CN115732658A - Silicon/carbon anode material with nano-pore structure and preparation method thereof - Google Patents
Silicon/carbon anode material with nano-pore structure and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a silicon/carbon anode material with a nano-pore structure and a preparation method thereof, belonging to the technical field of lithium batteries. The method is to accurately deposit Al with different thicknesses on the surface of a nano-scale Si anode material by an atomic layer deposition technology 2 O 3 As a void template, then Si @ Al by conventional chemical polymerization 2 O 3 The polydopamine with a certain thickness is deposited on the surface, and then the subsequent annealing treatment and acid-washing template treatment are carried outAnd preparing the Si @ void @ C composite negative electrode material. The template can synchronously regulate and control the thickness of the carbon coating layer and the size of the nanometer gap, and Al with different thicknesses is coated 2 O 3 The layers on the one hand produce void structures of different sizes to buffer the huge volume expansion of the Si material and form a stable SEI layer, and on the other hand the added Al 2 O 3 The thickness of the carbon coating layer can be regulated by inhibiting the polymerization rate of dopamine, and the silicon content in a sample can be further regulated, so that the silicon/carbon composite negative electrode material with extremely high silicon content, higher capacity retention rate and good cycle stability can be prepared. Meanwhile, the overall conductivity of the electrode material and the transmission rate of lithium ions and electrons are improved, so that the cycle stability and the cycle life of the battery are improved, and the lithium storage performance with high capacity, long service life and rate performance is realized.
Description
Technical Field
The invention relates to the technical field of lithium ion battery cathode materials, in particular to a silicon/carbon cathode material capable of synchronously regulating and controlling the thickness of a carbon coating layer and a nanometer gap and a preparation method thereof.
Background
The lithium ion battery has the advantages of high battery voltage, high charge and discharge rate, high specific energy, no memory effect, long service life, less environmental pollution and the like, so that the lithium ion battery becomes an important device for storing and converting energy and is a good choice for developing novel power automobiles. However, the theoretical specific capacity of the graphite widely used as the cathode material of the commercial lithium ion battery at present is only 372mAh/g which is relatively low, and the demand of further development of the lithium ion battery cannot be met. While low cost silicon has its extremely high theoretical capacity (4200 mA g) -1 ) And lower operating voltages are considered key negative electrode materials for the development of next generation high energy density lithium ion batteries.
However, the silicon negative electrode material undergoes a large volume change (> 300%) in the process of lithium intercalation and deintercalation, which results in the collapse of the structure and the differentiation of the electrode, and the active material and the current collector lose electric contact, thereby causing the rapid attenuation of the electrochemical performance. At the same time, silicon, as a semiconductor material, has inherently poor electron conductivity and Li + The conductivity will be furtherIncreasing electrochemical polarization during discharge/charge and significantly reducing its rate capability at high current densities.
Aiming at the problems of the silicon negative electrode material, the method for preparing the porous silicon-carbon composite material is mainly adopted at present. Patent CN108682817A discloses a preparation method of a porous silicon carbon negative electrode material for a lithium ion battery. The porous silicon-carbon composite material is mainly prepared by thermally reducing silicon dioxide, then carrying out acid cleaning to obtain porous silicon, then combining with a carbon source solution through vacuum absorption, and finally carbonizing at high temperature. However, when the lithium ion battery is applied to the lithium ion battery, although the stability is good, the specific capacity is low, and the practical application cannot be met.
