CN115911306A - High-energy-density graphite composite material and preparation method thereof - Google Patents
High-energy-density graphite composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high energy density graphite composite material and a preparation method thereof, the material is composed of a shell and an inner core, the inner core is graphite, the porous cerium oxide of the shell is 10wt% -30 wt%, the lithium titanate is 0.5wt% -2 wt%, and the balance is amorphous carbon. The mass ratio of the shell to the core is (1-10): (90-100). After the porous cerium oxide is coated on the surface of the graphite, a hard carbon coating layer material is obtained through polymerization reaction, and the porous cerium oxide and the hard carbon composite material are simultaneously coated on the surface of the graphite. The invention can improve the electronic conductivity of the graphite composite material, reduce the expansion, and improve the power and the energy density of the graphite composite material.
Description
Technical Field
The invention belongs to the field of preparation of lithium ion battery materials, particularly relates to a high-energy-density graphite composite material, and also relates to a preparation method of the high-energy-density graphite composite material.
Background
Along with the improvement of the market on the high-energy density battery and the quick charging performance requirement thereof, the performance requirement on the lithium ion battery cathode material is also improved. At present, raw materials of a graphite material mainly comprise petroleum coke/needle coke, artificial graphite is formed after carbonization and amorphous carbon is arranged on the surface of the artificial graphite, and the problems of low specific capacity (less than or equal to 358 mAh/g), low compaction density (less than or equal to 1.7g/cm & lt 3 & gt), low first efficiency (less than or equal to 94%), general quick charging performance and the like mainly exist, and meanwhile, the problems that the energy density and the quick charging performance cannot be considered simultaneously exist; the cerium oxide negative electrode has the characteristics of high energy density, good power performance and the like, but the cerium oxide negative electrode cannot be used purely due to poor circulation and large expansion, and needs to be mixed with other composite materials for use so as to reduce the application risk of the materials. For example, patent application No. 201910629061.7 discloses an artificial graphite negative electrode material, and a preparation method and application thereof, wherein the preparation method comprises the steps of crushing and screening coal, fully and uniformly mixing a catalyst and the coal, and carrying out graphitization treatment to obtain the artificial graphite material with a highly-graphitized structure; the catalyst is metal oxide or non-metal acid, wherein the metal oxide is one or more of praseodymium oxide, lanthanum oxide, cerium oxide or titanium dioxide. Because the metal oxide catalyzes and graphitizes coal, praseodymium oxide, lanthanum oxide, titanium dioxide, boric acid and the like can form carbide with the coal in the graphitization process, the graphitization degree of the material is improved, but the initial efficiency is low, the interlayer spacing is reduced, the dynamic performance is reduced, and the expansion is increased.
Disclosure of Invention
The invention aims to overcome the defects and provide a high-energy-density graphite composite material which can improve the electronic conductivity and reduce the expansion of a graphite material and improve the power and the energy density of the graphite material.
Another object of the present invention is to provide a method for preparing the high energy density graphite composite material.
The invention relates to a high-energy-density graphite composite material which comprises a shell and an inner core, wherein the inner core is graphite, the porous cerium oxide of the shell accounts for 10-30 wt%, the lithium titanate accounts for 0.5-2 wt%, and the balance is amorphous carbon.
