CN110898838A - Preparation method and application for synthesizing Ni-doped FeOOH/NF by millisecond laser direct writing technology - Google Patents
Preparation method and application for synthesizing Ni-doped FeOOH/NF by millisecond laser direct writing technology Download PDFInfo
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- 229910002588 FeOOH Inorganic materials 0.000 title claims abstract description 26
- 238000005516 engineering process Methods 0.000 title claims abstract description 8
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 230000002194 synthesizing effect Effects 0.000 title claims description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 70
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 31
- 239000006260 foam Substances 0.000 claims abstract description 15
- 239000012266 salt solution Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 150000002505 iron Chemical class 0.000 claims abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000001301 oxygen Substances 0.000 claims abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- 239000011521 glass Substances 0.000 claims description 7
- 238000013519 translation Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 6
- 230000009471 action Effects 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 230000001678 irradiating effect Effects 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- -1 iron ions Chemical class 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 9
- 230000015572 biosynthetic process Effects 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000001308 synthesis method Methods 0.000 abstract description 2
- 231100000331 toxic Toxicity 0.000 abstract description 2
- 230000002588 toxic effect Effects 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000010411 electrocatalyst Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000007630 basic procedure Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000002277 temperature effect Effects 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 229910002555 FeNi Inorganic materials 0.000 description 1
- 229910000863 Ferronickel Inorganic materials 0.000 description 1
- 229910021577 Iron(II) chloride Inorganic materials 0.000 description 1
- 229910002640 NiOOH Inorganic materials 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910001447 ferric ion Inorganic materials 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 238000001075 voltammogram Methods 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
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Abstract
本申请涉及毫秒激光直写技术合成Ni掺杂FeOOH/NF的制备方法及应用。本申请利用毫秒激光器辐照铁盐溶液中的泡沫镍，制备具有三维结构的Ni掺杂FeOOH及其在氧析出反应中的应用，利用其丰富的缺陷位点和边缘镍掺杂带来的高活性位点以及良好的导电率来提升氧析出反应(OER)催化性能。本申请所采用的合成方法工艺简单、操作方便、易于控制，且未使用有毒反应原料，是一种环境友好的绿色合成工艺。
The present application relates to a preparation method and application of Ni-doped FeOOH/NF synthesized by millisecond laser direct writing technology. This application utilizes millisecond laser irradiation to irradiate nickel foam in iron salt solution to prepare Ni-doped FeOOH with three-dimensional structure and its application in oxygen evolution reaction. Active sites and good electrical conductivity can improve the catalytic performance of oxygen evolution reaction (OER). The synthesis method adopted in the present application is simple in process, convenient in operation, easy to control, and does not use toxic reaction raw materials, and is an environment-friendly green synthesis process.
Description
Technical Field
The invention relates to a method for preparing Ni-doped FeOOH with a three-dimensional structure by irradiating foamed nickel in an iron salt solution with a millisecond laser and application of the Ni-doped FeOOH in an oxygen precipitation reaction.
Background
Currently, environmental energy shortage and environmental crisis are becoming more serious, and the search for clean energy to replace fossil fuel is urgent. The electrolysis of water to produce hydrogen and oxygen is currently the most promising and effective way to obtain renewable hydrogen energy. However, the OER reaction involved in the electrolysis of water involves complex multiple proton coupling and multiple electron transfer processes, so that a higher overpotential is required to drive the reaction, and therefore, the development of hydrogen production by electrolysis of water is severely restricted by the higher water oxidation overpotential, and the search for efficient OER electrocatalysts becomes a research focus at home and abroad.
Research has now found that ferronickel bimetallic hydroxide is the most excellent non-noble metal OER electrocatalyst. As early as 80 s in the last century, Corrigan et al found that nickel oxide containing iron impurities as a catalyst had a great influence on the OER reaction, and that even 0.01% of iron could significantly reduce the OER overpotential and improve the activity of the catalyst. See: corrigan, D.A. journal of The Electrochemical Society,134(2),377-384. since then, a great deal of work has been done to investigate The catalytic mechanism of FeNi oxides/hydroxides for OER. The Bell topic group uses in-situ Raman spectrum characterization to find that Fe is in Ni (OH)2Is an active center, when the content of Fe exceeds 11%, the Fe-rich phase starts to separate from Ni, and proper amount of Fe doping produces good OER activity and low overpotential, which is related to the adsorption energy of intermediate products of OER on the surface of Fe sites. See: friebel, D, et al, journal of the American Chemical Society 137.3(2015):1305-2And relatively little research is done on Ni doped FeOOH. This is because in the synthesis process, the Ni-doped FeOOH phase is unstable and forms the Fe-doped NiOOH phase more easily, so the OER performance of the Ni-doped FeOOH phase is also rarely reported. In summary, we imagine the synthesis of Ni-doped FeOOH electrocatalyst with the transient high temperature action of millisecond laser and explore its OER performance.
