CN112928232A - Polyhedral structure iron oxide material and preparation method and application thereof - Google Patents
Polyhedral structure iron oxide material and preparation method and application thereof Download PDFInfo
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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Abstract
The invention provides a polyhedral structure iron oxide material and a preparation method and application thereof, belonging to the technical field of iron oxide product preparation. According to the method, firstly, lattice defects are formed on the surface of an iron matrix through acid treatment, then the surfactant is used as an accelerator, the electronegativity of an S element in the surfactant is strong, the electronic structure of the surface of the iron matrix can be changed, the surface of the iron matrix can be easily oxidized with water in an electrolyte in a hydrothermal reaction process, the crystal structure of iron oxide can grow in situ along the lattice defects, and the in-situ grown polyhedral iron oxide material is obtained. The size of the prepared polyhedral particles is micron-sized, the inherent structural characteristics of the polyhedron enable more active sites to be available, the loading capacity of the active material can be increased, and the utilization rate of the material is improved.
Description
Technical Field
The invention relates to the technical field of iron oxide product preparation, in particular to a polyhedral structure iron oxide material and a preparation method and application thereof.
Background
In recent years, the application fields of electrochemical energy storage devices are becoming more and more extensive, including electric vehicles, aerospace, electronic products, renewable energy storage and the like. Lithium ion batteries and supercapacitors are the current focus of research. However, the lithium battery has the defects of large safety problem, high price, low power density and the like, and the industrial application of the lithium battery is limited; the super capacitor has the common characteristics of a lithium battery and a common capacitor, and has potential application value.
At present, the iron-based oxide is considered to be a suitable cathode material due to the characteristics of low price, easily available raw materials, no toxicity, relatively negative voltage window (-1 Vto 0Vvs. Ag/AgCl), capability of generating reversible oxidation-reduction reaction and the like. However, the existing iron-based oxide has the disadvantages of low conductivity, low energy density per unit area, low activity and the like, so that the iron-based oxide is difficult to meet the actual requirement. Therefore, designing a proper electrode material, improving the conductivity and increasing the active sites is a main research direction for improving the electrochemical performance of the iron-based oxide.
Disclosure of Invention
The invention aims to provide a polyhedral structure iron oxide material, a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a polyhedral structure iron oxide material, which comprises the following steps:
carrying out acid treatment on the iron matrix to obtain a treated iron matrix;
mixing a surfactant solution with an alkaline aqueous solution to obtain an electrolyte;
immersing the processed iron matrix into the electrolyte, and carrying out hydrothermal treatment to obtain a polyhedral structure iron oxide material;
the surfactant in the surfactant solution is an alkali metal sulfide.
Preferably, the pH value of the acid used for acid treatment is 5.5-6.5; the temperature of the acid treatment is 25-30 ℃; the treatment time is 5-15 s.
Preferably, the alkali metal sulfide is sodium sulfide or potassium sulfide, and the concentration of the surfactant solution is 1-150 g/L.
Preferably, the alkali in the alkaline aqueous solution comprises NaOH or KOH, and the concentration of the alkaline aqueous solution is 1-500 g/L.
Preferably, the volume ratio of the surfactant solution to the alkaline aqueous solution is 1 (1-3).
Preferably, the iron matrix is flat plate iron, iron foil or porous iron, and the iron content in the iron matrix is greater than 98 wt%.
Preferably, the temperature of the hydrothermal treatment is 120-250 ℃ and the time is 12-48 h.
The invention provides the polyhedral structure iron oxide material prepared by the preparation method in the technical scheme.
The invention provides application of the polyhedral structure iron oxide material in the technical scheme in a super capacitor.
The invention provides a preparation method of a polyhedral structure iron oxide material, which comprises the following steps: carrying out acid treatment on the iron matrix to obtain a treated iron matrix; mixing a surfactant solution with an alkaline aqueous solution to obtain an electrolyte; immersing the processed iron matrix into the electrolyte, and carrying out hydrothermal treatment to obtain a polyhedral structure iron oxide material; the surfactant in the surfactant solution is an alkali metal sulfide. According to the method, firstly, lattice defects are formed on the surface of an iron matrix through acid treatment, then the surfactant is used as an accelerator, the electronegativity of an S element in the surfactant is strong, the electronic structure of the surface of the iron matrix can be changed, the surface of the iron matrix can be easily oxidized with water in an electrolyte in a hydrothermal reaction process, the crystal structure of iron oxide can grow in situ along the lattice defects, and the in-situ grown polyhedral iron oxide material is obtained. The size of the prepared polyhedral particles is micron-sized, the inherent structural characteristics of the polyhedron enable more active sites to be available, the loading capacity of the active material can be increased, and the utilization rate of the material is improved.
