CN109775675B - Re6P13Preparation method and preparation method of composite anode material of carbon material - Google Patents
Re6P13Preparation method and preparation method of composite anode material of carbon material Download PDFInfo
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- CN109775675B CN109775675B CN201811607897.9A CN201811607897A CN109775675B CN 109775675 B CN109775675 B CN 109775675B CN 201811607897 A CN201811607897 A CN 201811607897A CN 109775675 B CN109775675 B CN 109775675B
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Abstract
The invention discloses Re6P13The rhenium phosphide material is prepared by a one-step gas transport technology, so that a safer cathode material is prepared; the rhenium phosphide material has a rod-shaped structure and a high specific surface area, is beneficial to full contact with electrolyte, ensures that the diffusion path of lithium ions is short, greatly improves the discharge specific capacity and the rate capability of the battery, and improves the quick charge and quick discharge performance of the battery; the electrode conductivity is improved by compounding with the carbon material, the microscopic morphology can be protected from being damaged by the action of physical wrapping or chemical bonding formed between the electrode and the carbon material, and the multiplying power performance of the battery is obviously improved; the gas-phase transport technology for preparing the rhenium oxide has simple production process, is easy for batch preparation and has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of battery materials, and particularly relates to Re6P13A preparation method and a preparation method of the composite cathode material of the carbon material.
Background
Among numerous power energy storage technologies, lithium ion batteries have the advantages of high working voltage, small size, high energy density, no memory effect, good safety performance and the like, and are widely applied to the fields of electric automobiles, consumer electronics and the like. In recent years, with the driving of the industrial demands of small-sized portable devices (e.g., smart phones, tablet computers), and high-power electric vehicles, the development of lithium ion batteries with fast charging and discharging capabilities and higher energy density is the current objective of relevant research. Currently, commercial lithium ion batteries generally adopt carbon-based negative electrode materials, such as graphite, which have high stability but theoretical capacity of 372mAh/g only, so research and development of new battery negative electrode material systems are imperative. Elemental phosphorus possesses theoretical capacities as high as 2596mAh/g compared to graphite cathodes, and thus phosphorus-based materials are considered to be an excellent choice for commercial lithium ion battery cathodes. In general, the phosphorus contained in the transition metal phosphide can reversibly react with metallic lithium to provide reversible capacity, and the first lithium intercalation process is as follows:
M'xPy+3yLi++3ye-—xM+yLi3P。
the potential platform of the reaction lithiation/delithiation is about 1V and is far higher than the electrodeposition potential of metallic lithium, so that the potential platform is favorable for inhibiting the formation of lithium dendrites, and has higher safety performance than a graphite electrode. Meanwhile, due to the low discharge platform, the battery assembled by the transition metal phosphide and the anode material has considerable potential difference, which is beneficial to realizing high energy density. However, the transition metal phosphide still has the following problems in the application of lithium ion negative electrode materials. On one hand, the phosphorus-based material has low conductivity, so that the utilization rate of active substances in the sodium ion battery is low, and the displayed capacity is far lower than the theoretical capacity; on the other hand, although the phosphorus lithiation reaction can provide higher capacity, the volume change is large in the lithium extraction process, and especially in the large-rate cycle process, the micro morphology of the electrode material is damaged, so that the capacity is rapidly reduced. In addition, phosphide of different metals has different crystal structures and activities, and corresponds to different charge-discharge behaviors and rate stability. Currently, the development of metal phosphides for lithium ion electrode negative electrode materials remains a challenge.
Disclosure of Invention
The invention aims to overcomeThe disadvantages of the prior art mentioned above, provide a Re6P13A preparation method and a preparation method of the composite cathode material of the carbon material.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
re6P13The preparation method comprises the following steps:
1) mixing rhenium powder and red phosphorus under the atmosphere of inert gas to obtain a two-phase mixture; wherein the mass ratio of rhenium powder to red phosphorus is 6: (3.5-4.5);
2) adding a transmission agent into the two-phase mixture to obtain a three-phase mixture, wherein the pressure of a space where the three-phase mixture is located is vacuum pressure; wherein, the mass ratio of the mass of the transmission agent to the total mass of the rhenium powder and the red phosphorus is 1 to 5 percent;
3) heating the three-phase mixture to 850-900 ℃ by adopting a chemical vapor transport method, preserving heat for 3-12 days, and then cooling to obtain a mixture containing rhenium phosphide;
4) taking out the mixture, and washing, centrifuging and drying the mixture to obtain the rhenium phosphide powder.
Further, the inert gas in the step 1) is argon or nitrogen.
Further, the transmission agent in step 2) comprises I2Or Br2。
Further, the vacuum pressure in step 2) is 10-2～10-6Pa。
Further, in the step 3), the temperature rising rate is 3-10 ℃/min, and the temperature reducing rate is 3-10 ℃/min.