Disclosure of Invention
The invention aims to solve the problem that the existing synthesis process can not effectively synthesize the Ni-doped FeOOH electrocatalyst with high OER catalytic activity, and the millisecond laser direct writing technology can be used for synthesizing a stable target catalyst, causing more defects in the catalyst and forming edge Ni doping so as to improve the OER performance.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method for synthesizing Ni-doped FeOOH/NF by utilizing a millisecond laser direct writing technology comprises the following steps:
(1) preparing 50mL of hydrochloric acid solution with the concentration of 3 mol/L: measuring 12.99mL of hydrochloric acid with the concentration of 36% in a 100mL beaker by using a measuring cylinder, adding 37.01mL of deionized water, and uniformly stirring by using a glass rod;
(2) taking a piece of foam nickel with the thickness of 2cm by 2cm, soaking the foam nickel in the solution prepared in the step (1) for a set time, taking out the foam nickel, then washing the foam nickel with deionized water for five times, and washing off hydrochloric acid on the surface;
(3) preparing 30mL of FeCl with the concentration of 0.036mol/L2·4H2O or FeCl3·6H2Solution O: 214.6mgFeCl was weighed2·4H2O or 291.7mgFeCl3·6H2Dissolving O in 30mL of deionized water, and stirring with a glass rod until the powder is completely dissolved to obtain an iron salt solution;
(4) placing the foamed nickel obtained in the step (2) into the ferric salt solution prepared in the step (3) to form a sample;
(5) and (3) placing the sample obtained in the step (4) on an electric translation table, irradiating the sample by millisecond laser, taking the translation table at the moving speed of 0.2mm/s, finally taking the foamed nickel subjected to the laser action out of the iron salt solution, washing the foamed nickel for 5 times by deionized water, and washing off iron ions on the surface of the sample to obtain the Ni-doped FeOOH/NF with the three-dimensional structure.
And (3) soaking the foamed nickel in the solution prepared in the step (1) for 30min in the step (2) and taking out.
In the step (5), the energy of the millisecond laser is 1.7J, 3.6J or 5.5J, the wavelength is 1064nm, the repetition frequency of the laser is 1Hz, and the total time of acting on the sample is 1 h.
The Ni-doped FeOOH/NF with the three-dimensional structure prepared by the method is applied to oxygen precipitation reaction.
The invention uses millisecond laser to irradiate the foam nickel soaked in the ferric salt solution, and uses the instant high temperature effect generated by a millisecond laser to induce the formation of FeOOH phase on the foam nickel, and simultaneously, because the instant high temperature inducing effect can form a plurality of edge defects and form edge doping of Ni, the edge doping improves the OER catalytic performance of the material together.
The invention provides a controllable large-scale preparation method of a Ni edge-doped FeOOH material, and realizes high-efficiency OER catalytic activity. In addition, the synthesis method adopted by the invention has the advantages of simple process, convenient operation and easy control, does not use toxic reaction raw materials, and is an environment-friendly green synthesis process.
Drawings
FIG. 1 is a diagram of a process apparatus for irradiating foamed nickel immersed in a ferric salt solution with millisecond laser, wherein the process apparatus comprises a 1-laser, a 2-reflector, a 3-beaker, a 4-solution containing ferric ions, a 5-foamed nickel, and a 6-electric translation stage.
FIG. 2 is a representation of Ni-doped FeOOH/NF in which (a) (b) is a scanning electron map; (c) a transmission electron map; (d) an XRD spectrum; (e) - (h) EDS-MAPPING diagram.
FIG. 3: (a) different salt solutions (FeCl)2、FeCl3Versus water) versus OER performance; (b) using FeCl2Saline solution, effect of different laser energies on OER performance is plotted versus time.
FIG. 4 is a graph of the OER stability test of Ni doped FeOOH/NF, wherein (a) the stability i-t curve; (b) linear voltammograms.
