CN114023942B - Reduced graphene oxide loaded FeTe composite material and preparation method and application thereof - Google Patents
Reduced graphene oxide loaded FeTe composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to the technical field of electrode materials, in particular to a reduced graphene oxide loaded FeTe composite material, and a preparation method and application thereof. The invention provides a reduced graphene oxide loaded FeTe composite material, which comprises reduced graphene oxide and FeTe nano particles loaded on the surface of the reduced graphene oxide. The reduced graphene oxide loaded FeTe composite material has good cycle stability and rate capability.
Description
Technical Field
The invention relates to the technical field of electrode materials, in particular to a reduced graphene oxide loaded FeTe composite material, and a preparation method and application thereof.
Background
As is well known, the secondary battery can be repeatedly charged and discharged, has high efficiency and strong environmental adaptability, has better economical practicability, and becomes a main direction of energy storage research. At present, the lithium ion battery has excellent performances such as high voltage, high energy density, long cycle life and the like, and is widely applied in daily life. Along with the rapid development of the lithium ion battery in the application aspects of electric automobiles and large-scale smart grids, the consumption of lithium resources is continuously increased, the abundance of the lithium resources in the crust is low, the distribution is uneven (mainly concentrated in south america), and the price is high, so that the lithium ion battery is severely restricted to large-scale storageCan be applied to development. In contrast, sodium and lithium belong to the same main group, have similar physical and chemical properties, and have very rich sodium reserves, uniform distribution and low price. Sodium ion batteries are therefore considered to be an ideal choice for the next generation of large scale energy storage technologies. But Na is + Ratio Li + The radius of the lithium ion battery electrode material is large, the reversible deintercalation reaction requires that the material structure has larger sodium containing position and ion migration channel, and the direct use of the derivative of the lithium ion battery electrode material as the electrode material of the sodium ion battery is not suitable.
In view of the above problems, several promising electrochemical sodium storage anode materials have been studied, including carbon materials, alloys (Sn, bi, etc.), metal oxides (MoO 3 、Fe 2 O 3 、Sb 2 O 3 Or NiO, etc.) and transition metal chalcogenides (SnS 2 、MoS 2 、FeS 2 、MoSe 2 、CoSe 2 、CoTe 2 Or FeTe, etc.). It is reported that metal telluride (e.g., feTe) having similar characteristics to metal selenide has the advantages of high specific capacity and wide sources, and is a very potential negative electrode material for sodium ion batteries. However, pure-phase FeTe crystals cause pulverization of materials due to large volume change in the process of sodium ion deintercalation, so that electrode materials fall off from the surface of a current collector, the reversible capacity of the materials is rapidly attenuated in the circulating process, and the lower conductivity also limits the rate capability of the materials.
Disclosure of Invention
The invention aims to provide a reduced graphene oxide loaded FeTe composite material, and a preparation method and application thereof. The reduced graphene oxide loaded FeTe composite material has good cycle stability and rate capability.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a reduced graphene oxide loaded FeTe composite material, which comprises reduced graphene oxide and FeTe nano particles loaded on the surface of the reduced graphene oxide.
Preferably, the mass ratio of the reduced graphene oxide to the FeTe nano-particles is (0.1-0.6): 1, a step of;
the particle size of the FeTe nano particles is 20-200 nm.
The invention also provides a preparation method of the reduced graphene oxide loaded FeTe composite material, which comprises the following steps:
mixing an iron source, tellurite, strong alkali, a surfactant and a reduced graphene oxide solution, and performing solvothermal reaction to obtain a precursor;
and calcining the precursor to obtain the reduced graphene oxide loaded FeTe composite material.
Preferably, the iron source comprises a soluble ferric salt;
the tellurite comprises an alkali metal salt of tellurite;
the strong base comprises one or more of hydrazine hydrate, sodium hydroxide and potassium hydroxide;
the surfactant comprises sodium dodecyl sulfate and/or cetyltrimethylammonium bromide.