Further, in the step 4), the specific steps of cleaning are as follows:
1) soaking the mixture in carbon disulfide for 3-6 hours;
2) soaking the mixture in acetone for 3-6 hours;
3) and finally, ultrasonically cleaning the substrate in ethanol for 1-4 hours.
Re of rod-shaped body with layered structure6P13。
Re6P13With carbon materialsThe preparation method of the composite anode material comprises the following steps:
mixing Re with6P13Mixing with a carbon material, and performing ball milling and mixing after mixing to obtain a composite cathode material of rhenium phosphide and the carbon material; wherein the mass ratio of the rhenium phosphide to the carbon material is (4-8): 1.
further, the carbon material is acetylene black, carbon nanotubes, graphene or super P.
Furthermore, the ball milling speed is 300-900 r/min, and the ball milling time is 3-1 h. Compared with the prior art, the invention has the following beneficial effects:
re of the invention6P13The rhenium phosphide material is prepared by a one-step gas transport technology, and the purity of the product prepared by a chemical vapor transport method is higher, so that a safer cathode material is prepared; the layered rhenium phosphide has a rod-shaped structure and a high specific surface area, is beneficial to full contact with electrolyte, ensures that the diffusion path of lithium ions is short, greatly improves the discharge specific capacity and the rate capability of the battery, and improves the quick charge and quick discharge performance of the battery; the electrode conductivity is improved by compounding with the carbon material, the microscopic morphology can be protected from being damaged by the action of physical wrapping or chemical bonding formed between the electrode and the carbon material, and the multiplying power performance of the battery is obviously improved; the gas-phase transport technology for preparing the rhenium oxide has simple production process, is easy for batch preparation and has wide application prospect.
Drawings
FIG. 1 is an XRD pattern of rhenium phosphide prepared in example 1 of the present invention;
FIG. 2 is the crystal structure of rhenium phosphide prepared in example 1 of the present invention;
FIG. 3 is a scanning electron micrograph of rhenium phosphide prepared in example 1 of the present invention;
FIG. 4 is a transmission electron micrograph of rhenium phosphide prepared in example 1 of the present invention;
FIG. 5 is a charge and discharge curve of the first three circles at 0.1A/g of a composite anode material of rhenium phosphide and a carbon material prepared in example 1 of the present invention;
fig. 6 is a rate performance curve of a rhenium phosphide and carbon composite anode material prepared by using example 1 of the present invention.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
chemical vapor transport is an important method for single crystal growth, synthesis of new compounds, purification of substances, and the like. In the method, Re and P can perform correlation action with a gasified transmission agent in a vacuum high-temperature environment to generate a volatile intermediate product, and further can perform interaction to generate Re6P13And depositing the following, wherein the general chemical reaction formula is as follows:
6Re+13P→Re6P13
the product prepared by the chemical vapor transport method has higher purity, and the non-volatile reactant or the product with high purity can be obtained by controlling the temperature gradient.
Example 1
1) Weighing rhenium powder and red phosphorus according to the mass ratio of 6:3.5, mixing under the protection of Ar gas, and placing in a quartz tube with one end sealed;
2) adding I into a quartz tube2Vacuum pumping to 10-6Pa, sealing the other end of the quartz tube; wherein the mass ratio of iodine to the total mass of rhenium and red phosphorus is 1%;
3) use of I2As a transmission agent, a quartz tube is placed in a heating furnace to be heated to 900 ℃ at the speed of 5 ℃/min by a chemical vapor transmission method, and after the temperature is kept for 3 days, the quartz tube is slowly cooled to the room temperature at the speed of 5 ℃/min, and rhenium phosphide powder is grown;
4) taking out the mixture in the quartz tube, firstly soaking in carbon disulfide for 3 hours, then soaking in acetone for 3 hours, finally ultrasonically cleaning in ethanol for 1 hour, and then centrifugally drying in a vacuum drying oven to obtain rhenium phosphide powder;
5) and (2) mixing the components in a mass ratio of 8: mixing the rhenium phosphide powder and the graphene of 1, and then placing the mixture in a high-energy ball mill for ball milling and mixing at the rotating speed of 300r/min for 3 hours to obtain the composite cathode material of the rhenium phosphide and the carbon material.
Referring to fig. 1, fig. 1 is an XRD pattern of rhenium phosphide prepared in example 1 of the present invention; the XRD pattern was obtained from X-ray diffraction analysis of the rhenium phosphide prepared in this example, which was a rhombohedral Re by comparison with a standard JCPDS card6P13Phase, crystal structure is shown in fig. 2;
referring to fig. 3, fig. 3a and 3b are scanning electron microscope images of rhenium phosphide prepared in example 1 of the present invention at different magnifications, and as can be seen from fig. 3, the rhenium phosphide material prepared in this example is a rod-shaped body with a layered structure, has a high specific surface area, and is beneficial to full contact with an electrolyte, so that the diffusion path of lithium ions is short, the specific discharge capacity and the rate capability of a battery are greatly improved, and the fast charge and fast discharge performance of the battery is improved.
