CN115911306B - High-energy-density graphite composite material and preparation method thereof - Google Patents
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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 an outer shell and an inner core, the inner core is graphite, the porous cerium oxide of the outer shell is 10 wt-30 wt%, the lithium titanate is 0.5-wt-2 wt% and the rest is amorphous carbon. The mass ratio of the shell to the core is (1-10): (90-100). The porous cerium oxide is coated on the surface of graphite, and then the hard carbon coating layer material is obtained through polymerization reaction, and the porous cerium oxide and the hard carbon composite material are coated on the surface of the graphite at the same time. 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, in particular to a high-energy-density graphite composite material and also relates to a preparation method of the high-energy-density graphite composite material.
Background
With the improvement of the requirements of the market on the high-energy density battery and the quick charge performance thereof, the performance requirements on the lithium ion battery cathode material are also improved. At present, the raw materials of the graphite material mainly take petroleum coke/needle coke as the main materials, artificial graphite is formed after carbonization, and amorphous carbon is formed on the surface of the artificial graphite, and the artificial graphite mainly has 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 < 3 >), low first efficiency (less than or equal to 94%), general quick charge performance and the like, and meanwhile, the energy density and the quick charge performance cannot be simultaneously considered; the cerium oxide cathode has the characteristics of high energy density, good power performance and the like, but has poor circulation and can not be used purely due to the expansion of the cerium oxide cathode, and the cerium oxide cathode needs to be mixed with other composite materials for use so as to reduce the application risk of the cerium oxide cathode. For example, patent application number 201910629061.7 discloses an artificial graphite negative electrode material, 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 an 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. The metal oxide catalyzes graphitization of coal, so that 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 first efficiency is low, the interlayer spacing is reduced, the dynamics performance is reduced, and the expansion is increased.
Disclosure of Invention
The invention aims to overcome the defects and provide the high-energy-density graphite composite material which can improve the electronic conductivity and reduce the expansion of the 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 consists of an outer shell and an inner core, wherein the inner core is graphite, the porous cerium oxide of the outer shell is 10-30wt%, the lithium titanate is 0.5-2wt% 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 high molecular polymer: coupling agent: boron source: the mass ratio of the ammonium persulfate is 100 (1-5) to (0.5-2): (1-10), respectively weighing the raw materials, uniformly mixing, and reacting at 100-200 ℃ for 1-6h to obtain a crosslinked polymer;
s2: dissolving the crosslinked polymer in an organic solvent, filtering, and vacuum drying filter residues for 48 hours at 80 ℃ to obtain a precursor material A;
s3: porous cerium oxide: precursor material a: the mass ratio of the 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 spray-drying; then pre-carbonizing for 1-6h at 800-1000 ℃, then cooling to room temperature under inert atmosphere, and crushing; heating to 1000-1600 ℃ for carbonization for 1-6h, and crushing to obtain a precursor coating material B;
s4: according to the graphite: resin: the mass ratio of the precursor coating material B is 100: (1-10): (0.5-2), respectively weighing graphite, resin and a precursor coating material B, putting into a grinding machine, uniformly mixing, grinding to a granularity D50 of 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: and (3) after carbonization, continuously heating to 800-1200 ℃, preserving heat for 1-6h, then cooling under an inert atmosphere of argon, cooling to room temperature, and crushing to the granularity D50 of less than or equal to 20 mu m.
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 acyloxy phosphate) titanate, isopropyl trioleate acyloxy titanate, isopropyl tri (dodecylbenzenesulfonyl) titanate, tetraisopropoxytitanium 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 comprises the steps of preparing 100 parts of 1-5% cerium sulfate solution, adding 10 parts of thiourea into the cerium sulfate solution, and fully stirring; meanwhile, 8 parts of sodium hydroxide solution with the concentration of 1mol/L is prepared, the prepared sodium hydroxide solution is slowly added into the cerium sulfate solution, and the pH value is controlled to be 6; then, introducing oxygen to oxidize the solution, and introducing the solution for 30-90min; heating the oxidized solution to 50-100 ℃, reacting for 1h, sintering at 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 adopted 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 and the expansion reduction of the material are improved by utilizing the porous structure of the porous cerium oxide; in addition, the hard carbon coating material is obtained through polymerization reaction, and the porous cerium oxide and the hard carbon composite material are coated on the surface of the graphite at the same time, so that the liquid retention performance can be improved, the expansion of the composite material is reduced, the first efficiency is improved, and the multiplying power and the cycle performance are 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: 100g of a 3% cerium sulfate solution is weighed, and then 10g of thiourea is added into the cerium sulfate solution and fully stirred; meanwhile, preparing 8g of 1mol/L sodium hydroxide solution, slowly adding the prepared sodium hydroxide solution into the cerium sulfate solution, and controlling the pH value to be 6; then, introducing oxygen to oxidize the solution, and introducing the solution for 60min; and heating the oxidized solution to 80 ℃, reacting for 1h, filtering, sintering at 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 150 ℃ for 3 hours to obtain a crosslinked polymer;
s2: 100g of the crosslinked polymer is dissolved in 1000g of toluene organic solvent, stirred uniformly, filtered and dried in vacuum at 80 ℃ for 48 hours to obtain a precursor material A.
