CN108390028B - Silicon-alkene/carbon composite negative electrode material and preparation method thereof - Google Patents
Silicon-alkene/carbon composite negative electrode material and preparation method thereof Download PDFInfo
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- CN108390028B CN108390028B CN201810064192.0A CN201810064192A CN108390028B CN 108390028 B CN108390028 B CN 108390028B CN 201810064192 A CN201810064192 A CN 201810064192A CN 108390028 B CN108390028 B CN 108390028B
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Abstract
The invention provides a silylene/carbon composite negative electrode material and a preparation method thereof. The composite anode material comprises a spherical amorphous carbon matrix, and silylene and conductive particles which are dispersed in the carbon matrix. The preparation method of the composite anode material comprises the following steps: mixing silylene, conductive particles and a carbon source in a solvent to obtain slurry; spray drying the slurry to obtain a silylene/carbon spherical precursor; and carbonizing the precursor in a non-oxidizing atmosphere to obtain the silylene/carbon composite negative electrode material. The silicon alkene/carbon composite cathode material provided by the invention has the advantages of high energy density, proper specific surface area, high first coulombic efficiency, excellent cycle performance and rate capability, and good application prospect.
Description
Technical Field
The invention relates to the technical field of lithium battery cathode materials, in particular to a silylene/carbon composite cathode material and a preparation method thereof.
Background
The current commercialized lithium ion battery cathode material mainly uses graphite, the theoretical specific capacity of the material is only 372mAh/g, and the material far cannot meet the increasing demand of the market for high-energy density lithium ion batteries. The theoretical capacity of the simple substance silicon reaches 4200mAh/g, which is almost 11 times of graphite, and the silicon has a higher charging and discharging platform, which can avoid the precipitation of the simple substance lithium on the negative pole, thus having higher safety performance. However, the silicon negative electrode has several problems: 1. during the charging and discharging processes, the volume expansion of 300-400% exists, so that the active substance is pulverized and loses electric contact, and the capacity is rapidly attenuated; 2. in the process of charging and discharging, the pulverization of the material exposes a new surface, an SEI film is repeatedly formed, and a large amount of lithium ions are consumed, so that the charging and discharging efficiency of the material is low and the cycle life is poor; 3. elemental silicon has very low conductivity.
The application of silicon negative electrodes to lithium ion batteries is hindered by the existence of the above problems, and in recent years, silicon nanocrystallization and silicon-carbon composite technologies have become the most effective approaches to solve the above problems.
CN104143629A discloses a preparation method of a Si/C/graphite negative electrode material, which comprises the following steps: preparing nano silicon slurry by taking micron silicon as a raw material, coating silicon particles on the surface of graphite by spray drying, and finally carbonizing to obtain the silicon-carbon composite material. The material takes graphite as a matrix to buffer the volume expansion of silicon, but the effect is very limited, and the capacity fading speed is high.
CN106067547A discloses a method for preparing a silicon-carbon negative electrode material, in which carbon-coated silicon particles are dispersed in graphene to form spherical particles, and a pyrolytic carbon layer is coated on the surface of the spherical particles. The graphene not only plays a role of a conductive network, but also plays a role of a support frame, the volume expansion in the charge and discharge process is greatly reduced due to the structure of the graphene and the double-layer carbon layer, and the material has higher electrical property. However, the method does not completely solve the problem of volume expansion of silicon itself, and thus the cycle performance of the method is far from the cycle performance of graphite.
CN160532047A discloses a silicon-carbon composite material prepared by simultaneously generating silicon and graphene from silicon and graphite raw materials by a mechanical stripping method. The material takes the silylene with small volume effect as a raw material, solves the problem of volume expansion of silicon, has the cycle life of more than 1000 times, and has the advantages of low resistance, high capacity and the like. But the method has low production efficiency, and the material has the defect of overlarge specific surface area, so that the first effect is low.
Therefore, the technical problems of the silicon-carbon composite anode material at present are not completely solved.
