CN112794360B - Preparation of nano SnO 2 Method for preparing/GC composite anode material - Google Patents
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Abstract
The invention relates to a method for preparing nano SnO 2 The method for preparing the/GC composite anode material is characterized by comprising the following steps of: a) Dropwise adding the gelatin solution into the tin salt solution and uniformly stirring, then dropwise adding the ammonia water solution until a viscous white solid is generated, and stopping stirring; b) Drying at constant temperature of 80 +/-2 ℃, transferring to a tubular furnace for carbonization heat treatment to prepare a target product SnO 2 a/GC composite material. The advantages are that: preparation of nano SnO by using gelatin and tin salt as raw materials 2 the/GC composite negative electrode material reduces the production cost, simplifies the production process, obtains better cycle stability and rate capability, and is suitable for industrial production.
Description
Technical Field
The invention belongs to the field of lithium ion battery manufacturing, and relates to a method for preparing nano SnO 2 A method for compounding a negative electrode material by adopting/GC (gelatin carbon).
Background
With the improvement of the environmental awareness of people, renewable energy gradually replaces the traditional fossil energy. The lithium ion battery is used as important energy storage equipment, has the advantages of high energy density and power density, high voltage and low cost, greatly improves the universality of the lithium ion battery energy storage equipment, and is widely applied to the fields of portable electronic equipment, wearable flexible equipment, electric vehicles, energy storage power grids and the like. The most widely used current negative electrode material is still graphite, however the relatively low theoretical lithium intercalation capacity (372 mAh/g) and poor rate capability limit its application in commercial energy storage systems. Therefore, in order to improve the capacity, cycle life and cycle stability of lithium ion batteries, it is important to develop new anode materials.
SnO 2 The lithium ion battery cathode material can replace graphite due to the characteristics of high theoretical specific capacity (1492 mAh/g), proper lithium-intercalation voltage platform, rich reserve and low price. However, snO 2 The crystal lattice collapse material has huge volume change in the charging and discharging process, can cause the pulverization of the crystal lattice collapse material, and has poor conductivity, so that poor cycle performance and rate capability are finally caused. In addition, when pure nano SnO is adopted 2 As an electrode material, the material is influenced by small particles and large specific surface area, and is easy to agglomerate into secondary particles with larger sizes, so that the electrochemical performance of the material is greatly influenced. To solve this problem, many researchers have prepared SnO with different nanostructures 2 And by reducing SnO 2 Crystal size and control of framework structure to improve SnO 2 The electrochemical performance of (2). For example, naF is used as a morphology control agent in liu et al, and SnO with a directional cone structure is synthesized by a one-step hydrothermal method 2 The nanoparticle shell hollow sphere serving as a negative electrode material still has a reversible capacity of 758mAh/g after being cycled for 100 times under the current density of 0.1A/g. Wang et al prepared octahedral nano SnO by one-step hydrothermal reaction without surfactant 2 The porous microspheres with self-assembled structures still have a reversible capacity of 690mAh/g after being cycled for 50 times under the current density of 0.5A/g. Although these nano SnO with unique morphological structure 2 The reduction of the capacity can be slowed down, but the SnO can not be fundamentally solved by the pure nanocrystallization and the shape design 2 The mechanical stress caused by the volume change is gradually enhanced along with the increase of the cycle times due to the huge volume change in the cycle process, and finally SnO is caused 2 The structure of (2) collapses and electrochemical performance deteriorates. Aiming at the phenomenon, scientific researchers can not only be used as a support framework of a negative electrode structure by utilizing the carbon material with good conductivity and mechanical property, so that the completeness of the electrode structure is prevented from being damaged by stress extrusion, but also the transfer rate of electrons is enhanced by the good conductivity, so that SnO can be effectively improved 2 Thus, it is proposed to use SnO 2 Preparation of SnO by compounding with carbon material 2 Courtel et al, graphite carbon is used as a carbon source, and nano-SnO is synthesized by using an in-situ polyol microwave-assisted technology 2 the/C composite material still has the capacity of 370mAh/g after being cycled for 100 circles under the current density of 0.2A/g. Such SnO 2 The-carbon recombination method indeed improves SnO 2 The lithium ion battery cathode material has capacity and cycling stability, but the capacity tends to be reduced in a long-term cycling process, and the lithium ion battery cathode material is difficult to be practically applied to industrial production due to complex and complicated synthesis technology. To ensure SnO 2 The industrial production of the/carbon composite cathode material in the lithium ion battery must be adhered to improve SnO with low cost and high efficiency 2 The electrochemical performance of (2). Therefore, there is an urgent need for a low-cost and easy-to-operate SnO 2 A method for preparing the/C composite material.