The mass ratio of the shell to the core is (1-10): (90-100);
the invention relates to a preparation method of a high-energy density graphite composite material, which comprises the following steps:
s1: according to the weight ratio of high molecular polymer: coupling agent: a boron source: the mass ratio of ammonium persulfate is 100 (1-5) to 0.5-2): (1-10), respectively weighing the raw materials, uniformly mixing, and reacting at the temperature of 100-200 ℃ for 1-6h to obtain a cross-linked polymer;
s2: dissolving the cross-linked polymer in an organic solvent, filtering, and vacuum-drying filter residue for 48 hours at 80 ℃ to obtain a precursor material A;
s3: according to the porous cerium oxide: precursor material A: the mass ratio of lithium titanate is (10-30) 100: (1-5), preparing a porous cerium oxide solution with the mass concentration of 1% -10%, adding a precursor material A and lithium titanate into the porous cerium oxide solution, uniformly stirring, and performing spray drying; then carrying out pre-carbonization treatment for 1-6h at the temperature of 800-1000 ℃, then cooling to room temperature under inert atmosphere, and crushing; then heating to 1000-1600 ℃, carbonizing for 1-6h, and crushing to obtain a precursor cladding material B;
s4: according to the proportion of graphite: resin: the mass ratio of the precursor coating material B is 100: (1-10): (0.5-2), respectively weighing graphite, resin and the precursor coating material B, putting the materials into a grinding machine, uniformly mixing the materials, grinding the materials until the granularity D50 is less than or equal to 100 mu m, and carrying out pre-carbonization treatment at the temperature of 200-400 ℃ for 1-6 h;
s5: after carbonization, continuously heating to 800-1200 ℃, preserving heat for 1-6h, then cooling in an argon inert atmosphere, and crushing until the granularity D50 is less than or equal to 20 mu m after the temperature is reduced to room temperature.
The preparation method of the high-energy density graphite composite material comprises the following steps: in the step S1, the high molecular polymer is one or more of epoxy resin, furfural resin and phenolic resin; the boron source is one or more of boric acid, boron chloride, boron oxide, boron sulfide and sodium perborate.
The preparation method of the high-energy density graphite composite material comprises the following steps: in the step S1, the coupling agent is one or more of diisopropyl titanate, isopropyl tri (dioctyl phosphate acyloxy) titanate, isopropyl trioleate acyloxy titanate, isopropyl tri (dodecyl benzenesulfonyl) titanate, tetra-isopropoxy titanium and tetra-n-butyl titanate.
The preparation method of the high-energy density graphite composite material comprises the following steps: in the step S2, the organic solvent is one or more of toluene, xylene, and acetone.
The preparation method of the high-energy density graphite composite material comprises the following steps: the preparation method of the porous cerium oxide in the step S3 is that 100 parts of 1-5% cerous sulfate solution is prepared, and then 10 parts of thiourea is added into the cerous sulfate solution and is fully stirred; simultaneously preparing 8 parts of 1mol/L sodium hydroxide solution, slowly adding the prepared sodium hydroxide solution into the cerous sulfate solution, and controlling the pH value to be 6; then, introducing oxygen to oxidize the solution for 30-90min; and heating the oxidized solution to 50-100 ℃, reacting for 1h, sintering at the temperature of 300-500 ℃ for 1-6h, and crushing to obtain the porous cerium oxide.
Compared with the prior art, the invention has obvious beneficial effects, and the technical scheme can be seen as follows: according to the invention, the porous cerium oxide is coated on the surface of graphite, so that the power performance of the porous cerium oxide is improved by utilizing the characteristic of high electronic conductivity of the porous cerium oxide, and the liquid absorption and retention capacity of the material is improved and the expansion is reduced by utilizing the porous structure of the porous cerium oxide; in addition, a hard carbon coating layer material is obtained through polymerization reaction, and the surface of graphite is coated with the porous cerium oxide and the hard carbon composite material at the same time, so that the liquid retention performance can be improved, the expansion of the graphite can be reduced, the first efficiency can be improved, and the multiplying power and the cycle performance can be further improved
Drawings
FIG. 1 is an SEM image of a high energy density graphite composite material of the present invention.
Detailed Description
Preparation of porous cerium oxide: weighing 100g of a 3% cerous sulfate solution, then adding 10g of thiourea into the cerous sulfate solution, and fully stirring; simultaneously preparing 8g of 1mol/L sodium hydroxide solution, slowly adding the prepared sodium hydroxide solution into the cerous sulfate solution, and controlling the pH value to be 6; then, introducing oxygen to oxidize the solution for 60min; and heating the oxidized solution to 80 ℃, reacting for 1h, filtering, sintering at the temperature of 400 ℃ for 3h, and crushing to obtain the porous cerium oxide.