S3: adding 20g of porous cerium oxide into 400g of carbon tetrachloride solution to prepare a porous cerium oxide solution with the concentration of 5wt%, adding 100g of precursor material A and 3g of lithium titanate into the porous cerium oxide solution, uniformly stirring, and spray-drying; then pre-carbonizing for 3 hours at 900 ℃, then cooling to room temperature under the inert atmosphere of argon, and crushing; then heating to 1200 ℃ for carbonization for 3 hours, 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 into a grinder, uniformly mixing, grinding to obtain a particle size D50=80 mu m, carrying out pre-carbonization treatment at 300 ℃, and carbonizing for 3 hours;
s5: and (3) after carbonization, continuously heating to 1000 ℃, preserving heat for 3 hours, then cooling under an inert argon atmosphere, cooling to room temperature, and crushing to obtain the product with the granularity D50=16 mu m.
Example 2:
a preparation method of a high-energy-density graphite composite material comprises the following steps:
s1: 100g of furfural resin, 1g of isopropyl tri (dioctyl phosphate acyloxy) titanate, 0.5g of boron chloride and 1g of ammonium persulfate are weighed and added into a mixer, uniformly stirred, and reacted for 6 hours at the temperature of 100 ℃ to obtain a crosslinked polymer;
s2: dissolving 100g of crosslinked polymer in 1000g of xylene organic solvent, filtering, and vacuum drying at 80 ℃ for 48 hours to obtain a precursor material A;
s3: 10g of porous cerium oxide is added into 1000g of cyclohexane solvent to prepare a porous cerium oxide solution with the concentration of 1%, then 100g of precursor material A and 1g of lithium titanate are added into the porous cerium oxide solution, and the mixture is uniformly stirred and spray-dried; then pre-carbonizing treatment is carried out for 6 hours at 800 ℃, then the temperature is reduced to room temperature under the inert atmosphere of argon, and the powder is crushed; then heating to 1000 ℃ for carbonization for 6 hours, 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 grinder, uniformly mixing, grinding to obtain a particle size D50=100 mu m, and carrying out pre-carbonization treatment for 6 hours at the temperature of 200 ℃;
s5: and (3) after carbonization, continuously heating to 800 ℃, preserving heat for 6 hours, then cooling under an argon inert atmosphere, cooling to room temperature, and crushing to obtain the product with the granularity D50=10μm.
Example 3:
a preparation method of a high-energy-density graphite composite material comprises the following steps:
s1: 100g of phenolic resin, 5g of isopropyl trioleate acyloxy titanate, 2g of boron sulfide and 2g of ammonium persulfate are weighed and added into a mixer, and uniformly stirred, and reacted for 1h at the temperature of 200 ℃ to obtain a crosslinked polymer;
s2: dissolving 100g of crosslinked polymer in 1000g N-methyl pyrrolidone organic solvent, filtering, and vacuum drying at 80 ℃ for 48 hours to obtain a precursor material A;
s3: adding 30g of porous cerium oxide into 300g N-methyl pyrrolidone to prepare a porous cerium oxide solution with the concentration of 10%, adding 100g of precursor material A and 5g of lithium titanate into the porous cerium oxide solution, uniformly stirring, and spray-drying; then pre-carbonizing at 1000 ℃ for 1h, cooling to room temperature under the inert atmosphere of argon, and crushing; then heating to 1600 ℃ for carbonization 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 grinder, uniformly mixing, grinding to obtain a particle size D50=50 mu m, and carrying out pre-carbonization treatment at 400 ℃ for 1h;
s5: and (3) after carbonization, continuously heating to 1200 ℃, preserving heat for 1h, then cooling under an inert argon atmosphere, cooling to room temperature, and crushing to obtain the product with the granularity D50=10μm.