Detailed Description
Example 1
(1) Preparing 50mL of hydrochloric acid solution with the concentration of 3 mol/L: measuring 12.99mL of hydrochloric acid with the concentration of 36% in a 100mL beaker by using a measuring cylinder, adding 37.01mL of deionized water, and uniformly stirring by using a glass rod;
(2) taking a piece of foam nickel with the thickness of 2cm by 2cm, soaking the foam nickel in the solution prepared in the step (1) for 30min, taking out the foam nickel, then washing the foam nickel with deionized water for five times, and washing off hydrochloric acid on the surface;
(3) preparing 30mL of FeCl with the concentration of 0.036mol/L2·4H2Solution O: 214.6mgFeCl was weighed2·4H2Dissolving O in 30mL of deionized water, and stirring with a glass rod until the powder is completely dissolved to obtain an iron salt solution;
(4) placing the foamed nickel obtained in the step (2) into the ferric salt solution prepared in the step (3) to form a sample;
(5) and (3) placing the sample obtained in the step (4) on an electric translation table, then irradiating the sample by using millisecond laser, taking the foamed nickel subjected to the laser action out of the iron salt solution, washing the foamed nickel with deionized water for 5 times to wash away iron ions on the surface of the sample, and obtaining the Ni-doped FeOOH/NF with a three-dimensional structure, wherein the moving speed of the translation table is 0.2mm/s, the energy of the millisecond laser is 3.6J, and the action time is 1 h.
Example 2
The basic procedure was the same as in example 1, except that in step (3), 30mL of FeCl was prepared at a concentration of 0.036mol/L3·6H2Solution O: 291.7mg of FeCl was weighed3·6H2O was dissolved in 30mL of deionized water and stirred with a glass rod until the powder was completely dissolved.
Example 3
The basic procedure was the same as in example 1, except that in step (5), the energy of the millisecond laser was 1.7J.
Example 4
The basic procedure was the same as in example 1, except that in step (5), the energy of the millisecond laser was 5.5J.
Compared with the prior art, the method utilizes the millisecond laser to irradiate the foamed nickel soaked in the ferric salt solution, utilizes the instantaneous high temperature effect generated by the millisecond laser to induce the formation of FeOOH phase on the foamed nickel, and simultaneously can form a plurality of edge defects and form edge doping of Ni due to the instantaneous high temperature induction effect, so that the OER catalytic performance of the material is improved.
Claims (4)
1. A preparation method for synthesizing Ni-doped FeOOH/NF by utilizing a millisecond laser direct writing technology is characterized by comprising the following steps of:
(1) preparing 50mL of hydrochloric acid solution with the concentration of 3 mol/L: measuring 12.99mL of hydrochloric acid with the concentration of 36% in a 100mL beaker by using a measuring cylinder, adding 37.01mL of deionized water, and uniformly stirring by using a glass rod;
(2) taking a piece of foam nickel with the thickness of 2cm by 2cm, soaking the foam nickel in the solution prepared in the step (1) for a set time, taking out the foam nickel, then washing the foam nickel with deionized water for five times, and washing off hydrochloric acid on the surface;
(3) preparing 30mL of FeCl with the concentration of 0.036mol/L2■4H2O or FeCl3■6H2Solution O: 214.6mgFeCl was weighed2■4H2O or 291.7mgFeCl3■6H2Dissolving O in 30mL of deionized water, and stirring with a glass rod until the powder is completely dissolved to obtain an iron salt solution;
(4) placing the foamed nickel obtained in the step (2) into the ferric salt solution obtained in the step (3) to form a sample;
(5) and (3) placing the sample obtained in the step (4) on an electric translation table, irradiating the sample by millisecond laser, taking the translation table at the moving speed of 0.2mm/s, finally taking the foamed nickel subjected to the laser action out of the iron salt solution, washing the foamed nickel for 5 times by deionized water, and washing off iron ions on the surface of the sample to obtain the Ni-doped FeOOH/NF with the three-dimensional structure.
2. The preparation method for synthesizing Ni-doped FeOOH/NF by the millisecond laser direct writing technology according to claim 1, wherein in the step (2), the foamed nickel is soaked in the solution prepared in the step (1) for 30min and then taken out.
3. The preparation method for synthesizing Ni-doped FeOOH/NF according to the millisecond laser direct writing technology of claim 1, wherein the energy of the millisecond laser in the step (5) is 1.7J, 3.6J or 5.5J, the wavelength is 1064nm, the repetition frequency of the laser is 1Hz, and the total time of acting on the sample is 1 h.
4. The application of the Ni-doped FeOOH/NF with the three-dimensional structure prepared by the method of claim 1 is characterized in that the Ni-doped FeOOH/NF with the three-dimensional structure is applied to oxygen evolution reaction.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112080760A (en) * | 2020-09-15 | 2020-12-15 | 中南大学 | A kind of graphene oxide doped nickel oxide layer/nickel matrix composite material and preparation method thereof and application of hydrogen evolution electrode |
| CN113913858A (en) * | 2021-10-25 | 2022-01-11 | 天津大学 | Preparation method for preparing catalytic electrode rich in crystal defects by liquid nitrogen environment pulse laser direct writing |
| CN114277400A (en) * | 2021-12-06 | 2022-04-05 | 江苏大学 | A kind of self-etching preparation method of nickel-doped iron oxyhydroxide self-supporting electrode material and its application |
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