.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (4)

1. The preparation method of the phosphorus-doped passivated foamed nickel is characterized by comprising the following steps of:
(1) cleaning foamed nickel: sequentially placing the foamed nickel in acetone, acid liquor, distilled water and ethanol for treatment for 10min, and removing surface grease and metal oxide;
(2) and (3) drying the foamed nickel: putting the foamed nickel obtained in the step (1) into an oven for drying treatment to obtain dried foamed nickel for later use;
(3) putting the dried foam nickel in the step (2) into a muffle furnace for passivation treatment, wherein the passivation process is to heat the foam nickel to 500 ℃ at a heating rate of 3 ℃/min and then keep the temperature for 3h to obtain passivated foam nickel for later use;
(4) dissolving sodium hypophosphite in deionized water, magnetically stirring for 5-20min to obtain a sodium hypophosphite solution with the concentration of 5mol/L, adding 2ml of hydrogen peroxide, and uniformly stirring to obtain a solution A for later use;
(5) adding the passivated foamed nickel in the step (3) into the solution A, heating to 500 ℃ at the heating rate of 2 ℃/min, keeping the temperature, standing and reacting for 3 hours to obtain a phosphorus-doped passivated foamed nickel precursor for later use;
(6) and (4) putting the phosphorus-doped passivated foamed nickel precursor in the step (5) into a tubular furnace, and reacting in an argon atmosphere to obtain a phosphorus-doped passivated foamed nickel compound.
2. The method for preparing the phosphorus-doped passivated foamed nickel according to claim 1, characterized by comprising the following steps: the specification of the foamed nickel in the step (1) is 20 multiplied by 30 multiplied by 1 mm; the acid solution is hydrochloric acid aqueous solution with concentration of 3 mol/L.
3. The method for preparing the phosphorus-doped passivated foamed nickel according to claim 1, characterized in that: in the step (2), the drying temperature of the foamed nickel is 60 ℃, and the drying time is 3 hours.
4. A passivated phosphorus-doped foamed nickel obtained by the method of claim 1, wherein the passivated phosphorus-doped foamed nickel is used as an electrocatalytic hydrogen evolution electrode material.
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CN114457345B (en) * 2022-02-23 2024-03-22 南通大学 Nitrogen-doped and phosphorylation-combined modified electrode and preparation method thereof
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CN110354875A (en) * 2019-05-24 2019-10-22 深圳欧赛技术有限公司 It is supported on Co (OH) F and its preparation method and application of foam nickel surface yttrium phosphor codoping

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