CN112517011B - Carbon-based nickel-iron bimetal oxygen evolution catalyst and preparation method thereof - Google Patents
Carbon-based nickel-iron bimetal oxygen evolution catalyst and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000003054 catalyst Substances 0.000 title claims abstract description 28
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 239000001301 oxygen Substances 0.000 title claims abstract description 22
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 22
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 16
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 46
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 16
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052796 boron Inorganic materials 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 150000002815 nickel Chemical class 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- 239000011812 mixed powder Substances 0.000 claims abstract description 8
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 7
- 239000005416 organic matter Substances 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 150000003839 salts Chemical class 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- 239000012298 atmosphere Substances 0.000 claims abstract description 3
- 229910000863 Ferronickel Inorganic materials 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- -1 sodium tetraphenylborate Chemical compound 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical group [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 3
- 150000002505 iron Chemical class 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical group [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 8
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000010411 electrocatalyst Substances 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 229910002588 FeOOH Inorganic materials 0.000 description 4
- 229910002640 NiOOH Inorganic materials 0.000 description 4
- 229910000510 noble metal Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- HTXDPTMKBJXEOW-UHFFFAOYSA-N iridium(IV) oxide Inorganic materials O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000002048 multi walled nanotube Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229920000557 Nafion® Polymers 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910021397 glassy carbon Inorganic materials 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910000474 mercury oxide Inorganic materials 0.000 description 1
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
-
- B01J35/61—
Abstract
The invention discloses a carbon-based nickel-iron bimetal oxygen evolution catalyst and a preparation method thereof, wherein the preparation method of the catalyst comprises the following steps: mixing the carbon nano tube and the boron-containing organic matter to obtain mixed powder, and calcining to obtain the boronated carbon nano tube; dispersing the boronized carbon nanotubes in water, adding nickel salt and ferric salt to fully impregnate the carbon nanotubes to obtain a mixed material, separating the mixed material to obtain a solid matter, and drying the solid matter to obtain precursor powder; and placing the precursor powder in an inert atmosphere for heat treatment, and naturally cooling to room temperature to obtain a target product. According to the invention, the surface of the carbon nano tube is modified by boron, the reducing capability of the surface of the carbon nano tube is reduced, the NiFeOOH cluster is successfully grown on the surface of the carbon nano tube, and the NiFeOOH cluster catalyst loaded on the carbon nano tube is obtained. And the production cost is low, and the method can be applied to industrialization.
Description
Technical Field
The invention belongs to the technical field of new chemical materials, and particularly relates to a carbon-based nickel-iron bimetal oxygen evolution catalyst and a preparation method thereof.
Background
High performance Oxygen Evolution Reaction (OER) catalysts in renewable energy technologies (e.g. electrolysis of water, metal air cells, fuel cells and CO)2Transformation, etc.) plays a crucial role. However, the complicated and slow reaction kinetics of the OER catalyst severely restrict the catalytic performance and the practical application. Therefore, it is highly desirable to develop efficient and stable OER catalysts to accelerate reaction kinetics and reduce excessive reaction overpotentials. At present, the catalyst considered as a benchmarking in the OER reaction is the noble metal RuO2、IrO2And the like. However, these noble metals are not stable due to their low natural reserves, high prices, and easy corrosion during oxidation in electrochemical processes, and these problems limit RuO2、IrO2Etc. for further use of the material. The green and cheap layered nickel-iron double metal hydroxide (NiFe-LDH) is considered to be an ideal non-noble metal-based catalyst, but the catalytic oxygen evolution performance and stability under high current density are poor, and the electrical conductivity is relatively low, and the defects are main obstacles for restricting the industrial application of the catalyst. Therefore, the preparation of clean, cheap and high-efficiency catalyst becomes the focus of research in recent years, and is also a technical problem to be solved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a carbon-based nickel-iron bimetal oxygen evolution catalyst, wherein the surface of a carbon nano tube is modified by boron, the reduction capability of the surface of the carbon nano tube is reduced, so that NiFeOOH clusters are successfully grown on the surface of the carbon nano tube, and the catalyst shows extremely high catalytic activity.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a carbon-based nickel-iron bimetal oxygen evolution catalyst comprises the following steps:
s1, weighing the carbon nano tube and the boron-containing organic matter, putting the carbon nano tube and the boron-containing organic matter into a ball mill, and uniformly mixing by ball milling to obtain mixed powder; preferably, the boron-containing organic substance is sodium tetraphenylborate; the mass ratio of the carbon nano tube to the sodium tetraphenylborate is 1: 1-1: 3, such as 1:1, 1:2 or 1: 3.