Preferably, the concentration of the reduced graphene oxide solution is 2-3 mg/mL;
the solvent of the reduced graphene oxide solution is a mixed solution of water and N, N-dimethylformamide in a volume ratio of 1:1.
Preferably, the mass ratio of the iron source, tellurite, strong alkali, surfactant and reduced graphene oxide in the reduced graphene oxide solution is (10-30): (10-30): (30-300): (30-100): (4-15).
Preferably, the solvothermal reaction is carried out at a temperature of 160-200 ℃ for 18-24 hours.
Preferably, the calcination is performed in an inert atmosphere.
Preferably, the calcination temperature is 550-650 ℃ and the calcination time is 3-6 h.
The invention also provides an application of the reduced graphene oxide supported FeTe composite material prepared by the technical scheme or the preparation method of the reduced graphene oxide supported FeTe composite material as an electrode material in a sodium ion battery.
The invention provides a reduced graphene oxide loaded FeTe composite material, which comprises reduced graphene oxide and FeTe nano particles loaded on the surface of the reduced graphene oxide. According to the invention, feTe nano particles on the surface of the reduced graphene oxide are loaded on the surface of the reduced graphene oxide, so that agglomeration of the FeTe nano particles can be effectively inhibited, and the composite material has good initial specific capacity and excellent rate capability; meanwhile, the conductivity and the electrochemical reaction rate of FeTe can be improved by reducing graphene oxide, and in addition, the graphene oxide serving as a buffer substrate can effectively release stress generated by volume change in the charge-discharge cycle process of FeTe and can effectively improve the cycle stability of a sodium ion battery.
The invention also provides a preparation method of the reduced graphene oxide loaded FeTe composite material, which comprises the following steps: mixing an iron source, tellurite, strong alkali, a surfactant and a reduced graphene oxide solution, and performing solvothermal reaction to obtain a precursor; and calcining the precursor to obtain the reduced graphene oxide loaded FeTe composite material. The reduced graphene oxide loaded FeTe composite material prepared by the preparation method is uniform in appearance, high in material purity and simple in preparation method.
Drawings
FIG. 1 is an XRD pattern of a reduced graphene oxide supported FeTe composite material prepared in example 1;
fig. 2 is a TEM image of the reduced graphene oxide supported FeTe composite material prepared in example 1;
fig. 3 is an HRTEM spectrum of the reduced graphene oxide supported FeTe composite material prepared in example 1;
FIG. 4 shows that the button half cell prepared in example 1 was at 0.1 A.g -1 A cycle performance curve at current density of (2);
fig. 5 is a graph showing the rate performance of the button half cell prepared in example 1.
Detailed Description
The invention provides a reduced graphene oxide loaded FeTe composite material, which comprises reduced graphene oxide and FeTe nano particles loaded on the surface of the reduced graphene oxide.
In the present invention, the average particle diameter of the reduced graphene oxide is preferably 5 to 15. Mu.m, more preferably 7 to 10. Mu.m.
In the present invention, the particle size of the FeTe nanoparticle is preferably 20 to 200nm.
In the present invention, the mass ratio of the reduced graphene oxide to the FeTe nanoparticle is preferably (0.1 to 0.6): 1, more preferably (0.2 to 0.6): 1, most preferably (0.4 to 0.6): 1.
the invention also provides a preparation method of the reduced graphene oxide loaded FeTe composite material, which comprises the following steps:
mixing an iron source, tellurite, strong alkali, a surfactant and a reduced graphene oxide solution, and performing solvothermal reaction to obtain a precursor;
and calcining the precursor to obtain the reduced graphene oxide loaded FeTe composite material.
In the present invention, all the preparation materials are commercially available products well known to those skilled in the art unless specified otherwise.
According to the method, an iron source, tellurite, strong alkali, a surfactant and a reduced graphene oxide solution are mixed and subjected to solvothermal reaction to obtain a precursor.