Patent CN113851627A discloses a porous silicon carbon negative electrode material and a preparation method thereof. It mainly adopts several carbon sources with different properties to compound in stages and control the heat treatment temperature, so as to form pores with certain size in the material. Although the specific capacity and the first coulombic efficiency of the porous silicon-carbon composite material prepared by the method are improved, the aperture size of the porous silicon-carbon composite material is difficult to accurately control, and the consistency of the material is poor.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of a silicon/carbon anode material capable of synchronously regulating and controlling the thickness of a carbon coating layer and the size of a nanometer gap by combining the characteristics of an Atomic Layer Deposition (ALD) technology. The method creatively provides a method for rapidly and controllably growing a low-cost template in the nano-scale silicon-carbon composite anode material by utilizing an atomic layer deposition technology, so that the accurate regulation and control of the nano-void structure and the size in the nano-scale silicon-carbon composite anode material are realized, and the synchronous regulation and control of the thickness of a carbon coating layer are realized, so that the porous silicon-carbon composite anode material with high capacity, long service life and high multiplying power is prepared.
The invention is realized by the following technical scheme:
a silicon/carbon cathode material for synchronously regulating and controlling the thickness of a carbon coating layer and the size of a nanometer gap and a preparation method thereof comprise the following steps:
(1) Accurately depositing Al with certain thickness on the surface of the silicon powder by adopting an atomic layer deposition technology 2 O 3 As a void formerA plate;
(2) Reacting Si @ Al 2 O 3 Dispersing powder and tris (hydroxymethyl) aminomethane in deionized water solution, adjusting pH with dilute hydrochloric acid, adding dopamine, stirring for 20-30 hr under Si @ Al 2 O 3 The surface of the powder is deposited with polydopamine with a certain thickness by using a traditional chemical polymerization method;
(3) p-Si @ Al 2 O 3 The @ PDA is carbonized at high temperature in argon-hydrogen mixed atmosphere to convert into Si @ Al 2 O 3 @C；
(4) Cleaning Si @ Al with excess dilute hydrochloric acid solution 2 O 3 Al in @ C 2 O 3 And (3) forming a template to obtain the Si @ void @ C composite negative electrode material with the nano voids.
Preferably, in the step (1), the silicon powder has a purity of 99.9% and a particle size of 50 to 200nm.
Preferably, in step (1), the Al is 2 O 3 The deposition thickness of (2) to (20) nm.
Preferably, in step (2), si @ Al 2 O 3 The adding amount ratio of the powder, the trihydroxymethyl aminomethane, the deionized water and the dopamine is (0.1-0.5) g, (0.5-1) g, (50-200) mL and (0.1-1) g.
Preferably, the pH in step (2) is adjusted to 8.0-9.0 with dilute hydrochloric acid.
Preferably, in the step (3), the carbonization temperature is 600-800 ℃, and the carbonization time is 2-4 h.
Preferably, the carbonized carbon layer has a thickness of 5 to 20nm.
Preferably, in the step (4), the concentration of the dilute hydrochloric acid is 0.1 to 0.2 mol.L -1 The acid treatment time is 10-30 h.
The silicon content in the Si @ void @ C composite negative electrode material is 80-95%.
The beneficial effects of the invention are as follows:
1. the invention creatively utilizes the advantages of uniform and complete coating and accurate and controllable thickness of the atomic layer deposition technology, prepares a template with controllable thickness and complete appearance on the surface of the nano-scale silicon material to regulate and control the nano-void structure in the Si @ void @ C cathode material, and obtains the cathode material with high silicon density content, wherein the silicon content reaches 80-95%. During the cycling process, due to the proper void space between the silicon core and the outer carbon shell, the volume expansion of silicon can be adapted and a solid electrolyte layer (SEI) with controllable thickness and uniform components can be formed, thereby improving the cycling stability and the cycle life of the battery.
2. The invention takes polydopamine as a carbon source and introduces a polymer coating method on Si @ Al 2 O 3 Carbon coating is carried out on the template, the carbon coating layer increases the conductivity of the Si @ void @ C material, improves the overall conductivity of the electrode material and the transmission rate of lithium ions and electrons, and is used as a buffer layer to relieve the stress released by the silicon material due to volume expansion. Thereby prepare Si @ void @ C composite anode material with high capacity, long life and high multiplying power, thereby realized the lithium storage performance that high capacity, long life, multiplying power performance compromise.
