CN110176602B - Preparation process of phosphorus-doped biomass three-dimensional porous carbon nano electrode material for long-life sodium-ion battery - Google Patents
Preparation process of phosphorus-doped biomass three-dimensional porous carbon nano electrode material for long-life sodium-ion battery Download PDFInfo
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Abstract
The invention discloses a preparation process of a phosphorus-doped biomass three-dimensional porous carbon nano electrode material for a long-life sodium ion battery, which comprises the steps of sequentially ultrasonically cleaning biomass waste by deionized water and ethanol, drying and crushing the biomass waste into powder, and sieving the powder to obtain powder A; adding a phosphoric acid solution into the powdery A, and performing ultrasonic-assisted mixing to obtain a mixture B; transferring the mixture B into a hydrothermal induction kettle, taking the added carbon cloth as an induction source, transferring the hydrothermal induction kettle into hydrothermal induction heating equipment for reaction, cooling to room temperature, taking out the carbon cloth, scraping the obtained product, washing with deionized water and ethanol, performing suction filtration, and drying to obtain C; mixing the C with a phosphorus source, calcining, cooling to room temperature, washing the obtained product with deionized water and ethanol, and centrifuging to obtain D; and activating the D to obtain the phosphorus-doped biomass three-dimensional porous carbon nano electrode material.
Description
Technical Field
The invention belongs to the field of preparation of a sodium ion battery cathode material, and particularly relates to a preparation process of a phosphorus-doped biomass three-dimensional porous carbon nano electrode material for a long-life sodium ion battery.
Background
Lithium ion batteries have been widely used in people's daily lives. In the face of increasing lithium ion battery demands, the situation of resource exhaustion of lithium ores which can be exploited on the earth is faced, and from the perspective of sustainable development, the search for novel batteries is inevitable. The sodium element and the lithium element are in the same main group and have similar properties, and the earth abundance of the sodium element is more than 400 times that of the lithium element, so that the development of a novel sodium-ion battery is trended. Among them, research on negative electrode materials of sodium ion batteries has become a hot spot.
The biomass carbon prepared from the biomass material has the properties of light weight, rich pore structure, large specific surface area, good structural stability, excellent conductivity and the like, and can be applied to the cathode material of the sodium-ion battery. The existing research shows that the capacitance and the rate capability of the biomass carbon as the negative electrode material of the sodium-ion battery need to be improved. Introducing impurity atoms into biomass carbon materials has become an effective method for improving electrochemical performance.
The introduction of heteroatoms such as nitrogen, sulfur, phosphorus or boron into the porous biomass carbon material can significantly improve the electrochemical, mechanical or electrical conductivity of the porous biomass carbon material. Particularly, the phosphorus element can partially replace the carbon element, change the morphological structure of the biomass carbon, provide larger space for the intercalation process of sodium ions, reduce the volume expansion and the adsorption energy of the sodium ions, and improve the capacity of the sodium ion battery. After the phosphorus is doped, the diffusion rate and the electron transmission performance of sodium ions can be improved, and the conductivity is favorably improved, so that the multiplying power performance of the sodium ion battery is improved. For example, Wang et al ([ J ]. RSC adv.2015,5(68): 55136-. The process is complex, the energy consumption is high, and the silicon element of the large material in the raw material is also removed. Therefore, the method has important significance in developing a process which has wide raw material sources, low cost, excellent electrochemical performance, simplicity, controllability and good repeatability to prepare the phosphorus-doped porous carbon nano material.
Disclosure of Invention
The invention aims to provide a preparation process of a phosphorus-doped biomass three-dimensional porous carbon nano electrode material for a long-life sodium-ion battery, so as to overcome the defects in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation process of a phosphorus-doped biomass three-dimensional porous carbon nano electrode material for a long-life sodium ion battery comprises the following steps:
1) sequentially ultrasonically cleaning the biomass waste by using deionized water and ethanol, drying and crushing the biomass waste into powder, and sieving the powder to obtain powder A;
2) adding a phosphoric acid solution into the powdery A, and performing ultrasonic-assisted mixing to obtain a mixture B;
3) transferring the mixture B into a hydrothermal induction kettle, taking the added carbon cloth as an induction source, moving the hydrothermal induction kettle into hydrothermal induction heating equipment, heating the hydrothermal induction kettle to 150-180 ℃ from room temperature at an induction frequency of 200-500 KHz, preserving heat for 20-50 min, cooling to room temperature, taking out the carbon cloth, scraping the obtained product, washing with deionized water and ethanol, filtering, and drying to obtain C;
4) mixing the C and a phosphorus source, heating to 500-700 ℃ at a heating rate of 3 ℃/min, preserving heat for 1-3 h, cooling to room temperature, washing the obtained product with deionized water and ethanol, and centrifuging to obtain D;
5) and heating the D to 300 ℃ at a heating rate of 3-10 ℃, and preserving heat for 5-8 h for activation to obtain the phosphorus-doped biomass three-dimensional porous carbon nano-electrode material.