In the present invention, the iron source preferably includes a soluble ferric salt, more preferably one or more of ferric nitrate, ferric sulfate and ferric acetylacetonate; when the iron source is two or more of the above specific choices, the present invention does not have any particular limitation on the ratio of the above specific substances, and the above specific substances may be mixed in any ratio.
In the present invention, the tellurite preferably includes an alkali metal salt of tellurite, more preferably includes sodium tellurite and/or potassium tellurite; when the tellurite is sodium tellurite and potassium tellurite, the proportion of the sodium tellurite and the potassium tellurite is not limited in any particular way, and the sodium tellurite and the potassium tellurite are mixed according to any proportion.
In the present invention, the strong base preferably includes one or more of hydrazine hydrate, sodium hydroxide and potassium hydroxide; when the alkali is two or more of the above specific choices, the present invention does not have any particular limitation on the ratio of the above specific substances, and the above specific substances may be mixed in any ratio.
In the present invention, the surfactant preferably includes sodium dodecyl sulfate and/or cetyltrimethylammonium bromide; when the surfactant is sodium dodecyl sulfate and cetyl trimethyl ammonium bromide, the mixture ratio of the sodium dodecyl sulfate and the cetyl trimethyl ammonium bromide is not limited in any particular way, and the sodium dodecyl sulfate and the cetyl trimethyl ammonium bromide are mixed according to any mixture ratio.
In the present invention, the concentration of the reduced graphene oxide solution is preferably 2 to 3mg/mL, more preferably 2.2 to 2.8mg/mL, and most preferably 2.4 to 2.6mg/mL. In the invention, the solvent of the reduced graphene oxide solution is preferably a mixed solution of water and N, N-dimethylformamide in a volume ratio of 1:1; the water is preferably deionized water.
In the present invention, the reduced graphene oxide solution is preferably prepared by a method of preparing the reduced graphene oxide solution, which preferably includes the steps of:
firstly mixing water and N, N-dimethylformamide to obtain a mixed solvent;
and secondly mixing the reduced graphene oxide with the mixed solvent to obtain the reduced graphene oxide solution.
The first mixing process is not particularly limited, and the first mixing process is performed by a process well known to those skilled in the art and ensures that the water and the N, N-dimethylformamide are uniformly mixed.
In the present invention, the second mixing is preferably performed under ultrasonic conditions, and the ultrasonic conditions are not particularly limited in the present invention, and may be performed by a process well known to those skilled in the art.
In the present invention, the mass ratio of the iron source, tellurite, strong base, surfactant and reduced graphene oxide in the reduced graphene oxide solution is preferably (10 to 30): (10-30): (30-300): (30-100): (4 to 15), more preferably (10 to 30): (10-30): (30-50): (30-50): (10 to 15), most preferably (15 to 25): (15-25): 35-45): (35-45): (12-14)
In the present invention, the mixing is preferably performed under stirring, and the stirring speed is not particularly limited, and may be performed at a speed well known to those skilled in the art. In the present invention, the stirring time is preferably 1 to 4 hours, more preferably 2 to 3 hours.
In the present invention, the temperature of the solvothermal reaction is preferably 160 to 200 ℃, more preferably 170 to 190 ℃, and most preferably 175 to 180 ℃. In the present invention, the time of the solvothermal reaction is preferably 18 to 24 hours, more preferably 20 to 22 hours.
After the solvothermal reaction is completed, the invention also preferably comprises the steps of cooling, centrifuging, washing and drying which are sequentially carried out; the cooling process is not particularly limited, and may be performed by a process known to those skilled in the art. The centrifugation process is not particularly limited, and may be performed by a process known to those skilled in the art. In the present invention, the washing liquid used for the washing is preferably water and N, N-dimethylformamide. In the present invention, the temperature of the drying is preferably 70℃and the time is preferably 12 hours.
After the precursor is obtained, the precursor is calcined, and the reduced graphene oxide loaded FeTe composite material is obtained.