3. The preparation method of the nanometer gap template is simple, easy to operate and low in cost, and meanwhile, the nanometer gap structure can be introduced into the one-dimensional/two-dimensional/three-dimensional silicon-carbon cathode material by utilizing technical integration, and more importantly, deposited Al 2 O 3 The template can synchronously regulate and control the thickness of a carbon coating layer taking polydopamine as a precursor and the size of a nanometer gap, and Al is deposited 2 O 3 The pH value of the Si material in the dopamine polymerization process is compared with that of the uncoated Al 2 O 3 The Si material is obviously improved, so that the polymerization rate of dopamine is inhibited, the coating thickness is thinner, the silicon density of the obtained cathode material is higher, and meanwhile, al can be adjusted 2 O 3 The cladding thickness of the layer regulates the void size.
Drawings
FIG. 1 is an XRD pattern of a composite material of pure silicon powder, si @ C, si @ void @ C-1, si @ void @ C-2 and Si @ void @ C-3.
FIG. 2 shows TEM spectra of Si @ void @ C-1 (a), si @ void @ C-2 (b-c), and Si @ void @ C-3 (d).
FIG. 3 shows Si @ void @ C-2 at 0.2A g -1 Charge and discharge curves at current density.
FIG. 4 shows Si and example in comparative example 2Si @ Al in example 2 2 O 3 PH change during dopamine polymerization.
Detailed Description
In order to make the present invention more clear, the present invention is described in further detail below with reference to the accompanying drawings and examples.
Example 1
The preparation method of Si @ void @ C-1 comprises the following steps:
(1) Depositing Al with the thickness of 4nm on the surface of the silicon powder by an atomic layer deposition technology 2 O 3 A coating layer;
(2) 0.2g of Si @ Al 2 O 3 The powder and 0.6g of tris (hydroxymethyl) aminomethane were dispersed in 100mL of deionized water and the amount of the dispersion was adjusted to 0.1 mol. L -1 Adjusting pH to 8.5 with dilute hydrochloric acid, adding 0.1g dopamine, stirring for 24 hr to obtain Si @ Al 2 O 3 The @ PDA solution is centrifuged again, washed with deionized water and ethanol for several times, and vacuum dried at 60 deg.C for 12h to obtain Si @ Al 2 O 3 @ PDA powder;
(3) Reacting Si @ Al 2 O 3 Heating the @ PDA powder to 700 ℃ at a heating rate of 5 ℃/min in argon-hydrogen mixed reducing gas, and keeping the temperature for 3h to obtain Si @ Al 2 O 3 The material @ C;
(5) The obtained Si @ Al 2 O 3 @ C in 0.1 mol. L -1 After acid treatment for 24 hours, the Si @ void @ C-1 composite material can be obtained after centrifugation, washing and drying.
XRD analysis was performed on the silicon-carbon composite material with a void structure prepared in this example, and the obtained XRD pattern is shown in FIG. 1. As can be seen from FIG. 1, the characteristic peak of Si @ void @ C-1 material is well matched with that of pure Si, and no impurity peak appears, which indicates that the synthesized material has high purity. Meanwhile, the existence of the Si phase and the C phase in the composite material indicates that the polydopamine-derived carbon layer is successfully coated. The composite material obtained contained 91.36% of silicon and 15.5nm of carbon layer thickness.