And S2, calcining the mixed powder to obtain the boronated carbon nano tube, wherein in the calcining process, the boron-containing organic matter is subjected to thermal decomposition and graphitization at high temperature to generate boron-doped graphene on the surface of the carbon nano tube, so that the surface of the carbon nano tube is subjected to B-modification. Preferably, the temperature of the calcination is 700-900 deg.C, such as 700 deg.C, 800 deg.C or 900 deg.C.
S3, dispersing the boronized carbon nanotubes in water to obtain a dispersion liquid, adding nickel salt and ferric salt into the dispersion liquid and dissolving the nickel salt and ferric salt to obtain a mixed material, performing ultrasonic treatment to completely disperse the nickel salt and ferric salt, continuously stirring, greatly improving the hydrophilicity of the boronized carbon nanotubes, performing long-time impregnation, easily adsorbing nickel iron ions in an aqueous solution on the surfaces of the carbon nanotubes through physical adsorption, performing centrifugal separation to obtain a solid substance, and drying to obtain precursor powder; the ultrasonic treatment is to utilize the cavitation of ultrasonic waves, so that the components in the mixed material can be dispersed more uniformly. Preferably, the nickel salt is nickel nitrate, and the iron salt is ferric nitrate.
S4, placing the precursor powder in an inert atmosphere for heat treatment, wherein Ni (NO) adsorbed on the surface of the carbon nano tube in the heat treatment process3)2And Fe (NO)3)3Thermally decompose to form NiOOH and FeOOH speciesThe reason why NiOOH and FeOOH species are generated but NiO and FeO species are not generated is that the surface of the B-modified carbon nanotube has a very strong oxidizing property, thereby making Ni (NO) available3)2And Fe (NO)3)3High valence NiOOH and FeOOH species are generated in one step. And finally, naturally cooling to room temperature to obtain the ferronickel-doped boronized carbon nanotube, namely the carbon-based ferronickel bimetallic oxygen evolution catalyst. Preferably, the temperature of the heat treatment is 340-400 ℃, such as 340 ℃, 360 ℃, 380 ℃ or 400 ℃; the heat treatment time is 2 h.
The invention also provides the carbon-based nickel-iron bimetal oxygen evolution catalyst prepared by the preparation method.
The invention has the beneficial effects that:
unmodified carbon nanotubes have a hydrophobic surface and a low polarity carbon backbone, which makes them prone to aggregation and poorly soluble in water. According to the invention, the boron is used for modifying the carbon nano tube, so that the characteristic of strong hydrophobicity of the carbon nano tube is changed, the modified carbon nano tube has better hydrophilicity, and the original advantages of good conductivity, huge specific surface area and the like of the carbon nano tube are kept; in addition, the surface of the carbon nano tube has oxidability due to the existence of boron, the reducing capability of the surface of the carbon nano tube is reduced, and NiOOH and FeOOH species with high oxidation states tend to be generated in the high-temperature pyrolysis process of nickel salt and iron salt, so that NiFeOOH clusters are successfully grown on the surface of the carbon nano tube to obtain the ferronickel doped boronized carbon nano tube, and the ferronickel doped boronized carbon nano tube shows extremely high catalytic activity by taking the substances as an oxygen evolution catalyst. Compared with other layered ferronickel double hydroxides (NiFe-LDH), the catalyst prepared by the method has good conductivity and large specific surface area, exposes more active sites, increases the electrocatalytic active area, and has higher oxygen evolution activity. In addition, with a noble metal catalyst RuO2、IrO2In contrast, the catalyst of the invention has low production cost and can be applied industrially.
Drawings
FIG. 1 is a HRTEM image of a carbon nanotube feedstock;
FIG. 2 is a HRTEM image of a carbon-based nickel-iron bimetallic oxygen evolution catalyst prepared in example 1;
FIG. 3 is a LSV plot of OER performance tests for various samples.
Detailed Description
The present invention will be further described with reference to the following examples and the accompanying drawings. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The reagents and raw materials used in the present example are all commercially available products.
Example 1
S1, weighing the commercial multi-walled carbon nano-tube and the sodium tetraphenylborate according to the mass ratio of 1:2, and uniformly mixing by ball milling to obtain mixed powder.
S2, placing the mixed powder in a ceramic square boat, heating the mixed powder from room temperature to 800 ℃ at a heating rate of 10 ℃ per minute in an argon atmosphere, and keeping the temperature for 4 hours to obtain the boronated carbon nano tube.
S3, dispersing 10mg of boronized carbon nanotubes in 5mL of water, and adding 40 wt% of Ni (NO) based on the mass of the carbon nanotubes3)2·6H2O and 25 wt% Fe (NO)3)3·9H2And O. Ultrasonically dispersing the mixture completely, continuously stirring for 12h, and centrifugally separating the mixture to obtain Ni dipped on the surface2+And Fe3+Drying the carbon nano tube to obtain the precursor powder of the boronized carbon nano tube for absorbing the nickel iron.