Referring to FIG. 4, FIG. 4 is a Transmission Electron Microscope (TEM) image of rhenium phosphide prepared in example 1 of the present invention, and it can be seen from FIG. 4 that the rhenium phosphide material prepared by this example has a rod-like structure with an average diameter of 300 nm.
The lithium ion battery negative electrode material prepared in the embodiment is uniformly ground and mixed with conductive carbon black and polyvinylidene fluoride according to the mass ratio of 8:1:1, a proper amount of N-methyl pyrrolidone (NMP) is added to be prepared into slurry, the slurry is coated on copper foil and dried for 6 hours in a drying oven at 120 ℃, and then the copper foil is cut into pieces to prepare the lithium ion battery negative electrode piece. And assembling the lithium ion battery negative pole piece into a button cell to test the performance of the button cell.
Referring to fig. 5, fig. 5 is a charge and discharge curve of the first three circles at 0.1A/g of the composite anode material of rhenium phosphide and a carbon material prepared in example 1 of the present invention; as can be seen from FIG. 4, the first charge specific capacity of the battery reaches 1249.1 mAh/g.
Referring to fig. 6, fig. 6 is a rate performance curve of a rhenium phosphide and carbon composite anode material prepared by using example 1 of the present invention. As can be seen from FIG. 6, the material has excellent rate capability, and the specific cyclic capacity of the material still reaches 575.9mAh/g under the high current density of 20A/g, which indicates that the battery has better fast charge and fast discharge performance.
Example 2
1) Weighing rhenium powder and red phosphorus according to the mass ratio of 6:4 in the proportion of N2Mechanically mixing in gas atmosphere, and placing in a quartz tube with one sealed end;
2) adding Br into quartz tube2，Br2The mass of (A) is 3% of the total mass of rhenium and red phosphorus, and vacuum pumping is carried out until the mass reaches 10%-2Pa, sealing the other end of the quartz tube;
3) the quartz tube is placed in a heating furnace to be heated to 850 ℃ at the speed of 3 ℃/min, and after the temperature is kept for 12 days, the quartz tube is slowly cooled to the room temperature at the speed of 3 ℃/min, and rhenium phosphide powder is grown;
4) cleaning a product in a quartz tube, respectively soaking for 3 hours by using carbon disulfide and acetone in sequence, then ultrasonically cleaning for 3 hours in ethanol, centrifuging and then placing in a vacuum drying box to obtain rhenium phosphide powder;
5) and (3) mixing the following components in percentage by mass: mixing the rhenium phosphide powder 1 with the super P, and placing the mixture in a high-energy ball mill for ball milling and mixing at the rotating speed of 600r/min for 1.5 hours to obtain the composite cathode material of the rhenium phosphide and the carbon material.
The lithium ion battery negative electrode material prepared in the embodiment is uniformly ground and mixed with conductive carbon black and polyvinylidene fluoride according to the mass ratio of 8:1:1, a proper amount of N-methyl pyrrolidone (NMP) is added to be prepared into slurry, the slurry is coated on copper foil and dried for 6 hours in a drying oven at 120 ℃, and then the copper foil is cut into pieces to prepare the lithium ion battery negative electrode piece.
And assembling the lithium ion battery negative pole piece into a button cell to test the performance of the button cell. The first charging specific capacity of the battery reaches 1131.2mAh/g, and the circulating specific capacity of the battery still reaches 515.3mAh/g under the heavy current density of 20A/g, which indicates that the battery has better performance of quick charge and quick discharge.
Example 3
1) Weighing rhenium powder and red phosphorus in a mass ratio of 6:4.5, mechanically mixing the rhenium powder and the red phosphorus in an Ar atmosphere, and placing the mixture in a quartz tube with one sealed end;
2) adding I into a quartz tube2，I2The mass of (A) is 5% of the total mass of rhenium and red phosphorus, and vacuum pumping is carried out until the mass reaches 10%-4Pa, sealing the other end of the quartz tube;
3) making iodine I2As a transmission agent, heating the quartz tube to 860 ℃ at the speed of 10 ℃/min by a chemical vapor transmission method, preserving the temperature for 5 days, and slowly cooling to room temperature at the speed of 10 ℃/min to grow rhenium phosphide;
4) taking out a product in the quartz tube, soaking the product in carbon disulfide and acetone for 6 hours in sequence, then ultrasonically cleaning the product in ethanol for 4 hours, centrifuging the product, and placing the product in a vacuum drying oven to obtain rhenium phosphide powder;
5) mixing rhenium phosphide powder and carbon nanotubes in a ratio of 4: 1, placing the mixture in a high-energy ball mill for ball milling and mixing at the rotating speed of 900r/min for 1 hour to obtain the composite cathode material of the rhenium phosphide and the carbon material.