Example 1:
a preparation method of a high-energy density graphite composite material comprises the following steps:
s1: respectively weighing 100g of epoxy resin, 3g of diisopropyl titanate, 1g of boric acid and 5g of ammonium persulfate, adding into a mixer, uniformly stirring, and reacting at the temperature of 150 ℃ for 3 hours to obtain a crosslinked polymer;
s2: and dissolving 100g of the crosslinked polymer in 1000g of a toluene organic solvent, uniformly stirring, filtering, and carrying out vacuum drying for 48 hours at 80 ℃ to obtain a precursor material A.
S3: adding 20g of porous cerium oxide into 400g of carbon tetrachloride solution to prepare 5wt% porous cerium oxide solution, then adding 100g of precursor material A and 3g of lithium titanate into the porous cerium oxide solution, uniformly stirring, and spray-drying; then carrying out pre-carbonization treatment at 900 ℃ for 3h, then cooling to room temperature under the inert atmosphere of argon, and crushing; then heating to 1200 ℃, carbonizing for 3h, and crushing to obtain a precursor coating material B;
s4: respectively weighing 100g of artificial graphite, 5g of phenolic resin and 1g of precursor coating material B according to the mass ratio, putting the artificial graphite, the phenolic resin and the precursor coating material B into a grinding machine, uniformly mixing, grinding until the granularity D50=80 mu m, carrying out pre-carbonization treatment at the temperature of 300 ℃, and carbonizing for 3 hours;
s5: and after carbonization, continuously heating to 1000 ℃, keeping the temperature for 3h, then cooling in an argon inert atmosphere, and crushing until the granularity D50=16 μm after the temperature is reduced to room temperature.
Example 2:
a preparation method of a high-energy density graphite composite material comprises the following steps:
s1: weighing 100g of furfural resin, 1g of isopropyl tri (dioctyl phosphate acyloxy) titanate, 0.5g of boron chloride and 1g of ammonium persulfate, adding into a mixer, uniformly stirring, and reacting at 100 ℃ for 6h to obtain a crosslinked polymer;
s2: dissolving 100g of cross-linked polymer in 1000g of xylene organic solvent, filtering, and vacuum-drying at 80 ℃ for 48h to obtain a precursor material A;
s3: adding 10g of porous cerium oxide into 10000g of cyclohexane solvent to prepare a 1% porous cerium oxide solution, then adding 100g of precursor material A and 1g of lithium titanate into the porous cerium oxide solution, uniformly stirring, and performing spray drying; then carrying out pre-carbonization treatment at 800 ℃ for 6h, then cooling to room temperature under the inert atmosphere of argon, and crushing; then heating to 1000 ℃, carbonizing for 6h, and crushing to obtain a precursor coating material B;
s4: weighing 100g of artificial graphite, 1g of furfural resin and 0.5g of precursor coating material B, putting into a grinding machine, uniformly mixing, grinding until the granularity D50=100 μm, and carrying out pre-carbonization treatment for 6h at the temperature of 200 ℃;
s5: and after carbonization, continuously heating to 800 ℃, keeping the temperature for 6h, then cooling in an argon inert atmosphere, and crushing until the granularity D50=10 μm after the temperature is reduced to room temperature.