In the present invention, the calcination is preferably performed in an inert atmosphere, more preferably in an argon atmosphere.
In the present invention, the temperature of the calcination is preferably 550 to 650 ℃, more preferably 580 to 620 ℃; the time is preferably 3 to 6 hours, more preferably 4 to 5 hours; the rate of heating to the calcination temperature is preferably 2 to 5℃per minute, more preferably 3℃per minute.
The invention also provides an application of the reduced graphene oxide supported FeTe composite material prepared by the technical scheme or the preparation method of the reduced graphene oxide supported FeTe composite material as an electrode material in a sodium ion battery.
In the present invention, the method of application preferably comprises the steps of:
mixing the reduced graphene oxide loaded FeTe composite material, a conductive agent, a binder and water to obtain negative electrode slurry;
and coating the negative electrode slurry on the surface of a negative electrode current collector, and drying to obtain the negative electrode.
In the present invention, the conductive agent is preferably conductive carbon black; the binder is preferably sodium alginate; the mass ratio of the reduced graphene oxide loaded FeTe composite material, the conductive agent, the binder and the water is preferably (60-80): (8-20): (5-15): (10 to 50), more preferably 7:2:1:5.
the mixing process is not particularly limited, and may be performed by a process well known to those skilled in the art.
In the present invention, the negative electrode current collector is preferably a copper sheet.
The coating and drying process is not particularly limited, and may be performed by a process known to those skilled in the art.
In the present invention, after the negative electrode is obtained, the negative electrode is preferably applied to the sodium ion battery, and the application process is not particularly limited, and a method for assembling the sodium ion battery, which is well known to those skilled in the art, is adopted, and a conventional electrolyte and a conventional separator, which are well known and used for the sodium ion battery, are selected.
In the embodiment of the invention, in order to verify the electrochemical performance of the anode material, the electrolyte solution is NaClO 4 Is prepared from ethylene carbonate and propylene carbonate (the volume ratio of the ethylene carbonate to the propylene carbonate is 1:1, and NaClO is contained in the electrolyte 4 At a concentration of 1 mol/L). The membrane is Whatman GF/C glass fiber filter paper; the counter electrode is a metal sodium sheet.
The reduced graphene oxide supported FeTe composite material, the preparation method and the application thereof provided by the invention are described in detail below with reference to examples, but are not to be construed as limiting the scope of the invention.
Example 1
Mixing 20mL of deionized water with 20mLN, N-dimethylformamide, adding 90mg of reduced graphene oxide, and mixing under the condition of ultrasound to obtain a reduced graphene oxide solution;
0.4g of Fe (NO) 3 ) 3 ·9H 2 O、0.22g Na 2 TeO 3 、0.4g NaOH、2g N 2 H 4 ·H 2 O、0.57g C 12 H 25 SO 4 Mixing Na and the reduced graphene oxide solution, stirring for 1h, performing solvothermal reaction at 200 ℃ for 24h, sequentially cooling and centrifuging, washing a solid product obtained by centrifuging with water and N, N-dimethylformamide, and finally drying at 70 ℃ for 12h to obtain a precursor;
heating the precursor to 600 ℃ at a heating rate of 3 ℃/min in argon atmosphere, and preserving heat for 4 hours to obtain a reduced graphene oxide loaded FeTe composite material (the mass ratio of the reduced graphene oxide to the FeTe nano particles is 0.4:1, and the particle size of the FeTe nano particles is 20-200 nm);
XRD test is carried out on the reduced graphene oxide loaded FeTe composite material, and a test result is shown in figure 1, and as can be seen from figure 1, the diffraction spectrum of the reduced graphene oxide loaded FeTe composite material is completely matched with an FeTe standard card, and the material crystallinity is high, and the reduced graphene oxide loaded FeTe composite material belongs to a tetragonal system.