The lithium ion battery negative electrode material prepared in the embodiment is uniformly ground and mixed with conductive carbon black and polyvinylidene fluoride according to the mass ratio of 8:1:1, a proper amount of N-methyl pyrrolidone (NMP) is added to be prepared into slurry, the slurry is coated on copper foil and dried for 6 hours in a drying oven at 120 ℃, and then the copper foil is cut into pieces to prepare the lithium ion battery negative electrode piece.
And assembling the lithium ion battery negative pole piece into a button cell to test the performance of the button cell. The first charge specific capacity of the battery reaches 1210.2mAh/g, and the cycle specific capacity of the battery still reaches 523.7mAh/g under the heavy current density of 20A/g, which indicates that the battery has better performance of quick charge and quick discharge.
Example 4
1) Weighing rhenium powder and red phosphorus in a mass ratio of 6:4.5, mechanically mixing the rhenium powder and the red phosphorus in an Ar atmosphere, and placing the mixture in a quartz tube with one sealed end;
2) adding I into a quartz tube2，I2The proportion of the mass of (A) to the total mass of rhenium and red phosphorus is 4%, and the vacuum is drawn to 10%-5Pa, sealing the other end of the quartz tube;
3)I2as a transmission agent, heating the quartz tube to 900 ℃ at 8 ℃/min by a chemical vapor transmission method, preserving the heat for 8 days, and slowly cooling to room temperature at 8 ℃/min to grow rhenium phosphide;
4) taking out a product in the quartz tube, soaking the product in carbon disulfide and acetone for 5 hours in sequence, then ultrasonically cleaning the product in ethanol for 4 hours, centrifuging the product, and placing the product in a vacuum drying oven to obtain rhenium phosphide powder;
5) mixing rhenium phosphide powder and acetylene black in a ratio of 5: 1, placing the mixture in a high-energy ball mill for ball milling and mixing at the rotating speed of 1000r/min for 1 hour to obtain the composite cathode material of the rhenium phosphide and the carbon material.
The lithium ion battery negative electrode material prepared in the embodiment is uniformly ground and mixed with conductive carbon black and polyvinylidene fluoride according to the mass ratio of 8:1:1, a proper amount of N-methyl pyrrolidone (NMP) is added to be prepared into slurry, the slurry is coated on copper foil and dried for 6 hours in a drying oven at 120 ℃, and then the copper foil is cut into pieces to prepare the lithium ion battery negative electrode piece.
And assembling the lithium ion battery negative pole piece into a button cell to test the performance of the button cell. The first charging specific capacity of the battery reaches 1007.2mAh/g, and the circulating specific capacity of the battery still reaches 493.7mAh/g under the heavy current density of 20A/g, which indicates that the battery has better quick charging and discharging performances.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (5)
1. Re6P13The preparation method is characterized by comprising the following steps:
1) mixing rhenium powder and red phosphorus under the atmosphere of inert gas to obtain a two-phase mixture; wherein the mass ratio of rhenium powder to red phosphorus is 6: (3.5-4.5);
2) adding a transmission agent into the two-phase mixture to obtain a three-phase mixture, wherein the pressure of a space where the three-phase mixture is located is vacuum pressure; wherein, the mass ratio of the mass of the transmission agent to the total mass of the rhenium powder and the red phosphorus is 1 to 5 percent;
the vacuum pressure is 10-2～10-6Pa；
3) Heating the three-phase mixture to 850-900 ℃ by adopting a chemical vapor transport method, preserving heat for 3-12 days, and then cooling to obtain a mixture containing rhenium phosphide;
the heating rate is 3-10 ℃/min, and the cooling rate is 3-10 ℃/min;
4) taking out the mixture, and washing, centrifuging and drying the mixture to obtain the rhenium phosphide powder.
2. Re according to claim 16P13The method for producing (1) is characterized in that the atmosphere in the step 1) is nitrogen.
3. Re according to claim 16P13Characterized in that the delivery agent in step 2) comprises I2Or Br2。
4. Re according to claim 16P13Characterized in that, in the step 4), the specific cleaning is carried outThe method comprises the following steps:
1) soaking the mixture in carbon disulfide for 3-6 hours;
2) soaking the mixture in acetone for 3-6 hours;
3) and finally, ultrasonically cleaning the substrate in ethanol for 1-4 hours.
5. Re according to any one of claims 1 to 46P13Re obtained by the preparation method6P13Characterized in that Re6P13Is a rod-shaped body with a laminated structure.
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