Comparative example:
a preparation method of a graphite composite material comprises the following steps:
s1: respectively weighing 100g of epoxy resin, adding 1g of boric acid into a mixer, uniformly stirring, and reacting at 150 ℃ for 3 hours to obtain a crosslinked polymer;
s2: 100g of the crosslinked polymer is dissolved in 1000g of toluene organic solvent, stirred uniformly, filtered and dried in vacuum at 80 ℃ for 48 hours to obtain a precursor material A.
S3: 100g of precursor material A and 3g of lithium titanate are added into 500g of cyclohexane solution, stirred uniformly and spray dried; then pre-carbonizing for 3 hours at 900 ℃, then cooling to room temperature under the inert atmosphere of argon, and crushing; then heating to 1200 ℃ for carbonization for 3 hours, 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 300 ℃, and carbonizing for 3h;
s5: and (3) after carbonization, continuously heating to 1000 ℃, preserving heat for 3 hours, then cooling under an inert argon atmosphere, cooling to room temperature, and crushing to obtain the graphite composite material with the granularity D50=15 mu m.
Physical and chemical property detection:
(1) SEM examination
SEM testing was performed on example 1, and the results are shown in fig. 1.
From this, it was found that the graphite composite material obtained in example 1 had a granular structure, and was uniform in size and had a particle diameter of 10 to 15. Mu.m.
(2) Powder conductivity test
The graphite composite materials prepared in examples 1-3 and the graphite composite materials prepared in comparative examples were subjected to powder conductivity testing by the following method: powder was pressed into a block-like structure on a powder compaction densitometer with a pressure of 2T, and powder conductivity was tested using a four-probe tester, with the test results shown in table 1:
TABLE 1
| Project | Example 1 | Example 2 | Example 3 | Comparative example |
| Resistivity (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 is obviously higher than that of the comparative example, because the surface of the material is coated with cerium oxide with high doped electron conductivity to improve the electron conductivity.
(3) Tap Density, specific surface area, layer spacing D002 test
The detection is carried out according to the detection method of national standard GB/T-24533-2019 lithium ion battery graphite anode material, and the detection result is shown in Table 2:
TABLE 2
| Project | 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 1-3 have good tap density and a specific surface area significantly higher than that of the comparative example, because the porous cerium oxide of the coating material has a high specific surface area so as to improve the specific surface area of the graphite material, and the metal oxide itself has the characteristic of high tap density so as to improve the tap density of the material.
(4) Button cell testing
The graphite composite materials prepared in examples 1-3 and the graphite composite materials prepared in comparative examples were assembled into button cells A1, A2, A3, B1, respectively, by the following methods: adding an adhesive, a conductive agent and a solvent into the graphite composite material, stirring and mixing uniformly to prepare negative electrode slurry, coating the negative electrode slurry on a copper foil, drying, rolling and cutting to prepare a negative electrode plate, wherein the adhesive is an LA132 adhesive, the conductive agent is an SP conductive agent, and the solvent is secondary distilled water; wherein the mass ratio of the graphite composite material to the SP conductive agent to the LA132 binder to the secondary distilled water is 95:1:4:220, and the electrolyte is LiPF 6 /EC+DEC(LiPF 6 Concentration of (2)1.3mol/L, a volume ratio of EC to DEC of 1:1), the metallic lithium sheet as a counter electrode and the celegard2400 as a separator.
Specifically, the assembly of the button cell was performed in an argon-filled glove box, the electrochemical performance test was performed on a cell tester, the voltage range of charge and discharge was 0.005V-2.0V, the charge and discharge rate was 0.1C, and the discharge capacities thereof at 3C and 0.2C rates were tested, and the test results are shown in table 3:
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 the graphite composite material of examples 1-3 of the present invention are significantly higher than those of the comparative example, which illustrates that the porous cerium oxide is coated on the surface of the graphite core, and the high rate capability of the graphite core is improved by utilizing the characteristic of high electron conductivity of the cerium oxide itself; meanwhile, cerium oxide has high specific capacity, so that the specific discharge capacity of the material is improved; in addition, lithium titanate in the coating layer can improve lithium ion conductivity of the material, and is beneficial to improving rate performance of the button cell.
(5) Soft package battery test
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 material (LiNi 1/3 Co 1/3 Mn 1/3 O 2 ) Preparation of positive electrode as positive electrode material with LiPF 6 Solution (EC+DEC solvent, volume ratio of 1:1, liPF) 6 1.3 mol/L) as an electrolyte, and cellgard 2400 as a separator, 5Ah soft pack batteries A4, A5, A6, and B2 were prepared, and then the soft pack batteries were tested for cycle performance, rate performance, and expansion performance in different states under the following test conditions:
1) Cycle performance test conditions: the charge-discharge current is 1C/1C, the voltage range is 2.8-4.2V, the cycle number is 500, and the full-charge expansion of the negative electrode plate after the cycle is tested.