Disclosure of Invention
Aiming at the technical problems of the silicon-carbon composite negative electrode material in the prior art, the invention provides a silicon-alkene/carbon composite negative electrode material and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
in one aspect, the present invention provides a silylene/carbon composite anode material comprising a spherical amorphous carbon matrix and silylene and conductive particles dispersed in the carbon matrix.
Further, the mass fraction of the spherical amorphous carbon matrix is 60-95%.
More preferably, the mass fraction of the spherical amorphous carbon matrix is 80 to 95%, for example: 80%, 83%, 85%, 87%, 90%, 92%, or 95%, etc.
Further, the mass fraction of the silylene is 1-30%.
Further preferably, the mass fraction of the silylene is 5-10%, for example: 5%, 6%, 7%, 8%, 9% or 10%, etc.
Further, the mass fraction of the conductive particles is 0.5-10%.
Further preferably, the mass fraction of the conductive particles is 1 to 5%, for example: 1%, 2%, 3%, 4% or 5%, etc.
Further, the particle size D50 of the silylene/carbon composite negative electrode material is 1-50 μm.
More preferably, the particle size D50 of the silylene/carbon composite negative electrode material is 5 to 30 μm.
In some embodiments, the particle size D50 of the silylene/carbon composite anode material is 10-30 μm, for example: 10 μm, 12 μm, 16 μm, 17 μm, 19.5 μm, 20 μm, 25 μm, or 30 μm, and the like.
Further, the specific surface area of the silylene/carbon composite negative electrode material is 1-10m2/g。
More preferably, the specific surface area of the silylene/carbon composite negative electrode material is 2-6m2G, for example: 2m2/g、3m2/g、3.6m2/g、4m2/g、5m2G or 6m2G,/g, etc.
Furthermore, the silylene is prepared by adopting a physical vapor deposition or mechanical stripping method. The silicon alkene has a multilayer structure, and the number of layers is 1-300.
In some embodiments, the number of layers of the silylene is 5 to 50, for example: 5. 10, 15, 20, 25, 30, 35, 40, 45 or 50, etc.
Further, the particle diameter D50 of the silylene is 0.01 to 3 μm, and more preferably 0.1 to 3 μm.
In some embodiments, the particle size D50 of the silylene is 0.1 to 1 μm, for example: 0.1 μm, 0.2 μm, 0.4 μm, 0.5 μm, 0.6 μm, 0.7 μm, 0.8 μm, 0.9 μm or 1 μm, etc.
Further, the conductive particles are one or a combination of at least two of acetylene black, conductive carbon black (SP), conductive graphite, carbon nanotubes, copper powder and silver powder.
Further, the conductive particles have a particle diameter D50 of 10 to 500nm, preferably 20 to 100nm, for example: 20nm, 30nm, 40nm, 50nm, 60nm, 70nm, 80nm, 90nm, or 100nm, and the like.
On the other hand, the invention also provides a preparation method of the silylene/carbon composite anode material, which comprises the following steps:
s1: mixing silylene, conductive particles and a carbon source in a solvent to obtain slurry;
s2: spray drying the slurry to obtain a silylene/carbon spherical precursor;
s3: and carbonizing the precursor in a non-oxidizing atmosphere to obtain the silylene/carbon composite negative electrode material.
Further, in step S1, the carbon source is one of pitch, phenolic resin, glucose, sucrose, sodium carboxymethylcellulose, polyvinylpyrrolidone (PVP), polyacrylonitrile, and polyvinyl alcohol, or a combination of at least two of them.
Further, in step S1, the conductive particles are one or a combination of at least two of acetylene black, conductive carbon black (SP), conductive graphite, carbon nanotubes, copper powder, and silver powder, or an alloy of at least two of them.
Further, the particle diameter D50 of the conductive particles in the step S1 is 10 to 500nm, preferably 20 to 100nm, for example: 20nm, 30nm, 40nm, 50nm, 60nm, 70nm, 80nm, 90nm, or 100nm, and the like.