Carrying out TEM test on the reduced graphene oxide loaded FeTe composite material, wherein the test results are shown in figures 2-3, and figure 2 is a TEM image, wherein a is a TEM image under a small multiplying power, and b is a TEM image under a large multiplying power; as can be seen from fig. 2, the particle size of FeTe in the reduced graphene oxide loaded FeTe composite material is 20-200 nm, and the particles are uniformly distributed on the surface of the reduced graphene oxide; FIG. 3 is a HRTEM spectrum, and as can be seen from FIG. 3, the interplanar spacing is 0.326nm, belonging to FeTe (101) crystal planes;
mixing the reduced graphene oxide loaded FeTe composite material, conductive carbon black and sodium alginate according to the mass ratio of 7:2:1, adding 5mL of deionized water, and stirring for 4 hours to obtain slurry;
coating the slurry on the copper foil, and drying to obtain a negative electrode;
the metal sodium sheet is used as a counter electrode, naClO is used 4 Is prepared from ethylene carbonate and propylene carbonate (the volume ratio of the ethylene carbonate to the propylene carbonate is 1:1, and NaClO is contained in the electrolyte 4 1 mol/L) is used as electrolyte, whatman GF/C glass fiber filter paper is used as a diaphragm, and the button half cell is assembled;
the button half cell was assembled with pure phase FeTe in the above-described method for preparing button half cell, and as a comparative example, the button half cell was fabricated at 0.1 A.g -1 According to the current density of (2) and constant current charge and discharge tests, the test result is shown in figure 4, and as can be seen from figure 4, the reduced graphene oxide loaded FeTe composite material has 526 mAh.g when being used as a negative electrode material of a sodium ion battery -1 The specific discharge capacity of the first turn of the steel sheet is 100 mAh.g -1 The reversible discharge specific capacity of 100 circles of the current density is 360 mAh.g -1 . Whereas the first-turn specific capacity of the pure-phase FeTe as a comparison is 457 mAh.g -1 The reversible discharge specific capacity of the lithium ion battery is 236 mAh.g after 100 circles of circulation under the current density of 100mAg-1 -1 . Compared with pure-phase FeTe, the FeTe/RGO prepared by the method has better initial-cycle discharge specific capacity and cycle stability;
the button half cell was assembled with pure phase FeTe in the above-described method for preparing button half cell, and as a comparative example, the button half cell was fabricated at 0.1 A.g -1 、0.2A·g -1 、0.5A·g -1 、1A·g -1 、2A·g -1 、5A·g -1 And 10 A.g -1 The current density of (2) is tested for rate performance, and the test result is shown in FIG. 5. As can be seen from FIG. 5, the reduced graphene oxide loaded FeTe composite material is 0.1 A.g -1 、0.2A·g -1 、0.5A·g -1 、1A·g -1 、2A·g -1 、5A·g -1 And 10 A.g -1 Is maintained at 362 mAh.g at a current density of (C) -1 、346mAh·g -1 、322mAh·g -1 、299mAh·g -1 、266mAh·g -1 、212mAh·g -1 And 150 mAh.g -1 When the current density is returned to 0.10.1A g -1 When the specific discharge capacity was recovered to 346 mAh.g -1 . Compared with pure-phase FeTe, the reduced graphene oxide loaded FeTe composite material has more excellent rate capability.
Example 2
Mixing 20mL of deionized water with 20mLN, N-dimethylformamide, adding 100mg of reduced graphene oxide, and mixing under the condition of ultrasound to obtain a reduced graphene oxide solution;
0.278g FeSO 4 ·7H 2 O，0.25g K 2 TeO 3 ，0.56g KOH，2g N 2 H 4 ·H 2 Mixing and stirring 0.72g of hexadecyl trimethyl ammonium bromide and the reduced graphene oxide solution for 1h, performing solvothermal reaction at 190 ℃ for 18h, sequentially cooling and centrifuging, washing a solid product obtained by centrifuging with water and N, N-dimethylformamide, and finally drying at 70 ℃ for 12h to obtain a precursor;
and heating the precursor to 650 ℃ at a heating rate of 3 ℃/min in argon atmosphere, and preserving heat for 4 hours to obtain the reduced graphene oxide loaded FeTe composite material (the mass ratio of the reduced graphene oxide to the FeTe nano particles is 0.45:1, and the particle size of the FeTe nano particles is 20-200 nm).