Example 2
The preparation method of Si @ void @ C-2 comprises the following steps:
(1) Depositing Al with the thickness of 8nm on the surface of the silicon powder by an atomic layer deposition technology 2 O 3 A coating layer;
(2) 0.2g of Si @ Al 2 O 3 The powder and 0.6g of tris (hydroxymethyl) aminomethane were dispersed in 100mL of deionized water and the amount of the dispersion was adjusted to 0.1 mol. L -1 Adjusting pH to 8.5 with dilute hydrochloric acid, adding 0.1g dopamine, stirring for 24 hr to obtain Si @ Al 2 O 3 Subjecting to centrifugal treatment, washing with deionized water and ethanol for several times, and vacuum drying at 60 deg.C for 12 hr to obtain Si @ Al 2 O 3 @ PDA powder;
(3) Mixing Si @ Al 2 O 3 Heating the @ PDA powder to 700 ℃ at a heating rate of 5 ℃/min in argon-hydrogen mixed reducing gas, and preserving the temperature for 3h to obtain Si @ Al 2 O 3 The material @ C;
(5) The obtained Si @ Al 2 O 3 @ C is dispersed in 0.1 mol. L -1 After acid treatment for 24 hours in dilute hydrochloric acid, the Si @ void @ C-2 composite material can be obtained after centrifugation, washing and drying.
XRD analysis is carried out on the silicon-carbon composite material with the void structure prepared in the embodiment, and the result also shows that the Si @ void @ C-2 composite material is high in purity and has two phases of Si and C. The composite material obtained contained 89.25% of silicon and 7.8nm of carbon layer thickness.
Example 3
The preparation method of Si @ void @ C-3 comprises the following steps:
(1) Depositing Al with the thickness of 16nm on the surface of the silicon powder by an atomic layer deposition technology 2 O 3 A coating layer;
(2) 0.2g of Si @ Al 2 O 3 The powder and 0.6g of tris (hydroxymethyl) aminomethane were dispersed in 100mL of deionized water and the amount of the dispersion was adjusted to 0.1 mol. L -1 Adjusting pH to 8.5 with dilute hydrochloric acid, adding 0.1g dopamine, stirring for 24 hr to obtain Si @ Al 2 O 3 The @ PDA solution is centrifuged again, washed with deionized water and ethanol for several times, and vacuum dried at 60 deg.C for 12h to obtain Si @ Al 2 O 3 @ PDA powder;
(3) Mixing Si @ Al 2 O 3 Heating the @ PDA powder to 700 ℃ at a heating rate of 5 ℃/min in argon-hydrogen mixed reducing gas, and preserving the temperature for 3h to obtain Si @ Al 2 O 3 The material @ C;
(5) The obtained Si @ Al 2 O 3 @ C in 0.1 mol. L -1 After acid treatment for 24 hours in dilute hydrochloric acid, the Si @ void @ C-3 composite material can be obtained after centrifugation, washing and drying.
XRD analysis is carried out on the silicon-carbon composite material with the void structure prepared in the embodiment, and the result also shows that the Si @ void @ C-3 composite material is high in purity and has two phases of Si and C. The composite material obtained contained 73.61% of silicon and 5.5nm of carbon layer thickness.
Example 4
Preparation of Si @ void @ C-4, comprising the following steps:
(1) Depositing Al with the thickness of 8nm on the surface of the silicon powder by an atomic layer deposition technology 2 O 3 A coating layer;
(2) 0.2g of Si @ Al 2 O 3 The powder and 0.6g of tris (hydroxymethyl) aminomethane were dispersed in 100mL of deionized water and the amount of the dispersion was adjusted to 0.1 mol. L -1 Adjusting pH to 9.0 with dilute hydrochloric acid, adding 0.1g dopamine, stirring for 24 hr to obtain Si @ Al 2 O 3 The @ PDA solution is centrifuged again, washed with deionized water and ethanol for several times, and vacuum dried at 60 deg.C for 12h to obtain Si @ Al 2 O 3 @ PDA powder;
(3) Mixing Si @ Al 2 O 3 Heating the @ PDA powder to 700 ℃ at a heating rate of 5 ℃/min in argon-hydrogen mixed reducing gas, and keeping the temperature for 3h to obtain Si @ Al 2 O 3 The material @ C;
(5) The obtained Si @ Al 2 O 3 @ C in 0.1 mol. L -1 After acid treatment for 24 hours, the Si @ void @ C-4 composite material can be obtained after centrifugation, washing and drying.