Further, in step S1, the solvent is one or a combination of at least two of deionized water, ethanol, ethylene glycol and propanol
Further, the solvent content is 60 to 98%, more preferably 90 to 98% of the total mass of the slurry, for example: 91%, 92%, 93%, 94%, 95%, 96%, 97% or 98%, etc.
Further, the mixing method in step S1 is any one of mechanical stirring, centrifugal stirring, and ball milling.
Further preferably, the mixing manner in step S1 is ball milling, and the ball milling process is as follows: the ball-material ratio is 5-50:1, the rotating speed is 100-.
Further preferably, the ball to feed ratio is 10-30:1, for example: 10:1, 15:1, 20:1, 25:1, or 30:1, and so on.
Further preferably, the rotation speed is 1000-: 1000r/min, 1200r/min, 1500r/min, 1600r/min, 1800r/min, 2000r/min, 2200r/min, 2400r/min, 2600r/min, 2800r/min, or 3000r/min, and so forth.
Further preferably, the ball milling time is 1 to 10h, for example: 1h, 2h, 3h, 4h, 5h, 6h, 7h, 8h, 9h, or 10h, and so on.
Further, the spray drying atmosphere in step S2 is one or a combination of at least two of air, argon, nitrogen, helium, and carbon dioxide. The choice of the spray-drying atmosphere is determined by the solvent.
Further, the air inlet temperature in the spray drying in the step S2 is 100-300 ℃, and the air outlet temperature is 35-180 ℃.
Further preferably, the inlet temperature of the spray drying is 170-: 170 deg.C, 175 deg.C, 180 deg.C, 190 deg.C, 200 deg.C, 210 deg.C, 220 deg.C, 230 deg.C, 240 deg.C or 250 deg.C, etc.
Further preferably, the outlet air temperature is 70-120 ℃, for example: 70 deg.C, 75 deg.C, 80 deg.C, 85 deg.C, 89 deg.C, 91 deg.C, 95 deg.C, 100 deg.C, 105 deg.C, 110 deg.C, 115 deg.C or 120 deg.C, etc.
Further, in step S3, the non-oxidizing atmosphere is one of nitrogen, argon, and hydrogen, or a combination of at least two of them.
Further, in step S3, the carbonization conditions are: the heating rate is 1-10 ℃/min, the carbonization temperature is 400-.
Further preferably, the temperature rise rate is 1 to 6 ℃/min, for example: 1 deg.C/min, 2 deg.C/min, 3 deg.C/min, 4 deg.C/min, 5 deg.C/min or 6 deg.C/min, etc.
Further preferably, the carbonization temperature is 600-: 600 deg.C, 650 deg.C, 700 deg.C, 750 deg.C, 800 deg.C, 850 deg.C, 900 deg.C, 950 deg.C or 1000 deg.C, etc.
Further preferably, the carbonization time is 1 to 10h, for example: 1h, 2h, 3h, 4h, 5h, 6h, 7h, 8h, 9h, or 10h, and so on.
Further, in step S3, the carbonization apparatus is one of a tube furnace, a box furnace, a rotary furnace, and a bell jar furnace.
The invention has the beneficial effects that:
(1) according to the invention, the silicon-carbon composite negative electrode material is prepared by using the silylene as a silicon source, so that the problem of large silicon volume expansion is solved, and the excellent cycle performance of the material is ensured;
(2) according to the silylene/carbon composite negative electrode material provided by the invention, silylene and conductive particles are dispersed in the spherical amorphous carbon matrix, so that the direct contact between the silylene and an electrolyte is avoided, the improvement of the coulombic efficiency for the first time is facilitated, and the addition of the conductive particles improves the conductivity of the amorphous carbon matrix and simultaneously plays a role in isolating the silylene to prevent the silylene from agglomerating;
(3) according to the invention, the silicon/carbon composite negative electrode material is prepared by adopting a spherical coating technology, so that the defect of overlarge specific surface area of silicon is overcome, the first coulombic efficiency is improved, and a stable SEI film can be formed in the charging and discharging processes;
(4) the prepared silylene/carbon composite negative electrode material is high in energy density, high in first coulombic efficiency, excellent in cycle performance and rate capability and good in application prospect;
(5) the preparation method of the silylene/carbon composite negative electrode material provided by the invention is simple and is easy for industrial production.