The method has the advantages of cheap raw materials, simple process, easy operation, low production cost, short production period and high product purity, and is suitable for industrial production.
Drawings
FIG. 1 is an SEM image of a polyhedral iron oxide material prepared in example 1;
FIG. 2 is an XRD pattern of the polyhedral iron oxide material prepared in example 1 (control JPCDS card);
FIG. 3 is a constant current charge and discharge curve diagram of the polyhedral structure iron oxide material prepared in example 1 under different current densities;
FIG. 4 is a graph comparing the capacity of the polyhedral iron oxide material prepared in example 1 with that of the prior art reference;
FIG. 5 shows the current density of 50mA cm for the polyhedral iron oxide material prepared in example 1-2Cycle performance plot under conditions.
Detailed Description
The invention provides a preparation method of a polyhedral structure iron oxide material, which comprises the following steps:
carrying out acid treatment on the iron matrix to obtain a treated iron matrix;
mixing a surfactant solution with an alkaline aqueous solution to obtain an electrolyte;
immersing the processed iron matrix into the electrolyte, and carrying out hydrothermal treatment to obtain a polyhedral structure iron oxide material;
the surfactant in the surfactant solution is an alkali metal sulfide.
In the present invention, unless otherwise specified, all the starting materials required for the preparation are commercially available products well known to those skilled in the art.
The invention carries out acid treatment on the iron matrix to obtain the treated iron matrix. In the present invention, the iron matrix is preferably flat plate iron, iron foil or porous iron, the iron content in the iron matrix preferably being >98 wt%. The source of the iron matrix in the present invention is not particularly limited, and commercially available products known in the art may be used.
In the present invention, it is preferable that the iron matrix is washed before the iron matrix is subjected to acid treatment. In the invention, the washing process is preferably to wash the iron matrix by sequentially adopting ultrapure water and absolute ethyl alcohol respectively, and the invention obtains a clean iron surface by washing, dedusting and deoiling.
In the invention, the pH value of the acid used for acid treatment is preferably 5.5-6.5, and more preferably 6.0; the acid used for the acid treatment is preferably hydrochloric acid or sulfuric acid; the acid treatment temperature is preferably 25-30 ℃, and the time is preferably 5-15 s. According to the invention, a layer of iron on the surface of the iron matrix is dissolved through acid treatment, so that the surface of iron metal is changed into silver gray, thereby forming a lattice defect, and being beneficial to the formation of a polyhedral crystal structure in the subsequent iron oxide.
The invention mixes the surfactant solution and the alkaline aqueous solution to obtain the electrolyte. In the present invention, the surfactant in the surfactant solution is an alkali metal sulfide; the alkali metal sulfide is preferably sodium sulfide or potassium sulfide, and the concentration of the surfactant solution is preferably 1-150 g/L, more preferably 10-120 g/L, and further preferably 50-100 g/L; the solvent of the surfactant solution is preferably water. In the invention, the alkali in the alkaline aqueous solution preferably comprises NaOH or KOH, and the concentration of the alkaline aqueous solution is preferably 1-500 g/L, more preferably 10-120 g/L, and further preferably 50-100 g/L.
In the invention, the volume ratio of the surfactant solution to the alkaline aqueous solution is preferably 1 (1-3), and more preferably 1 (1.5-2.5). In the surfactant used in the invention, the electronegativity of the S element is strong, so that the electronic structure of the surface of the iron matrix can be changed, the iron matrix can be easily combined with oxygen in a solution to generate iron oxide, and the generation of the polyhedral structure iron oxide is promoted.
In the present invention, the process of mixing the surfactant solution with the alkaline aqueous solution is preferably to drop the surfactant solution into the alkaline aqueous solution under the nitrogen atmosphere.
After the electrolyte is obtained, the processed iron matrix is immersed into the electrolyte and subjected to hydrothermal treatment to obtain the polyhedral structure iron oxide material. In the present invention, the process of immersing the iron matrix in the electrolyte is preferably to transfer the electrolyte to a reaction kettle through a drainage device, and simultaneously immerse the pretreated iron matrix in the electrolyte under the protection of inert gas. In the present invention, the inert gas is preferably argon gas. In the invention, the drainage device is preferably a closed drainage device, and the flow velocity of the drainage device is preferably 3-10 m/s.