Disclosure of Invention
In order to overcome the prior artThe invention aims to provide a method for preparing nano SnO 2 The method for the/GC composite cathode material reduces the production cost, simplifies the process and improves the cycle stability and the rate capability of the lithium ion battery cathode material.
In order to realize the purpose, the invention is realized by the following technical scheme:
preparation of nano SnO 2 The method for preparing the/GC composite anode material is characterized by comprising the following steps of:
a) Dropwise adding the gelatin solution into the tin salt solution, uniformly stirring, dropwise adding the ammonia water solution until a viscous white solid is generated, and stopping stirring;
b) Drying at constant temperature of 80 +/-2 ℃, transferring to a tube furnace for carbonization heat treatment to prepare a target product SnO 2 a/GC composite material.
Respectively adding gelatin solutions with different volumes into the tin salt solution according to the step a) and the step b), and regulating and controlling the mass ratio of the tin salt to the gelatin in the precursor composite material to obtain different SnO 2 a/GC composite material.
The precipitator is ammonia solution.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts gelatin and tin salt as raw materials to prepare nano SnO 2 the/GC composite negative electrode material reduces the production cost, simplifies the production process, obtains better cycle stability and rate capability, and is suitable for industrial production. Gelatin is a linear polypeptide compound consisting of 18 amino acids, has the characteristics of low price, good biocompatibility and easy commercialization, has stronger physicochemical action with most compounds, and the synthesized material has better flexibility and mechanical property. The invention adopts the sol-gel method which can be amplified in the laboratory to prepare the composite material, the method has simple working procedure and convenient operation, and the prepared nano SnO with a small amount of mesopores 2 The gelatin-carbon composite material has better circulation stability and rate capability, greatly improves the electrochemical performance of the material, and is also suitable for the Sol-Gel method which takes gelatin as a carbon source for coatingAnd (c) an oxide of another metal.
Drawings
FIG. 1 is a process flow diagram of the first embodiment.
FIG. 2 shows GC (gelatin carbon) and SnO 2 And SnO in different mass ratios 2 XRD pattern of/GC (gelatin carbon) composite.
In FIG. 3, (a) to (c) are SnO, respectively 2 /GC-15、SnO 2 (iv) GC-40 and SnO 2 TG/DTG plot of the/GC-90 composite; in FIG. 3, (d) is SnO 2 /GC-15、SnO 2 (ii) GC-40 and SnO 2 Summary of the/GC-90 composite TG.
In FIG. 4, (a) and (b) are nano SnO 2 SEM images of the particles; FIGS. 4 (c) and (d) are SnO 2 SEM image of/GC-40 composite material.
FIG. 5 (a) is SnO 2 SEM image of/GC-40 composite material; in FIG. 5, (b) to (f) are SnO 2 EDS scanning of C, N, O, sn element of/GC-40 composite and its surface element semi-quantitative analysis chart.
In FIG. 6, (a) is SnO 2 XPS survey of the/GC-40 composite; (b) is XPS fine spectrum of C1 s; (c) is XPS fine spectrum of Sn3 d; (d) XPS Fine Spectroscopy (SnO) for N1s 2 /GC-40)。
FIG. 7 shows that the BJH method calculates SnO 2 /GC-15、SnO 2 (iv) GC-40 and SnO 2 Pore size distribution curve diagram of the/GC-90 composite material; fig. 7 (a) is an overall graph; fig. 7 (b) is a partial graph.
FIG. 8 (a) is SnO at a current density of 0.1A/g 2 、GC、SnO 2 /GC-15、SnO 2 (ii) GC-40 and SnO 2 A cycle capacity plot for the/GC-90 composite; (b) Is SnO at current densities of 0.1A/g,0.2A/g,0.5A/g,1A/g,2A/g and 0.1A/g 2 、SnO 2 /GC-15、SnO 2 (ii) GC-40 and SnO 2 Magnification diagram of the/GC-90 composite material, (c) is SnO at a current density of 0.1A/g 2 Long cycle capacity plot of the/GC-40 composite.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings, but it should be noted that the present invention is not limited to the following embodiments.
Preparation of nano SnO 2 The method for preparing the/GC composite anode material comprises the following steps:
1.SnO 2 preparation of nanospheres
a, dropwise adding a precipitator into a tin salt solution until the pH of the solution is =6 to obtain a milky precipitate, and centrifugally washing for multiple times to obtain SnO 2 The precursor solid powder of (4);
b, after drying treatment, carbonizing for 3 hours in an air atmosphere at 500 ℃, cooling, collecting a sample, and sealing and storing;
2.SnO 2 preparation of a/GC composite
a, dropwise adding a gelatin solution into a tin salt solution, uniformly stirring, dropwise adding an ammonia water solution until a viscous white solid is generated, and stopping stirring;
b drying at the constant temperature of 80 +/-2 ℃, transferring to a tubular furnace for carbonization heat treatment to prepare a target product SnO 2 a/GC composite material.
c, according to the step a and the step b, gelatin solutions with different volumes are respectively added into the tin salt solution, and different SnO is obtained by regulating and controlling the mass ratio of the tin salt and the gelatin in the precursor composite material 2 a/GC composite material.