Definition of terms
The terms "a" or "an" are used herein to describe elements and components described herein. This is done merely for convenience and to provide a general sense of the scope of the invention. Such description should be understood to include one or at least one and the singular also includes the plural unless it is obvious that it is meant otherwise.
The numbers in this disclosure are approximate, regardless of whether the word "about" or "approximately" is used. The numerical value of the number may have differences of 1%, 2%, 5%, 7%, 8%, 10%, etc. Whenever a number with a value of N is disclosed, any number with a value of N +/-1%, N +/-2%, N +/-3%, N +/-5%, N +/-7%, N +/-8% or N +/-10% is explicitly disclosed, wherein "+/-" means plus or minus, and a range between N-10% and N + 10% is also disclosed.
The following definitions, as used herein, should be applied unless otherwise indicated. For the purposes of the present invention, the chemical elements are in accordance with the CAS version of the periodic Table of elements, and the 75 th version of the handbook of chemistry and Physics, 1994. In addition, general principles of Organic Chemistry can be found in the descriptions of "Organic Chemistry", Thomas Sorrell, University Science Books, Sausaltito: 1999, and "March's Advanced Organic Chemistry" by Michael B.Smith and JerryMarch, John Wiley & Sons, New York:2007, the entire contents of which are incorporated herein by reference.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although methods and materials similar or equivalent to those described herein can also be used in the practice or testing of embodiments of the present invention, suitable methods and materials are described below. All publications, patent applications, patents, and other references mentioned herein are incorporated by reference in their entirety, unless a specific paragraph is cited. In case of conflict, the present specification, including definitions, will control. In addition, the materials, methods, and examples are illustrative only and not intended to be limiting.
Drawings
FIG. 1: the structure schematic diagram of the silylene/carbon cathode composite material provided by the invention is provided.
Wherein: 1-an amorphous carbon matrix; 2-conductive particles; 3-silylene.
Detailed Description
Example 1
Preparing a mixed aqueous solution with the solid content of 2% from silylene (D50 being 1 mu m and n being 10), SP (D50 being 30nm) and asphalt powder according to the mass ratio of 5:5:90, and carrying out ball milling and mixing in a ball mill (the ball-material ratio is 10:1) at the rotating speed of 2600r/min for 3 hours to obtain a slurry; spray drying the slurry in an air atmosphere, wherein the air inlet temperature is 250 ℃, the air outlet temperature is 89 ℃, and a silylene/carbon spherical precursor is obtained; and transferring the precursor into a tubular furnace for carbonization treatment, wherein the atmosphere is nitrogen, the heating rate is 2 ℃/min, heating to 900 ℃, preserving heat for 3h, naturally cooling to room temperature, crushing and sieving to obtain the silicon/carbon composite negative electrode material.
The obtained silylene/carbon composite negative electrode material has the particle size D50 of 19.5 mu m and the specific surface area of 3.61m2/g。
Example 2
Preparing a mixed ethanol solution with the solid content of 5% from silylene (D50 ═ 0.5 μm and n ═ 5), carbon nanotubes (D50 ═ 20nm) and phenolic resin powder according to the mass ratio of 5:5:90, and performing ball milling and mixing in a ball mill (the ball-to-material ratio is 15:1) at the rotating speed of 1000r/min for 3 hours to obtain slurry; spray drying the slurry under the nitrogen protection atmosphere, wherein the air inlet temperature is 175 ℃, and the air outlet temperature is 91 ℃ to obtain a silylene/carbon spherical precursor; and transferring the precursor into a tubular furnace for carbonization treatment, wherein the atmosphere is nitrogen, the heating rate is 5 ℃/min, heating to 850 ℃, preserving heat for 3h, naturally cooling to room temperature, crushing and sieving to obtain the silicon-alkene-carbon composite negative electrode material.
