CN113860390B - Co 2 (OH) 3 Cl microspheres and Fe 2+ Doped Co 2 (OH) 3 Cl preparation method - Google Patents
Co 2 (OH) 3 Cl microspheres and Fe 2+ Doped Co 2 (OH) 3 Cl preparation method Download PDFInfo
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- CN113860390B CN113860390B CN202010624486.1A CN202010624486A CN113860390B CN 113860390 B CN113860390 B CN 113860390B CN 202010624486 A CN202010624486 A CN 202010624486A CN 113860390 B CN113860390 B CN 113860390B
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- C01G51/085—Chlorides
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- C01P2002/00—Crystal-structural characteristics
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- C01P2002/54—Solid solutions containing elements as dopants one element only
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P2004/32—Spheres
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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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 patent name of the invention is: "Co 2 (OH) 3 Cl microspheres and Fe 2+ Doped Co 2 (OH) 3 Preparation of Cl ", belonging to the field: and (3) preparing an electrocatalyst. Weighing appropriate amount of Co (NO) 3 ) 2 ·6H 2 O, sodium hexadecyl benzene sulfonate and NaCl are dissolved in glycol and transferred into an autoclave with polytetrafluoroethylene as a lining, and the autoclave is placed in a baking oven at 90 ℃ for 6 hours, heated to 180 ℃ and kept for 2 hours. The obtained sample is filtered, washed and dried to obtain Co 2 (OH) 3 Cl microspheres. According to X% Fe-Co 2 (OH) 3 Molar ratio of Cl (x=5, 10, 15 and 20) and the same method as described above were used to prepare different Fe 2+ Doping amount of Co 2 (OH) 3 Cl microspheres. These materials are very good anode catalysts for alkaline electrolyzed water, and all have performance exceeding commercial RuO 2 Has good application prospect. The present invention discloses the material and its preparation process.
Description
Technical Field
The invention relates to basic cobalt chloride microspheres and Fe 2+ And preparing the doped basic cobalt chloride microspheres. Specifically, the method adopts a soft template-solvothermal method to prepare cobalt basic chloride and Fe 2+ Doped basic cobalt chloride microspheres.
Background
Co 2 (OH) 3 Cl is Co (OH) 2 And CoCl 2 Is a solid solution of (a). Co (Co) 2 (OH) 3 Cl is a compound which is simultaneously doped with Cl - And OH (OH) - The cobalt-based composite of groups exhibits an octahedral-like structure with a space group R3m consisting of slightly distorted corner tetrahedra thereof. In recent years, co 2 (OH) 3 Cl and its derivatives can be used as efficient negative electrode materials in lithium ion batteries and exhibit excellent electrochemical properties, while also being applicable to battery-supercapacitors due to the presence of chloride ions [ see: (a) Yin L W2015 J.Mater. Chem. A3 17659. (b) Shao G J2019 Materials Letters 237 344. (C) Yang C H2019 Journal of Alloys and Compounds 811 151905.]. However, co 2 (OH) 3 Cl has not been studied in detail in other leading edge fields, such as electrocatalysis. Recently, co with pyrochlore-like crystal structure has been proposed 2 (OH) 3 The rapid synthesis of Cl is of increasing interest. Current preparation of Co 2 (OH) 3 Cl processes generally require extreme environments or special reactants. For example, coCl 2 Mixing ethanol solution with propylene oxide to form gel, drying, calcining at 200deg.C for 6 hr to obtain Co 2 (OH) 3 Cl xerogel. Graphene-coated Co 2 (OH) 3 Cl was also prepared under hydrothermal conditions of 180 ℃ for 12 hours in the presence of graphene and dodecylamine. To dissolve CoCl 2 With insoluble Mg (OH) 2 The suspension reacts to prepare Co 2 (OH) 3 Cl. At 500-900 deg.C, adopting spay pyrolysis method to prepare Co 2 (OH) 3 Cl ball [ see: (a) Yin L W2015 J.Mater.Chem.A 3 17659, (b) Ma Z F2014 J.Mater.Chem.A 2 16925, (C) Dewolff P M1953 Acta Crystallogr 6 359 (d) Kang Y C2014 Sci.Rep.4 5785.]. However, synthesis of Co with a crystal structure having unique morphology and good particle size distribution 2 (OH) 3 Cl microparticles remain a challenging topic. More importantly, the microsphere has lower electro-catalytic Oxygen Evolution (OER) overpotential and better activity than commercial RuO 2 The activity of the catalyst after 500 electrochemical CV circulation activation is further enhanced, and when ferrous ions are doped, the activity is x% Fe-Co 2 (OH) 3 Cl (x=5-20%) is better than commercial RuO 2 The catalyst has the advantages of further enhanced activity after 500 electrochemical CV circulation activation, good stability and good application prospect in the aspect of electrocatalytic decomposition of water.