The reduced graphene oxide supported FeTe composite was tested for electrochemical performance according to the test method of example 1, with test results similar to example 1.
Example 3
Mixing 20mL of deionized water with 20mLN, N-dimethylformamide, adding 120mg of reduced graphene oxide, and mixing under the condition of ultrasound to obtain a reduced graphene oxide solution;
0.35g of Fe (C) 5 H 7 O 2 ) 3 、0.22g Na 2 TeO 3 、0.56g KOH、2g N 2 H 4 ·H 2 O and 0.57. 0.57g C 12 H 25 SO 4 Mixing Na and the reduced graphene oxide solution, stirring for 1h, performing solvothermal reaction at 200 ℃ for 20h, sequentially cooling and centrifuging, and adding water and N, N-dimethylformamide to the solid product obtained by centrifugingWashing with amine, and drying at 70 ℃ for 12 hours to obtain a precursor;
and heating the precursor to 620 ℃ at a heating rate of 3 ℃/min in argon atmosphere, and preserving heat for 4 hours to obtain the reduced graphene oxide loaded FeTe composite material (the mass ratio of the reduced graphene oxide to the FeTe nano particles is 0.5:1, and the particle size of the FeTe nano particles is 20-200 nm).
The reduced graphene oxide supported FeTe composite was tested for electrochemical performance according to the test method of example 1, with test results similar to example 1.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. The FeTe composite material loaded by the reduced graphene oxide is characterized by comprising the reduced graphene oxide and FeTe nano-particles loaded on the surface of the reduced graphene oxide;
the mass ratio of the reduced graphene oxide to the FeTe nano-particles is (0.4-0.6): 1.
2. the reduced graphene oxide supported FeTe composite material of claim 1, wherein the FeTe nanoparticles have a particle size of 20-200 nm.
3. The preparation method of the reduced graphene oxide supported FeTe composite material as claimed in claim 1 or 2, which is characterized by comprising the following steps:
mixing an iron source, tellurite, strong alkali, a surfactant and a reduced graphene oxide solution, and performing solvothermal reaction to obtain a precursor;
and calcining the precursor to obtain the reduced graphene oxide loaded FeTe composite material.
4. The method of preparing of claim 3, wherein the iron source comprises a soluble ferric salt;
the tellurite comprises an alkali metal salt of tellurite;
the strong base comprises one or more of hydrazine hydrate, sodium hydroxide and potassium hydroxide;
the surfactant comprises sodium dodecyl sulfate and/or cetyltrimethylammonium bromide.
5. The method of claim 3, wherein the concentration of the reduced graphene oxide solution is 2-3 mg/mL;
the solvent of the reduced graphene oxide solution is a mixed solution of water and N, N-dimethylformamide in a volume ratio of 1:1.
6. The production method according to any one of claims 3 to 5, wherein the mass ratio of reduced graphene oxide in the iron source, tellurite, strong base, surfactant and reduced graphene oxide solution is (10 to 30): (10-30): (30-300): (30-100): (4-15).
7. A process according to claim 3, wherein the solvothermal reaction is carried out at a temperature of 160 to 200 ℃ for a period of 18 to 24 hours.
8. A method of preparation according to claim 3, wherein the calcination is carried out in an inert atmosphere.
9. The method according to claim 3 or 8, wherein the calcination is carried out at 550 to 650 ℃ for 3 to 6 hours.
10. The application of the reduced graphene oxide supported FeTe composite material according to claim 1 or 2 or the reduced graphene oxide supported FeTe composite material prepared by the preparation method according to any one of claims 3 to 9 as an electrode material in a sodium ion battery.
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