The obtained silylene/carbon composite negative electrode material has the particle size D50 of 20.1 mu m and the specific surface area of 3.20m2/g。
Example 3
Preparing a mixed aqueous solution with the solid content of 3% by using silylene (D50 ═ 0.1 μm and n ═ 15), acetylene black (D50 ═ 50nm) and glucose according to the mass ratio of 10:5:85, and carrying out ball milling and mixing in a ball mill (the ball-to-material ratio is 10:1) at the rotating speed of 1500r/min for 1h to obtain a slurry; spray drying the slurry in an air atmosphere, wherein the air inlet temperature is 200 ℃, the air outlet temperature is 95 ℃, and a silylene/carbon spherical precursor is obtained; and transferring the precursor into a tube furnace for carbonization treatment, wherein the atmosphere is argon, the heating rate is 2 ℃/min, heating to 600 ℃, preserving heat for 3h, naturally cooling to room temperature, crushing and sieving to obtain the silicon/carbon composite negative electrode material.
Through detection, the obtained silylene-carbon composite cathodeThe particle diameter D50 of the material was 17.3 μm, and the specific surface area was 4.22m2/g。
Example 4
Preparing a mixed aqueous solution with the solid content of 2% by using silylene (D50 is 0.4 mu m, n is 50), copper powder (D50 is 100nm) and PVP according to the mass ratio of 10:5:85, and carrying out ball milling and mixing in a ball mill (the ball-material ratio is 20:1) at the rotating speed of 2600r/min for 3 hours to obtain slurry; spray drying the slurry in an air atmosphere, wherein the air inlet temperature is 220 ℃, the air outlet temperature is 89 ℃, and a silylene/carbon spherical precursor is obtained; and transferring the precursor into a tubular furnace for carbonization treatment, wherein the atmosphere is nitrogen, the heating rate is 2 ℃/min, heating to 800 ℃, preserving heat for 3h, naturally cooling to room temperature, crushing and sieving to obtain the silicon/carbon composite negative electrode material.
The obtained silylene/carbon composite negative electrode material has the particle size D50 of 16.2 mu m and the specific surface area of 4.96m2/g。
Comparative example 1
In the comparative example, the silylene in the example 1 is replaced by the same amount of nano silicon, and the preparation process is consistent.
The obtained silicon/carbon composite negative electrode material was found to have a particle diameter D50 of 16.5 μm and a specific surface area of 4.12m2/g。
Comparative example 2
This comparative example differs from example 1 in that no SP is added and the preparation process remains the same.
The obtained silylene/carbon composite negative electrode material has the particle size D50 of 16.0 mu m and the specific surface area of 4.79m2/g。
Comparative example 3
In the comparative example, the asphalt powder in example 1 was changed to the same amount of artificial graphite, and the preparation process was kept consistent.
The obtained silylene/carbon composite negative electrode material has the particle size D50 of 19.2 mu m and the specific surface area of 11.32m2/g。
Comparative example 4
In the comparative example, the SP and pitch powders in example 1 were replaced with the same amount of graphene, and the preparation process was kept consistent.
After detection, the obtained siliconThe particle diameter D50 of the ene/carbon composite negative electrode material was 10.6 μm, and the specific surface area was 20.32m2/g。
Performance testing
The composite negative electrode materials obtained in examples 1 to 4 and comparative examples 1 to 4, the conductive agent acetylene black and the SA binder are prepared into water-based slurry according to the mass ratio of 93:2:5, the water-based slurry is coated on a 10-micron copper foil, the copper foil is dried in an oven at the temperature of 80 ℃, and then rolling treatment is carried out. And (3) punching the rolled copper foil into an electrode plate with the diameter of 12mm by using a punching machine, and carrying out vacuum drying in a 120 ℃ oven for 12h to obtain the working electrode. The working electrode, lithium plate, separator, electrolyte (1mol/L lithium hexafluorophosphate EC: DEC: EMC ═ 1:1:1) were assembled into 2016 coin cell in a nitrogen blanketed glove box. The blue test system is adopted for testing, the charging and discharging voltage range is 0.01-1.5V, and the results are shown in Table 1.