In the present invention, the hydrothermal treatment is preferably performed in a muffle furnace under sealed conditions to prevent oxidation of the iron oxide material and the electrolyte; the temperature of the hydrothermal treatment is preferably 120-250 ℃, and more preferably 150-200 ℃; the time is preferably 12 to 48 hours, and more preferably 24 to 36 hours. In the hydrothermal treatment process, the surface of the metal iron matrix interacts with water in electrolyte, namely the surface of the iron matrix and oxygen in water molecules are subjected to oxidation reaction, so that the crystal structure of the iron matrix grows in situ along lattice defects generated on the surface of the iron matrix to form the polyhedral iron oxide.
After the hydrothermal treatment is completed, the obtained material is preferably taken out, washed by ultrapure water and absolute ethyl alcohol respectively, and dried to obtain the polyhedral structure iron oxide material. The specific washing process is not particularly limited in the present invention, and may be carried out according to a process well known in the art. In the invention, the drying is preferably carried out in a vacuum drying oven, and the drying time is preferably 2-5 h, and more preferably 2.5-3.5 h. Other conditions for the drying are not particularly limited in the present invention, and the drying can be carried out according to a process well known in the art.
The invention provides the polyhedral structure iron oxide material prepared by the preparation method in the technical scheme. In the iron oxide material with the polyhedral structure, polyhedral crystals grow uniformly in situ on the surface of an iron matrix, so that a larger specific surface area and more active sites can be provided, and the conductivity of the iron-based oxide is further improved.
The invention provides application of the polyhedral structure iron oxide material in the technical scheme in a super capacitor. The method of the present invention is not particularly limited, and the method may be applied according to a method known in the art.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. 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.
Example 1
Washing commercial porous iron (iron content >98 wt%) with ultrapure water and ethanol, respectively, to obtain a clean iron surface, acid-treating with dilute hydrochloric acid at pH 6.0 at 25 ℃ for 10s to obtain a pretreated iron matrix;
15mL of 336g/L KOH aqueous solution was prepared, and 5mL of 120g/L Na was added dropwise thereto2S, obtaining an aqueous solution of the electrolyte;
transferring the electrolyte into a reaction kettle through a closed drainage device (the flow rate is 5m/s), and simultaneously immersing the pretreated iron matrix into the electrolyte under the protection of argon; and (3) placing the reaction kettle in a muffle furnace at 180 ℃ for hydrothermal treatment for 24h, taking out the obtained material, respectively cleaning the material with ultrapure water and absolute ethyl alcohol, and drying the material in a vacuum drying oven for 3h to obtain the polyhedral structure iron oxide material.
Example 2
Commercial iron foil (iron content >98 wt%) was washed with ultrapure water and ethanol, respectively, to obtain a clean iron surface, and acid-treated with dilute hydrochloric acid at pH 6.0 at 25 ℃ for 10s to obtain a pretreated iron matrix;
15mL of 200g/L NaOH aqueous solution was prepared, and 5mL of 120g/L K was added dropwise thereto2S, obtaining an aqueous solution of the electrolyte;
transferring the electrolyte into a reaction kettle through a closed drainage device (the flow rate is 5m/s), and simultaneously immersing the pretreated iron matrix into the electrolyte under the protection of argon; and (3) placing the reaction kettle in a muffle furnace at 240 ℃ for hydrothermal treatment for 12h, taking out the obtained material, respectively cleaning the material with ultrapure water and absolute ethyl alcohol, and drying the material in a vacuum drying oven for 2.5h to obtain the polyhedral structure iron oxide material.
Example 3
Commercial iron foil (iron content >98 wt%) was washed with ultrapure water and ethanol, respectively, to obtain a clean iron surface, and acid-treated with dilute hydrochloric acid at pH 6.5 at 25 ℃ for 10s to obtain a pretreated iron matrix;
15mL of a 100g/L KOH aqueous solution was prepared, and 5mL of 150g/L Na was added dropwise thereto2S, obtaining an aqueous solution of the electrolyte;
transferring the electrolyte into a reaction kettle through a closed drainage device (the flow rate is 5m/s), and simultaneously immersing the pretreated iron matrix into the electrolyte under the protection of argon; and (3) placing the reaction kettle in a muffle furnace at 120 ℃ for hydrothermal treatment for 24h, taking out the obtained material, respectively cleaning the material with ultrapure water and absolute ethyl alcohol, and drying the material in a vacuum drying oven for 2.5h to obtain the polyhedral structure iron oxide material.