XRD analysis is carried out on the silicon-carbon composite material with the void structure, and the result also shows that the Si @ void @ C-4 composite material is high in purity and has two phases of Si and C. The composite material obtained contained 89.25% of silicon and 4.2nm of carbon layer thickness.
Comparative example 1
The comparative example uses silicon powder as a raw material, and obtains a Si material without any treatment.
Comparative example 2
Preparation of Si @ C, comprising the following steps:
(1) 0.2g of Si powder and 0.6g of tris (hydroxymethyl) aminomethane were dispersed in 100mL of deionized water, and the solution was washed with 0.1 mol. L -1 Adjusting pH to 8.5 with dilute hydrochloric acid, adding 0.1g dopamine, stirring for 24h to obtain Si @ PDA solution, centrifuging, washing with deionized water and ethanol alternately for multiple times, and vacuum drying at 60 deg.C for 12h to obtain Si @ PDA powder;
(2) Heating Si @ PDA powder to 700 ℃ at a heating rate of 5 ℃/min in argon-hydrogen mixed reducing gas, and preserving heat for 3h to obtain Si @ C powder;
(3) And (3) carrying out centrifugal treatment on the obtained Si @ C, alternately washing the obtained Si @ C by using deionized water and ethanol for multiple times, and carrying out vacuum drying at the temperature of 60 ℃ for 12 hours to obtain the Si @ C composite material. The composite material obtained contained 56.57% of silicon and 22.6nm of carbon layer thickness.
Comparative example 3: the preparation method is the same as example 2, except for the steps of: (1) Depositing SiO with the thickness of 8nm on the surface of silicon powder by an atomic layer deposition technology 2 A coating layer; to obtain Si @ void @ C-Si composite material. The composite material obtained contained 69.85% of silicon and 17.3nm of carbon layer thickness.
And (3) electrochemical performance testing:
the materials prepared in the examples 1 to 4 and the comparative examples 1 to 3 are respectively made into negative electrodes, and assembled into batteries, and the cycle performance of the batteries is tested by the following specific method: and adding deionized water into the silicon-carbon negative electrode material, the conductive carbon black and the binder (sodium carboxymethyl cellulose (CMC)) prepared in each embodiment and each proportion according to the mass ratio of 70: 15, mixing, stirring to obtain slurry, coating the slurry on a current collector copper foil, and drying in a vacuum drying oven at 60 ℃ for 12 hours to prepare the negative electrode plate. The metal lithium sheet is used as a counter electrode, the PP/PE/PP type composite membrane is used as a diaphragm, and the composite membrane contains 1mol/L LiPF 6 Electrolyte and addition of 10vol.% of fluoroethylene carbonateAn Ethylene Carbonate (EC)/diethyl carbonate (DEC)/dimethyl carbonate (DMC) (volume ratio 1: 1) solution of ester (FEC) and 2vol.% Vinylene Carbonate (VC) was used as an electrolyte, and the negative plate was placed in a glove box filled with argon gas to make a CR2032 type button cell. The prepared battery was subjected to 100 cycles at a current density of 0.2A/g, and the initial specific discharge capacity and the specific discharge capacities after 50 and 100 cycles were measured, as shown in table 1 below.
Table 1 cycle performance of the composite material of the present invention applied to a battery
Wherein, the cycle performance graphs of examples 1-3 and comparative examples 1 and 2 are shown in figure 2, wherein Si @ void @ C represents the silicon-carbon composite anode material with the nano-void structure obtained by the treatment of the invention; si represents the untreated negative electrode material in the comparative example 2, and as can be seen from figure 2 and table 1, after the Si @ void @ C negative electrode material prepared by the invention is manufactured into a button cell, the reversible capacity of above 983.43mAh/g can still be achieved after 100 cycles, especially, the Si @ void @ C-2 negative electrode material has higher reversible capacity of 1712.79mAh/g after 100 cycles, and the capacity retention rate is 54.5%. The Si cathode material which is not processed by the method has the capacity of 1178.97mAh/g after being cycled for 50 times, the capacity of 744.36mAh/g is remained after being cycled for 100 times, and the capacity retention rate is only 20.2%. Therefore, the nano-voids manufactured by the method can effectively relieve the huge volume expansion of silicon generated in the charge and discharge process, and improve the cycle stability of the silicon cathode. In general, the silicon-carbon composite anode material with the nano-void structure can still have higher capacity retention rate and good cycle stability under the condition of extremely high silicon content.