Example one
(1)SnO 2 Preparation of nanospheres
Adding 10mmol SnCl 4 ·5H 2 Dissolving O (0.3506 g) in 40mL of deionized water to obtain a solution A, then dropwise adding 4mol/L ammonia water solution while stirring until the pH of the solution is about 6, continuously stirring for 1 hour to obtain a milky white precipitate, and respectively centrifugally cleaning with deionized water and absolute ethyl alcohol for three times to obtain SnO 2 And (3) nanoparticles. Drying at 80 deg.C for 12h, carbonizing at 500 deg.C in air atmosphere for 3h, cooling, and collecting SnO 2 And (4) sealing and storing the nanoparticles.
(2)SnO 2 Preparation of a/GC composite
Dissolving 10g of gelatin in 100ml of deionized water, magnetically stirring for 1h to fully swell gelatin particles, transferring the gelatin particles to a water bath, and magnetically stirring at 80 ℃ to obtain a light yellow gelatin solution B. Then 10mmol SnCl 4 ·5H 2 O (0.3506 g) dissolved in 40mL to removeAnd (3) obtaining a colorless and clear tin salt solution C after 1 hour in the son water, respectively dropwise adding 15mL, 40mL and 90mL of gelatin B into the solution C, fully stirring for 30 minutes, then dropwise adding 4mol/L ammonia water solution until the pH of the solution is about 7, stirring at the constant temperature of 60 ℃ until the solution is milky viscous liquid, stopping heating, and cooling to obtain a gel white solid. Drying at 80 deg.C for 16h, grinding into powder, transferring into crucible, and placing in tube furnace N 2 Heating at 500 deg.C for 3h in atmosphere, and cooling to room temperature to obtain SnO 2 the/GC composite material is named SnO according to the volume amount of dropwise added gelatin 2 /GC-15、SnO 2 /GC-40、SnO 2 and/GC-90. For comparison, the cooled gelatin solution was also subjected to the same drying and carbonization treatments, and the obtained gelatin carbon sample was named GC. Finally, the lithium ion battery cathode material is used as a lithium ion battery cathode material to assemble a button battery and the electrochemical performance of the button battery is tested.
FIG. 2 shows GC (gelatin carbon), snO 2 And SnO in different mass ratios 2 XRD pattern of/GC (gelatin carbon) composite. SnO 2 The lattice parameters corresponding to the diffraction peaks are respectively
P42/mnm space group, and has four strong diffraction peaks at 2 theta =27 °, 34 °, 38 ° and 52 °, corresponding to SnO 2 The (110), (101), (200) and (211) crystal planes of (A) and (B), which are similar to those of SnO with a tetragonal rutile structure 2 Standard card consensus (ICOD 01-077-0448). But in SnO 2 No SnO was observed in XRD pattern of/GC composite material 2 May be such that SnO is not formed in the composite material 2 Yet another result may be the formation of SnO within the composite material 2 However, snO 2 Is amorphous and therefore does not show characteristic peaks.
From FIG. 3 (d), snO 2 /GC-15、SnO 2 (ii) GC-40 and SnO 2 The carbon content in the/GC-90 composite was 62.0%, 68.2% and 74.2%, respectively.
As shown in FIG. 4 (a), nano SnO with an amplification of 10KX 2 The particles are significantly agglomerated into large clusters. SnO for more intuitive observation 2 The microstructure of (a) is enlarged by 50KX SnO 2 The SEM image shows that the nano SnO 2 The particles are spherical, and the particle size range is 10-20 nm. Furthermore, as shown in FIGS. 4 (c) and (d), it is shown that SnO is more simple than SnO 2 Spherical nano particles, the microscopic appearance of the composite material is greatly changed, snO 2 Is completely wrapped by gelatin, has irregular block structure and smooth surface
As can be seen from FIG. 5, the signals of carbon element in gelatin and oxygen and tin element from tin dioxide are uniformly overlapped on the whole particle surface, which shows that the carbon layer is uniformly coated on SnO 2 The surface of the nanoparticles. The semi-quantitative analysis of each element is shown in table 1.