Disclosure of Invention
The invention aims to provide Co 2 (OH) 3 Cl micrometer spheres and Fe thereof 2+ Doped Co 2 (OH) 3 A preparation method of Cl microspheres.
The technical scheme of the invention is as follows:
co (cobalt) 2 (OH) 3 The Cl microspheres are of a rhombohedral system and a hollow structure, and are uniformly and singly dispersed and have the diameter of 0.6 mu m.
Fe element modified Co 2 (OH) 3 Cl microsphere (X% Fe-Co) 2 (OH) 3 Cl), which is a rhombohedral system, the amount of modification of Fe, i.e., the mole fraction of Fe (X% = Fe/(fe+co)) is 5%,10%,15% and 20%, respectively. X% Fe-Co 2 (OH) 3 The diameter of the Cl microsphere is 0.5-0.6 mu m.
Co of the present invention 2 (OH) 3 The Cl microspheres are measured by XRD, the positions and the intensities of the peaks are matched with literature values, and no other impurity peaks are found, so that the purity of the product is high. Co by SEM photograph 2 (OH) 3 The Cl microspheres were approximately 0.6 μm in diameter.
X% Fe-Co of the present invention 2 (OH) 3 Cl (x=5, 10, 15 and 20) microspheres were XRD-determined, peak positions and pure Co 2 (OH) 3 Cl is consistent and no other impurity peaks are found, indicating that the Fe element is doped into the lattice or highly dispersed Fe species are formed at the surface, exceeding the XRD limit. X% Fe-Co by SEM photograph 2 (OH) 3 The diameter of the Cl microsphere is 0.5-0.6um, and the nano particles on the surface of the microsphere increase along with the increase of the addition amount of Fe.
As can be seen from the electrochemical polarization curve (LSV), co 2 (OH) 3 The Cl microspheres have lower electro-catalytic Oxygen Evolution (OER) overpotential, and the activity is further enhanced after 500 electrochemical CV cycles of activation. Meanwhile, the modification of Fe can further increase OER activity, whether before or after CV activation. And 10% Fe-Co 2 (OH) 3 Cl shows the best activity, which is superior to the commercial RuO 2 Catalyst, at the same time, co 2 (OH) 3 Cl and Fe-Co 2 (OH) 3 The Cl microspheres also have good stability, therefore, co 2 (OH) 3 Cl and Fe-Co 2 (OH) 3 The Cl microspheres have good application prospect in the aspect of electrocatalytic decomposition of water.
Preparation of Co according to the present invention 2 (OH) 3 Cl and Fe-Co 2 (OH) 3 Cl microspheres, the method has the advantages of simple and easily obtained raw materials and simple and easy conditions.
Drawings
FIG. 1 is Co of the present invention 2 (OH) 3 Cl and X% Fe-Co 2 (OH) 3 XRD patterns of Cl (x=5, 10, 15 and 20) microspheres;
FIG. 2 is Co of the present invention 2 (OH) 3 Cl and X% Fe-Co 2 (OH) 3 SEM photographs of Cl (x=5, 10, 15 and 20) microspheres;
FIG. 3 (a, b) shows the X% Fe-Co of the present invention 2 (OH) 3 The activity of the microspheres OER of Cl (X=0, 5, 10, 15 and 20) (solid line is LSV curve of freshly prepared sample; dotted line is LSV curve of response color after 500 cyclic voltammetry, sweep speed 5 mVs) -1 Rotating disk electrode speed 1600 rpm); (c, d) stability diagram (chronoamperometric curve).
Detailed Description
EXAMPLE 1 Co 2 (OH) 3 Preparation of Cl microspheres
Solvothermal method: 1.82g of Co (NO) was weighed out 3 ) 2 ·6H 2 O,6.0g of sodium hexadecyl benzene sulfonate and 0.183g of NaCl were completely dissolved in 40ml of ethylene glycol, and stirring was continued for 30min to form a homogeneous solution. Transferring the solution into an autoclave with polytetrafluoroethylene as a lining, placing the autoclave in a 90 ℃ oven for 6 hours, then heating the autoclave to 180 ℃ and continuously maintaining the autoclave for 2 hours. Finally, the resulting sample was filtered and washed three times with deionized water and absolute ethanol, respectively, and dried naturally for 12 hours.
EXAMPLE 2.5% Fe-Co 2 (OH) 3 Preparation of Cl (x=5, 10, 15 and 20) microspheres
Solvothermal method: 1.73g of Co (NO) was weighed out 3 ) 2 ·6H 2 O，0.0396g FeCl 2 6.0g of sodium hexadecyl benzene sulfonate and 0.183g of NaCl were completely dissolved in 40ml of ethylene glycol, and stirring was continued for 30min, to form a homogeneous solution. Transferring the solution into an autoclave with polytetrafluoroethylene as a lining, placing the autoclave in a 90 ℃ oven for 6 hours, then heating the autoclave to 180 ℃ and continuously maintaining the autoclave for 2 hours. Finally, the resulting sample was filtered and washed three times with deionized water and absolute ethanol, respectively, and dried naturally for 12 hours.