Example 3:
a preparation method of a high-energy density graphite composite material comprises the following steps:
s1: weighing 100g of phenolic resin, 5g of isopropyl trioleate acyloxy titanate, 2g of boron sulfide and 2g of ammonium persulfate, adding into a mixer, uniformly stirring, and reacting at the temperature of 200 ℃ for 1h to obtain a crosslinked polymer;
s2: dissolving 100g of cross-linked polymer in 1000g of N-methyl pyrrolidone organic solvent, filtering, and vacuum-drying at 80 ℃ for 48h to obtain a precursor material A;
s3: adding 30g of porous cerium oxide into 300g of N-methylpyrrolidone to prepare a 10% porous cerium oxide solution, then adding 100g of precursor material A and 5g of lithium titanate into the porous cerium oxide solution, uniformly stirring, and spray-drying; then carrying out pre-carbonization treatment at the temperature of 1000 ℃ for 1h, then cooling to room temperature under the inert atmosphere of argon, and crushing; then heating to 1600 ℃, carbonizing for 1h, and crushing to obtain a precursor coating material B;
s4: weighing 100g of artificial graphite, 10g of phenolic resin and 2g of precursor coating material B, putting into a grinding machine, uniformly mixing, grinding until the granularity D50=50 μm, carrying out pre-carbonization treatment at 400 ℃, and carbonizing for 1h;
s5: and after carbonization, continuously heating to 1200 ℃, keeping the temperature for 1h, then cooling in an argon inert atmosphere, and crushing until the granularity D50=10 μm after the temperature is reduced to room temperature.
Comparative example:
a preparation method of a graphite composite material comprises the following steps:
s1: respectively weighing 100g of epoxy resin and 1g of boric acid, adding into a mixer, uniformly stirring, and reacting at the temperature of 150 ℃ for 3 hours to obtain a crosslinked polymer;
s2: dissolving 100g of the crosslinked polymer in 1000g of a toluene organic solvent, uniformly stirring, filtering, and carrying out vacuum drying at 80 ℃ for 48h to obtain a precursor material A.
S3: adding 100g of precursor material A and 3g of lithium titanate into 500g of cyclohexane solution, uniformly stirring, and carrying out spray drying; then carrying out pre-carbonization treatment for 3h at the temperature of 900 ℃, then cooling to room temperature under the inert atmosphere of argon, and crushing; then heating to 1200 ℃, carbonizing for 3h, and crushing to obtain a precursor coating material B;
s4: weighing 100g of artificial graphite, 5g of phenolic resin and 1g of precursor coating material B, putting into a grinding machine, uniformly mixing, grinding, carrying out pre-carbonization treatment at the temperature of 300 ℃, and carbonizing for 3 hours;
s5: and after carbonization, continuously heating to 1000 ℃, keeping the temperature for 3h, then cooling in an argon inert atmosphere, and crushing until the particle size D50=15 μm after the temperature is reduced to room temperature to obtain the graphite composite material.
And (3) detecting physical and chemical properties:
(1) SEM detection
Example 1 was subjected to SEM test and the results are shown in figure 1.
It is thus understood that the graphite composite material obtained in example 1 had a granular structure and was uniform in size, and the particle diameter was between 10 and 15 μm.
(2) Powder conductivity test
The graphite composite materials prepared in examples 1 to 3 and the graphite composite material prepared in the comparative example were subjected to a powder conductivity test, which was carried out by the following method: pressing the powder into a blocky structure on a powder compaction density instrument under the pressure of 2T, and testing the powder conductivity by adopting a four-probe tester, wherein the test results are shown in table 1:
TABLE 1
| Item | Example 1 | Example 2 | Example 3 | Comparative example |
| Conductivity (S/cm) | 6.23 | 6.45 | 6.57 | 9.56 |
As can be seen from table 1, the electrical conductivity of the porous cerium oxide hard carbon coated graphite composite material of the present invention is significantly higher than that of the comparative example, because the electronic conductivity of the material is improved by coating the surface of the material with cerium oxide doped with high electronic conductivity.
(3) Tap density, specific surface area, interlayer spacing D002 test
The detection is carried out according to the detection method of the national standard GB/T-243333-2019 graphite cathode material for lithium ion batteries, and the detection result is shown in Table 2:
TABLE 2
| Item | Example 1 | Example 2 | Example 3 | Comparative example |
| Tap density (g/cm) 3 ) | 1.12 | 1.13 | 1.10 | 0.94 |
| Specific surface area (m) 2 /g) | 1.75 | 1.73 | 1.71 | 1.23 |
| Interlayer spacing D002 (nm) | 0.3359 | 0.3358 | 0.3357 | 0.3354 |
As can be seen from table 2, the graphite composite materials prepared in examples 1 to 3 have good tap density and a significantly higher specific surface area than the comparative examples, for the reason that the porous cerium oxide of the coating material has a high specific surface area, thereby increasing the specific surface area of the graphite material, and the metal oxide itself has a high tap density, thereby increasing the tap density of the material.