Further, the biomass waste in the step 1) is nutshell, egg shell, coffee shell or coconut shell.
Further, the ultrasonic cleaning frequency in the step 1) is 30KHz, and the time is 1 h.
Further, the drying in the step 1) is specifically as follows: and drying for 3-6 h by adopting an infrared lamp.
Further, crushing the mixture obtained in the step 1) into powder, and sieving the powder through a 300-600-mesh sieve to obtain powder A.
Further, in the step 2), 1-4 g of powdery A is added into every 40-70 mL of phosphoric acid solution, and the concentration of the phosphoric acid solution is 1-3 mol/L.
Further, the ultrasonic frequency in the step 2) is 20-40 KHz, and the time is 10-30 min.
Further, the length, the width and the height of the carbon cloth in the step 3) are respectively 3cm, 3cm and 0.1cm, and the drying temperature in the step 3) is 70 ℃ and the time is 6 hours.
Further, in the step 4), the phosphorus source is sodium dihydrogen phosphate, potassium dihydrogen phosphate, solid phosphoric acid or elemental phosphorus.
Further, the mass ratio of C to the phosphorus source in the step 4) is (1-2): (1-6).
Compared with the prior art, the invention has the following beneficial technical effects:
1. the invention selects the biomass waste as the biomass carbon source, changes waste into valuable, is environment-friendly, and has extremely high resource advantage and cost advantage.
2. The preparation process of the sodium-ion battery cathode material provided by the invention is simple, the conditions are mild and controllable, the production cost is low, the repeatability is high, and the industrial production is easy to realize.
3. The negative electrode material of the sodium ion battery synthesized by the invention has a three-dimensional nano porous phosphorus-containing structure and larger interlayer spacing. The method is beneficial to intercalation of sodium ions, can provide a large number of reaction active sites, and effectively increases the adsorption rate, diffusion rate and electron transmission rate of the sodium ions.
4. The phosphorus-doped biomass porous carbon nanomaterial prepared by the invention can be applied to a sodium ion battery, can obviously prolong the cycle life of the battery, and has high capacity, excellent cycle stability, thermal stability, chemical stability and mechanical flexibility.
Drawings
FIG. 1 is an SEM image of a phosphorus-doped biomass porous carbon nanomaterial prepared in example 2;
FIG. 2 is an XRD pattern of the phosphorus doped biomass porous carbon nanomaterial prepared in example 2;
fig. 3 is a graph of the cycle performance of the phosphorus-doped biomass porous carbon nanomaterial prepared in example 2.
Detailed Description
Embodiments of the invention are described in further detail below:
a preparation process of a phosphorus-doped biomass three-dimensional porous carbon nano electrode material for a long-life sodium ion battery. The phosphorus-doped porous carbon nanomaterial can form a sample with a cellular porous three-dimensional carbon nanostructure after hydrothermal induction and carbonization treatment. The electrode material is simple in preparation process, environment-friendly in raw materials, wide in source, capable of changing waste into valuable, and excellent in long-cycle performance when applied to lithium ion batteries.
The method specifically comprises the following steps:
1. ultrasonically cleaning biomass waste such as nut shells, egg shells, coffee shells and coconut shells for 1h by deionized water and ethanol at the frequency of 30KHz in sequence, drying for 3-6 h by using an infrared lamp, crushing into powder by using a crusher, and sieving by using a 300-600-mesh sieve to obtain A;
2. weighing 1-4 g A, adding 40-70 ml of phosphoric acid solution with the concentration of 1-3 mol/L into the powdery A, and carrying out ultrasonic treatment for 10-30 min at the frequency of 20-40 KHz by using an ultrasonic machine to obtain a mixture B.