EXAMPLE 3.10% Fe-Co 2 (OH) 3 Preparation of Cl (x=5, 10, 15 and 20) microspheres
Solvothermal method: 1.64g of Co (NO) was weighed out 3 ) 2 ·6H 2 O，0.0793g FeCl 2 6.0g of sodium hexadecyl benzene sulfonate and 0.183g of NaCl are completely dissolved in 40ml of glycol and the mixture is continuedStirring for 30min, a homogeneous solution was formed. Transferring the solution into an autoclave with polytetrafluoroethylene as a lining, placing the autoclave in a 90 ℃ oven for 6 hours, then heating the autoclave to 180 ℃ and continuously maintaining the autoclave for 2 hours. Finally, the resulting sample was filtered and washed three times with deionized water and absolute ethanol, respectively, and dried naturally for 12 hours.
EXAMPLE 4.15% Fe-Co 2 (OH) 3 Preparation of Cl (x=5, 10, 15 and 20) microspheres
Solvothermal method: 1.55g of Co (NO) was weighed out 3 ) 2 ·6H 2 O，0.119g FeCl 2 6.0g of sodium hexadecyl benzene sulfonate and 0.183g of NaCl were completely dissolved in 40ml of ethylene glycol, and stirring was continued for 30min, to form a homogeneous solution. Transferring the solution into an autoclave with polytetrafluoroethylene as a lining, placing the autoclave in a 90 ℃ oven for 6 hours, then heating to 180 ℃ and continuously maintaining for 2 hours. Finally, the resulting sample was filtered and washed three times with deionized water and absolute ethanol, respectively, and dried naturally for 12 hours.
EXAMPLE 5.20% Fe-Co 2 (OH) 3 Preparation of Cl (x=5, 10, 15 and 20) microspheres
Solvothermal method: 1.46g of Co (NO) was weighed out 3 ) 2 ·6H 2 O，0.158g FeCl 2 6.0g of sodium hexadecyl benzene sulfonate and 0.183g of NaCl were completely dissolved in 40ml of ethylene glycol, and stirring was continued for 30min, to form a homogeneous solution. Transferring the solution into an autoclave with polytetrafluoroethylene as a lining, placing the autoclave in a 90 ℃ oven for 6 hours, then heating to 180 ℃ and continuously maintaining for 2 hours. Finally, the resulting sample was filtered and washed three times with deionized water and absolute ethanol, respectively, and dried naturally for 12 hours.
Co prepared in this example 2 (OH) 3 The Cl microspheres were XRD-measured, the positions and intensities of the peaks were matched with literature values, and no other impurity peaks were found, indicating that the purity of the product was relatively high (see FIG. 1). X% Fe-Co of the present invention 2 (OH) 3 Cl (x=5, 10, 15 and 20) microspheres were XRD-determined, peak positions and pure Co 2 (OH) 3 Cl is consistent, no other impurity peaks are found (see FIG. 1), indicating that Fe element is doped into the crystal lattice or forms high surfaceThe dispersed Fe species exceeded the XRD limit. Co by SEM photograph 2 (OH) 3 The diameter of the Cl microspheres was about 0.6um (see fig. 2). X% Fe-Co by SEM photograph 2 (OH) 3 The Cl microspheres were 0.5 to 0.6um in diameter, and nanoparticles on the surface of the microspheres increased with the addition of Fe (see fig. 2).
Co to be prepared 2 (OH) 3 Cl microspheres and X% Fe-Co 2 (OH) 3 The microspheres of Cl (x=5, 10, 15 and 20) were subjected to OER performance test, and the results are shown in fig. 3.
Claims (3)
1. Fe (Fe) 2+ Doped Co 2 (OH) 3 Cl microsphere, its characterized in that: the diameter of the microsphere is 0.5-0.6um, and the microsphere is a single rhombohedral system, and the composition of the microsphere is X% Fe-Co 2 (OH) 3 Cl, X% is Fe 2+ Molar doping amounts of 5%,10%,15% and 20%, fe 2+ Mole fraction X% = Fe 2+ /(Fe 2+ +Co 2+ )。
2. Use of the microspheres of claim 1, wherein: is used for electrocatalytic oxygen evolution.
3. A method for preparing the microspheres according to claim 1, wherein: co (NO) was weighed in the proportion of X% 3 ) 2 ·6H 2 O and FeCl 2 6.0g of sodium hexadecyl benzene sulfonate and 0.183g of NaCl are added and completely dissolved in 40ml of glycol, and stirring is continued for 30min to form a homogeneous solution; transferring the solution into an autoclave with polytetrafluoroethylene as a lining, placing the autoclave in a 90 ℃ oven for 6 hours, then heating the autoclave to 180 ℃ and keeping the temperature for 2 hours; finally, the precipitate was filtered and washed with deionized water and absolute ethanol, respectively, and dried naturally to obtain microspheres.
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