(4) Button cell test
The graphite composite materials prepared in the examples 1 to 3 and the graphite composite material prepared in the comparative example are assembled into button cells A1, A2, A3 and B1 respectively, and the assembling method comprises the following steps: adding a binder, a conductive agent and a solvent into the graphite composite material, stirring and mixing uniformly to prepare a negative electrode slurry, coating the negative electrode slurry on a copper foil, drying, rolling and cutting to prepare a negative electrode sheet, wherein the binder is a LA132 binder, the conductive agent is an SP conductive agent, and the solvent is secondary distilled water; wherein the graphite composite material, the SP conductive agent, the LA132 binder and the secondary distilled water are mixed in a mass ratio of 95 6 /EC+DEC(LiPF 6 The concentration of (1.3 mol/L), the volume ratio of EC to DEC is 1).
Specifically, the button cell was assembled in an argon-filled glove box, electrochemical performance testing was performed on a cell tester, the voltage range of charging and discharging was 0.005V-2.0V, the charging and discharging rate was 0.1C, and the discharge capacities at 3C and 0.2C rates were tested, with the test results shown in table 3:
TABLE 3
As can be seen from table 3, the first discharge capacity and the first charge-discharge efficiency of the lithium ion battery prepared by using the graphite composite material of embodiments 1 to 3 of the present invention are significantly higher than those of the comparative example, which indicates that the porous cerium oxide is coated on the surface of the graphite core, and the rate capability of the lithium ion battery is improved by using the characteristic of high electronic conductivity of the cerium oxide; meanwhile, the cerium oxide has high specific capacity, and the exertion of the discharge specific capacity of the material is promoted; in addition, the lithium titanate in the coating layer can improve the lithium ion conductivity of the material, and is favorable for improving the rate capability of the button cell.
(5) Pouch cell testing
Preparing a negative electrode by using the graphite composite materials of examples 1 to 3 and the graphite composite material of the comparative example as a negative electrode material; with ternary materials (LiNi) 1/3 Co 1/3 Mn 1/3 O 2 ) The positive electrode is prepared by LiPF 6 Solution (solvent EC + DEC, volume ratio 1, lipf 6 The concentration of 1.3 mol/L) is used as electrolyte, celegard2400 is used as a diaphragm, 5Ah soft package batteries A4, A5, A6 and B2 are prepared, and then the cycle performance, the rate performance and the expansion performance of the soft package batteries in different states are tested, wherein the test conditions are as follows:
1) Cycle performance test conditions: the charging and discharging current is 1C/1C, the voltage range is 2.8-4.2V, the cycle time is 500 times, and the full-electricity expansion of the negative pole piece after the cycle is tested.
2) Multiplying power performance test conditions: the charging multiplying power is 1C/3C/5C/8C, and the discharging multiplying power is 1C; the voltage range is 2.8-4.2V.
The cycle performance test results are shown in table 4, and the rate performance test structure is shown in table 5.
TABLE 4
From table 4, it can be seen that, under the condition of charge and discharge current of 1C/1C, after 500 cycles, the cycle performance of the pouch battery prepared by using the graphite composite material of examples 1 to 3 is significantly better than that of the comparative example, which indicates that the porous cerium oxide is coated on the surface of graphite, and the liquid absorption and retention capacity is improved by using the good power performance and the high specific surface area of the porous cerium oxide, which is beneficial to improving the cycle performance. While the porous structure of the example material and its large interlayer spacing reduce its full electrical expansion after cycling.
TABLE 5
As can be seen from table 5, the pouch batteries prepared from the composite materials of examples 1 to 3 have a better constant current ratio at different charging rates, which illustrates that the porous cerium oxide material is coated on the surface of the graphite core, and the intercalation/deintercalation rate of lithium ions can be increased by using the characteristic of high electronic conductivity of the porous cerium oxide, so that the rate charging performance is improved.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are within the scope of the present invention without departing from the technical spirit of the present invention.