2) Rate performance test conditions: charging multiplying power 1C/3C/5C/8C, discharging multiplying power 1C; the voltage range is 2.8-4.2V.
The test results of the cycle performance are shown in table 4, and the test structures of the rate performance are shown in table 5.
TABLE 4 Table 4
From Table 4, it can be seen that, after 500 times of circulation under the condition of charge-discharge current of 1C/1C, the circulation performance of the soft-packed battery prepared by the graphite composite material of examples 1-3 is obviously better than that of the comparative example, which shows that the porous cerium oxide is coated on the surface of the graphite, and the liquid absorption and retention capacity is improved by utilizing the good power performance and the high specific surface area of the porous cerium oxide, thereby being beneficial to improving the circulation performance. While the porous structure of the example material and its large interlayer spacing reduce its full electrical expansion after cycling.
TABLE 5
From table 5, it can be seen that under different charging rates, the soft-pack battery prepared from the composite materials of examples 1-3 has a better constant current ratio, which indicates that the porous cerium oxide material is coated on the surface of the graphite core, and the characteristic of high electronic conductivity of the porous cerium oxide is utilized to improve the rate of lithium ion intercalation/deintercalation, thereby improving the rate charging performance.
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the invention in any way, and any simple modification, equivalent variation and variation of the above embodiment according to the technical matter of the present invention still fall within the scope of the technical scheme of the present invention.
Claims (4)
1. A preparation method of a high-energy-density graphite composite material comprises the following steps:
s1: according to the high molecular polymer: coupling agent: boron source: the mass ratio of the ammonium persulfate is 100 (1-5) to (0.5-2): (1-10), respectively weighing the raw materials, uniformly mixing, and reacting at 100-200 ℃ for 1-6h to obtain a crosslinked polymer;
s2: dissolving the crosslinked polymer in an organic solvent, filtering, and vacuum drying filter residues for 48 hours at 80 ℃ to obtain a precursor material A;
s3: porous cerium oxide: precursor material a: the mass ratio of the 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 spray-drying; then pre-carbonizing for 1-6h at 800-1000 ℃, then cooling to room temperature under inert atmosphere, and crushing; heating to 1000-1600 ℃ for carbonization for 1-6h, and crushing to obtain a precursor coating material B;
s4: according to the graphite: resin: the mass ratio of the precursor coating material B is 100: (1-10): (0.5-2), respectively weighing graphite, resin and a precursor coating material B, putting into a grinding machine, uniformly mixing, grinding to a granularity D50 of 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: continuously heating to 800-1200 ℃ after carbonization, preserving heat for 1-6h, then cooling under an inert atmosphere of argon, cooling to room temperature, and crushing to a granularity D50 of less than or equal to 20 mu m to obtain the modified carbon fiber;
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;
in the step S1, the coupling agent is one or more of diisopropyl titanate, isopropyl tri (dioctyl acyloxy phosphate) titanate, isopropyl trioleate acyloxy titanate, isopropyl tri (dodecylbenzenesulfonyl) titanate, tetraisopropoxytitanium and tetra-n-butyl titanate;
the preparation method of the porous cerium oxide in the step S3 comprises the steps of preparing 100 parts of 1-5% cerium sulfate solution, adding 10 parts of thiourea into the cerium sulfate solution, and fully stirring; meanwhile, 8 parts of sodium hydroxide solution with the concentration of 1mol/L is prepared, the prepared sodium hydroxide solution is slowly added into the cerium sulfate solution, and the pH value is controlled to be 6; then, introducing oxygen to oxidize the solution, and introducing the solution for 30-90min; heating the oxidized solution to 50-100 ℃, reacting for 1h, sintering at 300-500 ℃ for 1-6h, and crushing to obtain the porous cerium oxide.
2. The method for preparing a high energy density graphite composite material as claimed in claim 1, wherein: in the step S2, the organic solvent is one or more of toluene, xylene and acetone.
3. The high energy density graphite composite material prepared by the preparation method of the high energy density graphite composite material as claimed in claim 1 or 2, which consists of a shell and an inner core, wherein the inner core is graphite, the porous cerium oxide of the shell is 10-wt-30 wt%, the lithium titanate is 0.5-wt-2 wt%, and the balance is amorphous carbon.
4. A high energy density graphite composite material prepared by the method of preparing a high energy density graphite composite material as claimed in claim 3, wherein: the mass ratio of the shell to the core is (1-10): (90-100).
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