3. And transferring the mixture B into a hydrothermal induction kettle, and adding carbon cloth with the length, width and height of 3cm, 3cm and 0.1cm as an induction source. Moving the hydrothermal induction kettle into hydrothermal induction heating equipment, heating the hydrothermal induction kettle to 150-180 ℃ from room temperature at an induction frequency of 200-500 KHz, preserving the heat for 20-50 min, cooling to room temperature, taking out carbon cloth, scraping the obtained product, washing with deionized water and ethanol, performing suction filtration, and drying in a 70 ℃ drying oven for 6h to obtain C;
4. mixing the C with a phosphorus source (one or more of sodium dihydrogen phosphate, potassium dihydrogen phosphate, solid phosphoric acid and elemental phosphorus) according to a mass ratio of C: and (3) mixing the phosphorus source in a ratio of 2:1, 1:2, 1:4 and 1:6, then moving the mixture to a tubular furnace, raising the temperature to 500-700 ℃ at a heating rate of 3 ℃/min, preserving the heat for 1-3 h, cooling the mixture to room temperature, and washing and centrifuging the obtained product by using deionized water and ethanol to obtain D.
5. And (3) activating the D in an oven, heating to 300 ℃ at a heating rate of 3-10 ℃, and preserving heat for 5-8 hours to obtain the phosphorus-doped biomass three-dimensional porous carbon nano electrode material.
The present invention is described in further detail below with reference to examples:
example 1
1. Ultrasonically cleaning biomass waste nutshells for 1h by deionized water and ethanol at the frequency of 30KHz in sequence, drying for 3h by an infrared lamp, crushing into powder by a crusher, and sieving by a 300-mesh sieve to obtain A;
2. weighing 1g A, adding 40ml of phosphoric acid solution with the concentration of 1mol/L into the powder A, and carrying out ultrasonic treatment for 10min at the frequency of 20KHz by using an ultrasonic machine to obtain a mixture B.
3. And transferring the mixture B into a hydrothermal induction kettle, and adding carbon cloth with the length, width and height of 3cm, 3cm and 0.1cm as an induction source. Moving the hydrothermal induction kettle into hydrothermal induction heating equipment, heating the hydrothermal induction kettle to 150 ℃ from room temperature at an induction frequency of 200KHz, preserving heat for 20min, cooling to room temperature, taking out carbon cloth, scraping the obtained product, washing with deionized water and ethanol, performing suction filtration, and drying in a 70 ℃ drying oven for 6h to obtain C;
4. mixing the C and phosphorus-derived sodium dihydrogen phosphate according to the mass ratio of C: and D, mixing the sodium dihydrogen phosphate with the ratio of 2:1, moving the mixture to a tubular furnace, heating to 500 ℃ at the heating rate of 3 ℃/min, keeping the temperature for 1h, cooling to room temperature, washing the obtained product with deionized water and ethanol, and centrifuging to obtain D.
5. And (3) putting the D into an oven for activation, heating to 300 ℃ at a heating rate of 3 ℃, and preserving heat for 5 hours to obtain the phosphorus-doped biomass three-dimensional porous carbon nano-electrode material.
Example 2
1. Ultrasonically cleaning eggshells of the biomass waste by deionized water and ethanol for 1 hour in sequence at the frequency of 30KHz, drying for 4 hours by using an infrared lamp, crushing into powder by using a crusher, and sieving by using a 400-mesh sieve to obtain A;
2. weighing 2g A, adding 50ml of 2mol/L phosphoric acid solution into the powder A, and performing ultrasonic treatment at 30KHz frequency for 20min by using an ultrasonic machine to obtain a mixture B.
3. And transferring the mixture B into a hydrothermal induction kettle, and adding carbon cloth with the length, width and height of 3cm, 3cm and 0.1cm as an induction source. Moving the hydrothermal induction kettle into hydrothermal induction heating equipment, heating the hydrothermal induction kettle to 160 ℃ from room temperature at an induction frequency of 300KHz, preserving heat for 30min, cooling to room temperature, taking out carbon cloth, scraping the obtained product, washing with deionized water and ethanol, performing suction filtration, and drying in a 70 ℃ drying oven for 6h to obtain C;
4. mixing the C and potassium dihydrogen phosphate according to the mass ratio of C: and D, mixing the monopotassium phosphate at the ratio of 1:2, moving the mixture to a tubular furnace, heating to 600 ℃ at the heating rate of 3 ℃/min, preserving the heat for 2 hours, cooling to room temperature, washing the obtained product with deionized water and ethanol, and centrifuging to obtain D.