Example 4
Washing commercial porous iron (iron content >98 wt%) with ultrapure water and ethanol, respectively, to obtain a clean iron surface, acid-treating with dilute hydrochloric acid at pH 5.5 at 25 ℃ for 10s to obtain a pretreated iron matrix;
15mL of 500g/L KOH aqueous solution was prepared, and 5mL of 50g/L Na was added dropwise thereto2S, obtaining an aqueous solution of the electrolyte;
transferring the electrolyte into a reaction kettle through a closed drainage device (the flow rate is 5m/s), and simultaneously immersing the pretreated iron matrix into the electrolyte under the protection of argon; and (3) placing the reaction kettle in a muffle furnace at 250 ℃ for hydrothermal treatment for 48h, taking out the obtained material, respectively cleaning the material with ultrapure water and absolute ethyl alcohol, and drying the material in a vacuum drying oven for 4h to obtain the polyhedral structure iron oxide material.
Performance testing
1) SEM characterization is carried out on the polyhedral structure iron oxide material prepared in example 1, and the result is shown in figure 1; as can be seen from fig. 1, the polyhedral crystal grows uniformly on the surface of the iron matrix, and the size of the polyhedral particle is micron-sized, which can provide a larger specific surface area and more active sites.
2) XRD test was performed on the polyhedral iron oxide material prepared in example 1, and the result is shown in FIG. 2; as shown in FIG. 2, the product obtained by the in-situ growth of example 1 is an iron oxide material as can be demonstrated by comparing standard cards (PDF # 39-1346).
3) Electrochemical tests are carried out on the polyhedral structure iron oxide prepared in example 1, in a three-electrode system, iron oxide is used as a working electrode, a graphite plate is used as a counter electrode, Ag/AgCl is used as a reference electrode, a KOH solution with the concentration of 336g/L is used as an electrolyte, constant current charging and discharging data under different current densities are plotted, and the result is shown in FIG. 3. As shown in FIG. 3, the prepared polyhedral iron oxide material had a current density of 50mA cm-2、100mA·cm-2、150mA·cm-2、200mA·cm-2And 250mA · cm-2The area capacity (area capacity: current density × discharge time (discharge time obtained from fig. 3)) exhibited under the conditions was 3.018mAh · cm, respectively-2、2.903mAh·cm-2、2.833mAh·cm-2、2.983mAh·cm-2And 2.931mAh cm-2. (the relation between the area capacity and the energy density is E-1/2 CV2Where E represents energy density, C represents area capacity, and V represents discharge voltage, i.e., the larger the area capacity, the larger the energy density).
4) The polyhedral iron oxide prepared in example 1 was compared with the iron oxide products of the prior art documents, and the results are shown in fig. 4. As shown in fig. 4, the area capacity of the iron oxide prepared by the present invention shows a higher area energy density than that of the prior art; wherein Ref.1 to Ref.9 represent the prior documents respectively, and the document information is [1 ] in sequence]X.Lu,Y.Zeng,M.Yu,T.Zhai,C.Liang,S.Xie,M.-S.Balogun,Y.Tong,Oxygen-Deficient Hematite Nanorods as High-Per formance and Novel Negative Electrodes for Flexible Asymmetric Supercap acitor[J].Adv.Mater.2014,26,3148.[2]C.Liu,Q.Li,Q.Zhang,B.H e,P.Man,Z.Zhou,C.Li,L.Xie,Y.Yao,Surface-functionalized Fe2O3 N anowire Arrays with Enhanced Pseudocapacitive Performance as Novel Ano de Materials for High-Energy-Density Fiber-shaped Asymmetric Supercapacit ors[J].Electrochimica Acta 2020,330,135247.[3]S Su,L Shi,W Yao,Y Wang,P Zou,K Liu,M Wang,F Kang,C Yang,Interface Metallization Enabled an Ultra-Stable Fe2O3 Hierarchical Anode for Pseudocapacitors[J].RSC Adv.,2020,10,8636-8644.