Claims (7)
1. A high-energy-density graphite composite material comprises a shell and an inner core, wherein the inner core is graphite, the porous cerium oxide of the shell accounts for 10wt% -30 wt%, the lithium titanate accounts for 0.5wt% -2 wt%, and the balance is amorphous carbon.
2. The high energy density graphite composite of claim 1, wherein: the mass ratio of the shell to the core is (1-10): (90-100).
3. A preparation method of a high-energy density graphite composite material comprises the following steps:
s1: according to the weight ratio of high molecular polymer: coupling agent: a boron source: the mass ratio of ammonium persulfate is 100 (1-5) to 0.5-2): (1-10), weighing the raw materials respectively, mixing uniformly, and reacting at the temperature of 100-200 ℃ for 1-6h to obtain a cross-linked polymer;
s2: dissolving the cross-linked polymer in an organic solvent, filtering, and vacuum-drying filter residue for 48 hours at 80 ℃ to obtain a precursor material A;
s3: according to the weight ratio of porous cerium oxide: precursor material A: the mass ratio of lithium titanate is (10-30) and is 100: (1-5), preparing a porous cerium oxide solution with the mass concentration of 1% -10%, adding a precursor material A and lithium titanate into the porous cerium oxide solution, uniformly stirring, and performing spray drying; then carrying out pre-carbonization treatment for 1-6h at the temperature of 800-1000 ℃, then cooling to room temperature under inert atmosphere, and crushing; then heating to 1000-1600 ℃, carbonizing for 1-6h, and crushing to obtain a precursor cladding material B;
s4: according to the proportion of graphite: resin: the mass ratio of the precursor coating material B is 100: (1-10): (0.5-2), respectively weighing graphite, resin and the precursor coating material B, putting the graphite, the resin and the precursor coating material B into a grinding machine, uniformly mixing, grinding until the granularity D50 is less than or equal to 100 mu m, carrying out pre-carbonization treatment at the temperature of 200-400 ℃, and carbonizing for 1-6 h;
s5: and after carbonization, continuously heating to 800-1200 ℃, preserving heat for 1-6h, then cooling in an argon inert atmosphere, and crushing until the particle size D50 is less than or equal to 20 mu m when the temperature is reduced to room temperature.
4. A method of preparing a high energy density graphite composite material as claimed in claim 3 wherein: in the step S1, the high molecular polymer is one or more of epoxy resin, furfural resin and phenolic resin; the boron source is one or more of boric acid, boron chloride, boron oxide, boron sulfide and sodium perborate.
5. A method of preparing a high energy density graphite composite material as claimed in claim 3 wherein: in the step S1, the coupling agent is one or more of diisopropyl titanate, isopropyl tri (dioctyl phosphate acyloxy) titanate, isopropyl trioleate acyloxy titanate, isopropyl tri (dodecyl benzene sulfonyl) titanate, tetra-isopropoxy titanium and tetra-n-butyl titanate.
6. A method of preparing a high energy density graphite composite material as claimed in claim 3, wherein: in the step S2, the organic solvent is one or more of toluene, xylene and acetone.
7. A method of preparing a high energy density graphite composite material as claimed in any one of claims 3 to 6 wherein: the preparation method of the porous cerium oxide in the step S3 is that 100 parts of 1-5% cerous sulfate solution is prepared, and then 10 parts of thiourea is added into the cerous sulfate solution and is fully stirred; preparing 8 parts of 1mol/L sodium hydroxide solution, slowly adding the prepared sodium hydroxide solution into the cerous sulfate solution, and controlling the pH value to be 6; then, introducing oxygen to oxidize the solution for 30-90min; and heating the oxidized solution to 50-100 ℃, reacting for 1h, sintering at the temperature of 300-500 ℃ for 1-6h, and crushing to obtain the porous cerium oxide.
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