TABLE 1 electrochemical Properties of composite anode materials obtained in examples 1 to 4 and comparative examples 1 to 4
From the test results of the examples 1-4 in table 1, it can be seen that the batteries prepared by using the silylene/carbon composite negative electrode material of the invention have the first discharge capacity of 0.2C as high as 910mAh/g, the first charge-discharge efficiency of 0.2C as high as 81.1%, excellent rate capability and cycle performance, and good comprehensive electrical properties. In the comparative example 1, the nano silicon is adopted to replace the silylene to prepare the silicon-carbon composite material, the rate capability and the cycle performance are obviously deteriorated, which shows that the nano silicon has larger volume expansion; compared with the comparative example 2, the specific volume, the rate capability and the cycle life are all reduced without adding conductive particles; in the comparative example 3, graphite is adopted to replace asphalt powder to prepare the silicon-carbon composite material, and the electrical property of the material is poor because a coating structure cannot be obtained; in comparative example 4, the graphene is used to replace SP and asphalt powder to prepare the silicon-olefin-carbon composite material, the first efficiency is only 50.2%, because the obtained composite material is of a non-coating structure, the specific surface area of the graphene is large, and the irreversible capacity of an SEI film formed in the first charge-discharge process is high.
Claims (9)
1. A silylene/carbon composite anode material, which is characterized by comprising a spherical amorphous carbon matrix, silylene and conductive particles which are dispersed in the carbon matrix; the mass fraction of the spherical amorphous carbon matrix is 60-95%, the mass fraction of the silylene is 5-10%, the mass fraction of the conductive particles is 1-5%, the silylene has a multilayer structure, the number of layers is 5-50, and the particle size D50 is 0.1-3 μm.
2. The silicon-ene-carbon composite anode material as claimed in claim 1, wherein the particle size D50 of the silicon-ene-carbon composite anode material is 1-50 μm, and the specific surface area is 1-10m2/g。
3. The silicon-ene-carbon composite anode material as claimed in claim 1, wherein the conductive particles are one or a combination of at least two of acetylene black, conductive carbon black, conductive graphite, carbon nanotubes, copper powder and silver powder, and the particle size D50 of the conductive particles is 10-500 nm.
4. The method for preparing the silylene/carbon composite anode material according to any one of claims 1 to 3, comprising the steps of:
s1: mixing silylene, conductive particles and a carbon source in a solvent to obtain slurry;
s2: spray drying the slurry to obtain a silylene/carbon spherical precursor;
s3: and carbonizing the precursor in a non-oxidizing atmosphere to obtain the silylene/carbon composite negative electrode material.
5. The method for preparing the silicon-ene-carbon composite anode material of claim 4, wherein the carbon source in step S1 is one or a combination of at least two of pitch, phenolic resin, glucose, sucrose, sodium carboxymethylcellulose, polyvinylpyrrolidone, polyacrylonitrile, and polyvinyl alcohol.
6. The method for preparing the silylene/carbon composite anode material according to claim 4, wherein the solvent in step S1 is one or a combination of at least two of deionized water, ethanol, ethylene glycol and propanol, and the content of the solvent is 60-98% of the total mass of the slurry.
7. The method for preparing the silylene/carbon composite anode material according to claim 4, wherein the mixing in step S1 is ball milling, and the ball milling process comprises: the ball-material ratio is 5-50:1, the rotating speed is 100-.
8. The method for preparing the silylene/carbon composite anode material according to claim 4, wherein the atmosphere of the spray drying in the step S2 is one or a combination of at least two of air, argon, nitrogen, helium and carbon dioxide; the air inlet temperature during spray drying is 100-300 ℃, and the air outlet temperature is 35-180 ℃.
9. The method for preparing the silylene/carbon composite anode material according to claim 4, wherein the non-oxidizing atmosphere in step S3 is one or a combination of at least two of nitrogen, argon and hydrogen; the carbonization conditions are as follows: the heating rate is 1-10 ℃/min, the carbonization temperature is 400-.
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