Meanwhile, the coating layers with the same thickness are deposited from the example 2 and the comparative example 3, but the silicon content of the composite material prepared by the comparative example 3 is far smaller than that of the example 2, the thickness of the carbon layer is thicker than that of the example 2, and the initial specific discharge capacity of the negative electrode material of the comparative example 3 is smaller than that of the negative electrode material obtained by the example 2The stability is also poor. It can be seen that Si @ Al used in the present invention 2 O 3 The template is different from other inert templates, and the alumina template can regulate and control the pH value in the polymerization process when dopamine is polymerized, so that the excellent template with the thickness of a carbon coating layer taking dopamine as a precursor and the size of a nanometer gap can be synchronously regulated and controlled.
The above description is only a detailed description of the preferred possible embodiments of the present invention, and is not intended to limit the present application, which may be modified and varied by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (7)
1. A preparation method of a silicon/carbon anode material capable of synchronously regulating and controlling the thickness of a carbon coating layer and the size of a nanometer gap comprises the following steps:
(1) Accurately depositing Al with certain thickness on the surface of Si powder by adopting atomic layer deposition technology 2 O 3 As a void template;
(2) Mixing Si @ Al 2 O 3 Dispersing powder and tris (hydroxymethyl) aminomethane in deionized water solution, adjusting pH to 8.0-9.0 with dilute hydrochloric acid, adding dopamine, stirring for 20-40h under Si @ Al 2 O 3 The surface of the powder is deposited with polydopamine with a certain thickness by using a traditional chemical polymerization method;
(3) p-Si @ Al 2 O 3 The @ PDA is carbonized at high temperature in argon-hydrogen mixed atmosphere to convert into Si @ Al 2 O 3 @C；
(4) Washing Si @ Al with excessive dilute hydrochloric acid solution 2 O 3 Al in @ C 2 O 3 The template is adopted to obtain the Si @ void @ C composite negative electrode material with the nanometer gap;
the mass content of silicon in the Si @ void @ C composite negative electrode material is 80-95%.
2. The method of claim 1, wherein: in the step (1), the purity of the silicon powder is 99.9%, and the particle size is 50-200 nm.
3. The production method according to claim 1, characterized in that: in the step (1), al 2 O 3 The deposition thickness of (2) to (20) nm.
4. The method of claim 1, wherein: in the step (2), si @ Al 2 O 3 The adding amount ratio of the powder, the trihydroxymethyl aminomethane, the deionized water and the dopamine is (0.1-0.5) g, (0.5-1) g, (50-200) mL and (0.1-1) g.
5. The production method according to claim 1, characterized in that: in the step (3), the carbonization temperature is 600-800 ℃, the carbonization time is 2-6 h, and the thickness of the carbonized carbon layer is 5-20nm.
6. The method of claim 1, wherein: in the step (4), the concentration of the dilute hydrochloric acid is 0.1-0.2 mol.L -1 The acid treatment time is 10-30 h.
7. A silicon/carbon anode material with a nano-void structure prepared by the preparation method of claims 1-6.
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| CN117894968A (en) * | 2024-03-15 | 2024-04-16 | 葫芦岛市铭浩新能源材料有限公司 | Doped coated spherical silicon-carbon anode material, and preparation method and application thereof |
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| CN117894968B (en) * | 2024-03-15 | 2024-05-14 | 葫芦岛市铭浩新能源材料有限公司 | Doped coated spherical silicon-carbon anode material, and preparation method and application thereof |
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