5. And (3) putting the D into an oven for activation, heating to 300 ℃ at the temperature rising rate of 5 ℃, and preserving heat for 6 hours to obtain the phosphorus-doped biomass three-dimensional porous carbon nano electrode material.
Example 3
1. Ultrasonically cleaning a biomass waste coffee shell for 1h by deionized water and ethanol in sequence at a frequency of 30KHz, drying for 5h by an infrared lamp, crushing into powder by a crusher, and sieving by a sieve of 500 meshes to obtain A;
2. 3g A was weighed, 60ml of 2mol/L phosphoric acid solution was added to the powder A, and the mixture was sonicated with a sonicator at 30KHz for 20min to obtain a mixture B.
3. And transferring the mixture B into a hydrothermal induction kettle, and adding carbon cloth with the length, width and height of 3cm, 3cm and 0.1cm as an induction source. Moving the hydrothermal induction kettle into hydrothermal induction heating equipment, heating the hydrothermal induction kettle to 170 ℃ from room temperature at an induction frequency of 400KHz, preserving heat for 40min, cooling to room temperature, taking out carbon cloth, scraping the obtained product, washing with deionized water and ethanol, performing suction filtration, and drying in a 70 ℃ drying oven for 6h to obtain C;
4. mixing the C with phosphorus source solid phosphoric acid according to the mass ratio of C: mixing the solid phosphoric acid with the proportion of 1:4, moving the mixture to a tubular furnace, heating to 600 ℃ at the heating rate of 3 ℃/min, preserving the heat for 2h, cooling to room temperature, washing the obtained product with deionized water and ethanol, and centrifuging to obtain D.
5. And (3) putting the D into an oven for activation, heating to 300 ℃ at the heating rate of 5 ℃, and preserving heat for 7 hours to obtain the phosphorus-doped biomass three-dimensional porous carbon nano-electrode material.
Example 4
1. Ultrasonically cleaning biomass waste coconut shells for 1h by deionized water and ethanol at the frequency of 30KHz in sequence, drying for 6h by an infrared lamp, crushing into powder by a crusher, and sieving by a 600-mesh sieve to obtain A;
2. weighing 4g A, adding 70ml phosphoric acid solution with concentration of 3mol/L into the powder A, and performing ultrasonic treatment at 40KHz frequency for 30min by using an ultrasonic machine to obtain a mixture B.
3. And transferring the mixture B into a hydrothermal induction kettle, and adding carbon cloth with the length, width and height of 3cm, 3cm and 0.1cm as an induction source. Moving the hydrothermal induction kettle into hydrothermal induction heating equipment, heating the hydrothermal induction kettle to 180 ℃ from room temperature at the induction frequency of 500KHz, preserving the heat for 50min, cooling to room temperature, taking out carbon cloth, scraping the obtained product, washing with deionized water and ethanol, performing suction filtration, and drying in a 70 ℃ drying oven for 6h to obtain C;
4. mixing the C with phosphorus source simple substance phosphorus according to the mass ratio of C: mixing the elemental phosphorus in the ratio of 1:6, moving the mixture to a tubular furnace, heating the mixture to 700 ℃ at the heating rate of 3 ℃/min, preserving the heat for 3 hours, cooling the mixture to room temperature, and washing and centrifuging the obtained product by deionized water and ethanol to obtain D.
5. And (3) activating the D in an oven, heating to 300 ℃ at a heating rate of 10 ℃, and preserving heat for 8 hours to obtain the phosphorus-doped biomass three-dimensional porous carbon nano-electrode material.