S4, heating the precursor powder in the step 3 from room temperature to 380 ℃ at a heating rate of 10 ℃ per minute in a tube furnace in an argon atmosphere, preserving heat for 2h, and then naturally cooling to room temperature to obtain the ferronickel-doped boronized carbon nanotube, namely the carbon-based ferronickel bimetallic oxygen evolution catalyst, which is marked as NiFe-B and CNT.
Fig. 1 is an electron microscope image of a raw material multi-walled carbon nanotube used, fig. 2 is an electron microscope image of a carbon-based nickel-iron bimetallic oxygen evolution catalyst prepared in example 1, and it is apparent from a comparison between fig. 1 and fig. 2 that nifeoh clusters are visible in fig. 2.
Comparative example 1
Comparative example 1 differs from example 1 only in that Fe (NO) was not added in step S33)3·9H2O, the other processes were the same as in example 1, and the product obtained was Ni-B, CNT.
Comparative example 2
Comparative example 1 differs from example 1 only in that Ni (NO) is not added in step S33)2·6H2O, the other processes were the same as in example 1, and Fe-B, CNT, was prepared.
For the products obtained in example 1, comparative example 1 and comparative example 2 and RuO2OER performance tests were performed, all on a CHI 760E electrochemical workstation equipped with a typical three electrode system, and the electrocatalyst was tested for oxygen evolution performance in a 1M potassium hydroxide solution in electrolyte. Wherein, a carbon rod is used as a counter electrode, a mercury oxide electrode is used as a reference electrode, 5mg of the prepared electrocatalyst powder is weighed, and 1mL of H is added2Mixed solution of O and ethanol (V)H2O：VEthanol2) fully performing ultrasonic treatment, adding 30ul of nafion solution, performing ultrasonic treatment for 30min, and dripping 5ul to 3mm of glassy carbon electrode by using a micro liquid transfer gun to dry the electrode to be used as a working electrode. The test piece was subjected to a linear voltammetric sweep test at a sweep rate of 10 mV/s.
FIG. 3 is a graph of the OER performance test CV for various samples, as can be seen in FIG. 3: when the current density is 10mA/cm2The overpotential of the nickel iron doped boronized carbon nanotube oxygen evolution electrocatalyst prepared in example 1 was as low as 189mV, the overpotential of the Ni doped boronized carbon nanotube electrocatalyst prepared in comparative example 1 was 222mV, and the overpotential of the Fe doped boronized carbon nanotube electrocatalyst prepared in comparative example 2 was 231 mV. Overpotential average ratio RuO2Therefore, the nickel-iron doped carbon-based nano oxygen evolution electrocatalyst is successfully prepared by the method and has excellent catalytic activity of oxygen evolution reaction. Especially NiFe-B, CNT, is one of the most active materials at present.
Claims (8)
1. A preparation method of a carbon-based nickel-iron bimetal oxygen evolution catalyst is characterized by comprising the following steps: the method comprises the following steps:
s1, uniformly mixing the carbon nano tube and the boron-containing organic matter to obtain mixed powder;
s2, calcining the mixed powder to obtain boronated carbon nanotubes;
s3, dispersing the boronized carbon nanotubes in water to obtain a dispersion liquid, adding nickel salt and ferric salt into the dispersion liquid, dissolving the nickel salt and ferric salt to obtain a mixed material, stirring to fully impregnate the boronized carbon nanotubes, then performing centrifugal separation to obtain a solid matter, and drying to obtain precursor powder;
s4, placing the precursor powder in an inert atmosphere for heat treatment, and then naturally cooling to room temperature to obtain the ferronickel-doped boronized carbon nanotube, namely the carbon-based ferronickel bimetallic oxygen evolution catalyst.
2. The method of claim 1, wherein: in step S1, the mass ratio of the carbon nano tube to the boron-containing organic matter is 1: 1-1: 3; the mode of mixing evenly is ball milling treatment.
3. The method of claim 2, wherein: the organic matter containing boron is sodium tetraphenylborate.
4. The method of claim 1, wherein: in step S2, the temperature of the calcination is 700-900 ℃.
5. The method of claim 1, wherein: in step S3, the nickel salt is nickel nitrate, and the iron salt is ferric nitrate.
6. The method of claim 1, wherein: in step S3, the mixture is subjected to ultrasonic dispersion and then stirred.
7. The method of claim 1, wherein: in step S4, the temperature of the heat treatment is 340-400 ℃.
8. A carbon-based nickel-iron bimetallic oxygen evolution catalyst prepared by the preparation method of any one of claims 1 to 7.
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