[4]J.Yang,Q.Zhang,Z.Wang,Z.Wan g,L.Kang,M.Qi,M.Chen,W.Liu,W.Gong,W.Lu,P.P.Shum,L.We i,Rational Construction of Self-Standing Surfur-Doped Fe2O3 Anodes with Promoted Energy Storage Capability for Wearable Aqueous Rechargeable Ni Co-Fe Batteries[J].Adv.Energy Mater.2020,2001064.[5]C.Guan,J.Li u,Y.Wang,L.Mao,Z.Fan,Z.Shen,H.Zhang,J.Wang,Iron Oxide-Dec orated Carbon for Supercapacitor Anodes with Ultrahigh Energy Density an d Outstanding Cycling Stability[J].ACS Nano,2015,5,5198.[6]C.Zhao,X.Shao,Z.Zhu,C.Zhao,X.Qian,One-pot Hydrothermal Synthesis of RGO/FeS Composite on Fe Foil for High Performance Supercapacitors[J].Electrochimica Acta 2017,246,497-506.[7]Y.Fan,L.Wang,Z.Ma,W.D ai,H.Shao,H.Wang,G.Shao,The In Situ Synthesis of Fe(OH)3Film o n Fe Foam as Efficient Anode of Alkaline Supercapacitor Based on a Pro mising Fe3+/Fe0 Energy Storage Mechanism[J].Part.Part.Syst.Charact.2018,1700484.[8]F.Li,Y.-L.Liu,G.-G.Wang,H.-Y.Zhang,B.Zhang,G.-Z.Li,Z.-P.Wu,L.-Y.Dang,J.-C.Han,Few-Layered Ti3C2TxMxenes Co upled with Fe2O3 Nanorod Arrays Grown on Carbon Cloth as Anodes for Flexible Asymmetric Supercapacitors[J].J.Mater.Chem.A,2019,7,22631-22641.[9]C.Zhou,T.Gao,Y.Wang,Q.Liu,D.Xiao,Through a Hydro thermal Phosphatization Method Synthesized NiCo and Fe-Based Efor High-Performance Battery-Supercapacitor Hybrid Device[J].Applied Surface Scie nce,2019,475,729-739.
5) The polyhedral structure iron oxide prepared in example 1 was subjected to cycle performance test, and the results are shown in fig. 5. As shown in FIG. 5, the polyhedral iron oxide material prepared by the present invention has a current density of 50mA cm-2Under the condition, after 3600 cycles, the area capacity is 3.013mAh cm-2Reducing to 2.619mAh cm-2And the capacity retention rate reaches 86.9 percent.
6) The area capacity test of the polyhedral structure iron oxide prepared in examples 2 to 4 was performed according to the method of the above 3), and the result showed that the area capacity of the polyhedral structure iron oxide prepared in example 2 was 1mAh · cm-2The area capacity of the polyhedral iron oxide prepared in example 3 was 1.2mAh · cm-2The polyhedral iron oxide prepared in example 4 had an area capacity of 0.8mAh cm-2。
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A preparation method of a polyhedral structure iron oxide material comprises the following steps:
carrying out acid treatment on the iron matrix to obtain a treated iron matrix;
mixing a surfactant solution with an alkaline aqueous solution to obtain an electrolyte;
immersing the processed iron matrix into the electrolyte, and carrying out hydrothermal treatment to obtain a polyhedral structure iron oxide material;
the surfactant in the surfactant solution is an alkali metal sulfide.
2. The method according to claim 1, wherein the acid used for the acid treatment has a pH of 5.5 to 6.5; the temperature of the acid treatment is 25-30 ℃; the treatment time is 5-15 s.
3. The method according to claim 1, wherein the alkali metal sulfide is sodium sulfide or potassium sulfide, and the concentration of the surfactant solution is 1 to 150 g/L.
4. The method according to claim 1, wherein the alkali in the aqueous alkali solution comprises NaOH or KOH, and the concentration of the aqueous alkali solution is 1 to 500 g/L.
5. The preparation method according to claim 3 or 4, wherein the volume ratio of the surfactant solution to the alkaline aqueous solution is 1 (1-3).
6. The method of claim 1, wherein the iron matrix is flat plate iron, iron foil or porous iron, and the iron content in the iron matrix is >98 wt%.
7. The preparation method according to claim 1, wherein the temperature of the hydrothermal treatment is 120 to 250 ℃ and the time is 12 to 48 hours.
8. The polyhedral structure iron oxide material prepared by the preparation method of any one of claims 1 to 7.
9. Use of the polyhedral iron oxide material according to claim 8 in a supercapacitor.
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