As can be seen from the SEM image of fig. 1, the phosphorus-doped biomass nanomaterial prepared in example 2 has a three-dimensional honeycomb-shaped morphology structure with both large and small apertures, and has thinner aperture walls. As can be seen from the XRD pattern of fig. 2, the sample of example 2 has more distinct graphite peaks at 24 ° and 43 ° 2 θ angles, indicating that the sample has a higher degree of graphitization. As can be seen from the cycle performance chart of FIG. 3, the samples of example 2 assembled into a sodium ion battery at 50mAg-1The capacity can reach 307mAhg at the current density-1The capacity retention rate is more than 90% after 500 cycles of circulation, and the composite material has high capacity and excellent circulation stability.
Claims (7)
1. A preparation process of a phosphorus-doped biomass three-dimensional porous carbon nano electrode material for a long-life sodium ion battery is characterized by comprising the following steps of:
1) sequentially ultrasonically cleaning the biomass waste by using deionized water and ethanol, drying and crushing the biomass waste into powder, and sieving the powder to obtain powder A;
2) adding a phosphoric acid solution into the powdery A, adding 1-4 g of the powdery A into every 40-70 mL of the phosphoric acid solution, wherein the concentration of the phosphoric acid solution is 1-3 mol/L, and performing ultrasonic-assisted mixing to obtain a mixture B;
3) transferring the mixture B into a hydrothermal induction kettle, taking the added carbon cloth as an induction source, moving the hydrothermal induction kettle into hydrothermal induction heating equipment, heating the hydrothermal induction kettle to 150-180 ℃ from room temperature at an induction frequency of 200-500 KHz, preserving heat for 20-50 min, cooling to room temperature, taking out the carbon cloth, scraping the obtained product, washing with deionized water and ethanol, filtering, and drying to obtain C;
4) mixing the C and a phosphorus source, heating to 500-700 ℃ at a heating rate of 3 ℃/min, preserving heat for 1-3 h, cooling to room temperature, washing an obtained product with deionized water and ethanol, and centrifuging to obtain D, wherein the phosphorus source is sodium dihydrogen phosphate, potassium dihydrogen phosphate, solid phosphoric acid or elemental phosphorus, and the mass ratio of the C to the phosphorus source is (1-2): (1-6);
5) and heating the D to 300 ℃ at a heating rate of 3-10 ℃, and preserving heat for 5-8 h for activation to obtain the phosphorus-doped biomass three-dimensional porous carbon nano-electrode material.
2. The preparation process of the phosphorus-doped biomass three-dimensional porous carbon nano-electrode material for the long-life sodium-ion battery as claimed in claim 1, wherein the biomass waste in step 1) is nutshell, eggshell, coffee shell or coconut shell.
3. The preparation process of the phosphorus-doped biomass three-dimensional porous carbon nano electrode material for the long-life sodium ion battery as claimed in claim 1, wherein the ultrasonic cleaning frequency in the step 1) is 30KHz, and the time is 1 h.
4. The preparation process of the phosphorus-doped biomass three-dimensional porous carbon nano-electrode material for the long-life sodium-ion battery according to claim 1, characterized in that the drying in the step 1) is specifically as follows: and drying for 3-6 h by adopting an infrared lamp.
5. The preparation process of the phosphorus-doped biomass three-dimensional porous carbon nano-electrode material for the long-life sodium-ion battery according to claim 1, characterized in that the phosphorus-doped biomass three-dimensional porous carbon nano-electrode material is crushed into powder in step 1) and then sieved with a 300-600-mesh sieve to obtain powder A.
6. The preparation process of the phosphorus-doped biomass three-dimensional porous carbon nano electrode material for the long-life sodium ion battery as claimed in claim 1, wherein the ultrasonic frequency in the step 2) is 20-40 KHz, and the time is 10-30 min.
7. The preparation process of the phosphorus-doped biomass three-dimensional porous carbon nano electrode material for the long-life sodium-ion battery as claimed in claim 1, wherein the length, the width and the height of the carbon cloth in the step 3) are respectively 3cm, 3cm and 0.1cm, and the drying temperature in the step 3) is 70 ℃ and the drying time is 6 hours.
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| CN112010302A (en) * | 2020-09-07 | 2020-12-01 | 合肥工业大学 | Method for preparing hierarchical porous phosphorus-doped carbon material from biomass |
| CN113381014B (en) * | 2021-06-08 | 2023-03-03 | 西安亚弘泰新能源科技有限公司 | Preparation method of ultralow-temperature lithium ion battery negative electrode material |
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