TABLE 1 semi-quantitative analysis table for each element of Map
As shown in FIG. 6 (a), snO 2 the/GC-40 composite material contains four elements of Sn, O, C and N. FIGS. 6 (b) - (d) are XPS high resolution fine spectra of Sn3d, C1s and N1s, respectively, and from the Sn3d spectrum of FIG. 6 (b), it is clear that the bonding energies of Sn3d5/2 and Sn3d3/2 are 487.02eV and 495.45eV, respectively, and the bonding energy difference between them is 8.47eV, and SnO 2 The peak value of the spin orbit is consistent, and the Sn element is proved to be Sn 4+ In ionic form. FIG. 6 (C) shows the C1s peak split into four types of carbon, with the peak at 284.66eV being sp for a C-C single bond 2 Graphitic hybrid carbon, the peak at 285.65eV belongs to sp of a C-O single bond 3 Diamond-like hybrid carbon, peaks at 287.8eV and 288.95eV correspond to carbon of C = O bond and C-O bond, respectively. The high resolution N1s peak of FIG. 6 (d) has four compositions with binding energies at 398.64eV, 400.0eV, 401.07eV, and 403.22eV, respectively, corresponding to 42.45wt% pyridine nitrogen, 13.77wt% nitro nitrogen, 26.72wt% pyrrole nitrogen, and 17.06wt% tetravalent nitrogen, respectively, and thus it can be seen that the main forms of nitrogen present in the carbon layers are pyridine nitrogen and pyrrole nitrogen.
As shown in FIG. 7, snO 2 -GC-15、SnO 2 -GC-40 and SnO 2 The specific surface areas of the-GC-90 samples are 4.879 respectively 2 /g、34.567m 2 /g and 2.642m 2 The pore size distribution is mostly concentrated between 3 and 12nm, indicating SnO 2 Most of samples obtained by mixing with the gelatin have mesoporous structures, which are related to the physicochemical properties of the gelatin.
Referring to FIG. 8 (a), after 100 times of charge and discharge, GC and SnO 2 The lithium storage capacities of the lithium batteries are respectively 111.9mAh/g and 57.8mAh/g, and SnO 2 -GC-15、SnO 2 -GC-40 and SnO 2 The lithium storage capacity of the-GC-90 sample was 321.9mAh/g, 353.6mAh/g, and 307.9mAh/g, respectively. Comparison found SnO 2 Lithium storage capacity ratio of/GC composite material of pure GC and SnO 2 The carbon coating can effectively relieve SnO 2 Structural stress generated by huge volume change in the charge-discharge cycle process stabilizes the lattice structure of the material and hinders the collapse of the lattice structure. See FIG. 8 (b), snO after 100 cycles at current densities of 0.1A/g,0.2A/g,0.5A/g,1A/g,2A/g, respectively 2 The lithium storage capacity performance of the/GC-40 is best shown and is respectively 379.2mAh/g, 298.3mAh/g, 206.8mAh/g, 135.3mAh/g and 61.1mAh/g, and when the current density returns to 0.1A/g again, snO 2 the/GC-40 still has a lithium storage capacity of 385.3 mAh/g. While SnO 2 、SnO 2 /GC-15、SnO 2 The results of the lithium storage capacities shown by/GC-90 were 50.5mAh/g, 274.6mAh/g, and 322.6mAh/g, respectively, and they showed that SnO 2 Relative to SnO in/GC-40 2 、SnO 2 (ii) GC-15 and SnO 2 the/GC-90 has better rate performance. FIG. 8 (c) is SnO after 500 cycles of charge-discharge cycle 2 the/GC-40 sample still had a lithium storage capacity of 397mAh/g, which further indicates that SnO 2 the/GC-40 composite material has excellent electrochemical stability. Simultaneously, snO is increased along with the increase of the number of cycles 2 The lithium storage capacity of the/GC-40 sample decreased first and then increased.
The invention takes GC as a carbon source and adopts a one-pot Sol-Gel (Sol-Gel) method to treat nano SnO 2 Carrying out carbon coating in-situ to generate a tin salt/GC composite precursor, and then carrying out high-temperature calcination to obtain porous SnO 2 a/GC composite material. Meanwhile, the electrochemical performance of the composite material is further optimized by regulating and controlling the mass ratio of tin salt to GC in the precursor composite material.
Claims (1)
1. Preparation of nano SnO 2 The method for preparing the/GC composite anode material is characterized by comprising the following steps of:
a) Respectively dropwise adding 15mL, 40mL and 90mL of 0.1 g/mL gelatin solution into 40mL of 0.25 mmol/mL tin salt solution, uniformly stirring, dropwise adding 4mol/L ammonia water solution until a viscous white solid is generated, and stopping stirring;
b) Drying at constant temperature of 80 +/-2 ℃, transferring to a tube furnace for carbonization heat treatment to prepare a target product SnO 2 a/GC composite;
the carbonization heat treatment is carried out in N 2 Heating at 500 deg.C for 3h; said SnO 2 SnO in/GC composites 2 Is an amorphous structure.
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