CN111747396A - Nitrogen-phosphorus-doped two-dimensional carbon/silicon compound and preparation method and application thereof - Google Patents
Nitrogen-phosphorus-doped two-dimensional carbon/silicon compound and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a nitrogen-phosphorus doped two-dimensional carbon/silicon compound and a preparation method and application thereof, wherein the preparation method comprises the following steps: step 1: dissolving a carbon source in deionized water, then adding a silicon source, uniformly mixing, adding NaCl, and uniformly mixing; drying the mixture to obtain a solid, and grinding the solid into powder; step 2: placing the powder in a tubular furnace, calcining in protective gas, etching away a NaCl template by using deionized water, and drying to obtain a two-dimensional carbon/silicon compound; and step 3: dissolving the two-dimensional carbon/silicon compound and the nitrogen source in deionized water, and stirring; then adding a phosphorus source and stirring; and finally, calcining in protective gas to obtain the nitrogen-phosphorus doped two-dimensional carbon/silicon compound, wherein the compound is low in cost, can be produced in large batch, has a high specific surface area and a good electron transport property, can greatly buffer the volume change of silicon in the lithium desorption process, and has a very good application prospect when applied to a lithium ion battery cathode material.
Description
Technical Field
The invention relates to the field of two-dimensional carbon/silicon compounds, in particular to a nitrogen-phosphorus doped two-dimensional carbon/silicon compound and a preparation method and application thereof.
Background
With the rise of new energy automobiles, rechargeable lithium ion batteries are widely concerned by people.
Silicon is one of the most promising anode candidate materials for next-generation lithium ion batteries in the battery anode material, and has low voltage and high theoretical specific capacity (room temperature forming Li)15Si4Phase 3580mA/h g), and in addition, it is abundant (the second most abundant element in the earth's crust) and environmentally friendly. However, during charge and discharge, the silicon negative electrode expands by about 300% in volume, which destroys electrical contact between particles, causes irreversible pulverization of the negative electrode material, and repeated breakage and increased SEI cause continuous consumption of electrolyte and lithium ions.
Compared with silicon, the layered graphite material has a long life but a relatively low energy density and a theoretical capacity of only 372 mAh/g. Therefore, the silicon-carbon composite material is considered as a promising material and is widely used for relieving the volume expansion of the silicon negative electrode and improving the conductivity thereof, and the silicon-carbon composite material is a hot spot of research at present.
Researchers have conducted various shape and structure researches on silicon-carbon composite materials, such as: compared with the structures, the two-dimensional material has higher specific surface area and better electron transmission performance, so the method has better application prospect, no method for preparing the nitrogen-phosphorus doped two-dimensional carbon/silicon composite cathode material by using NaCl as a template exists at present, and the NaCl template can be cleaned by using deionized water in an environment-friendly manner, so the development of the nitrogen-phosphorus doped two-dimensional carbon silicon composite cathode material which is simple in operation and low in cost and can be prepared in a large amount has important significance.
Disclosure of Invention
In order to overcome the defects of the prior art, the technical problem to be solved by the invention is to provide the following technical scheme.
In a first aspect, a method for preparing a nitrogen-phosphorus-doped two-dimensional carbon/silicon composite is provided, which comprises the following steps: the method comprises the following steps:
step 1: dissolving a carbon source in deionized water, then adding a silicon source, uniformly mixing, adding NaCl, and uniformly mixing; drying the mixture in a drying oven to obtain a solid, and grinding the solid into powder;
step 2: placing the powder in a tubular furnace, calcining in protective gas, etching away a NaCl template by using deionized water, and drying to obtain a two-dimensional carbon/silicon compound;
and step 3: dissolving the two-dimensional carbon/silicon compound and the nitrogen source in deionized water, and stirring; then adding a phosphorus source and stirring; and finally calcining in protective gas to obtain the nitrogen-phosphorus doped two-dimensional carbon/silicon compound.
Preferably, in the step 3, the nitrogen source is dissolved in deionized water and stirred for 1h to 1.5 h; adding a phosphorus source, and stirring for 0.5-1 h.
Preferably, the carbon source is one or more of glucose, starch or citric acid.
Preferably, the silicon source is one or more of simple substance silicon or porous silicon, and the particle diameter is 90nm-110 nm.
Preferably, the mass ratio of the silicon source, the carbon source and the NaCl is 1: (10-20): 200.
preferably, the calcination in the step 2 is heated to 750-900 ℃ at the temperature rising speed of 5-10 ℃/min, and the heat preservation time is 2-6 h.
Preferably, the protective gas in step 2 and step 3 is nitrogen or argon.
Preferably, the nitrogen source in step 3 is one or more of melamine or urea.
Preferably, the phosphorus source in step 3 is one or more of phytic acid or sodium hypophosphite.
Preferably, the calcination in the step 3 is heated to 700-800 ℃ at the temperature rising speed of 5-10 ℃/min, and the heat preservation time is 2-6 h.
Preferably, the drying temperature of the drying oven in the step 1 and the step 2 is 60-85 ℃, and the drying time is 11-13 h.
In a second aspect, a nitrogen-phosphorus-doped two-dimensional carbon/silicon composite is provided, which is prepared by the preparation method of the first aspect.
The third aspect provides the application of the nitrogen-phosphorus doped two-dimensional carbon/silicon composite as the negative electrode material of the lithium ion battery.
By adopting the technical scheme, the nitrogen-phosphorus-doped two-dimensional carbon/silicon compound prepared by the method has the beneficial effects that:
(1) the cost is low, all selected materials are common chemical raw materials, only conventional instruments and equipment are needed, the operation is simple, and mass low-cost production is facilitated;
(2) the NaCl template is low in price, can be removed in an environment-friendly and non-toxic manner only by using deionized water, and can be recycled after extraction, so that pollution is fundamentally removed, and the NaCl template is harmless to the environment;
(3) the nitrogen-phosphorus doped two-dimensional carbon/silicon composite has higher specific surface area and better electron transmission performance, so the nitrogen-phosphorus doped two-dimensional carbon/silicon composite has very good application prospect.
(4) The prepared phosphorus-doped two-dimensional carbon/silicon composite can greatly buffer the volume change of silicon in the process of lithium desorption and insertion, and can be applied to the lithium ion battery cathode material with long service life and high rate performance.
Drawings
Fig. 1 is a scanning and transmission analysis diagram of a nitrogen-phosphorous doped two-dimensional carbon/silicon composite in accordance with the present invention.
FIG. 2 is a mapping analysis diagram of the nitrogen-phosphorus doped two-dimensional carbon/silicon composite of the present invention.
Fig. 3 is an XRD picture of silicon nanoparticles, two-dimensional carbon/silicon composites and nitrogen-phosphorous doped two-dimensional carbon/silicon composites in the present invention.
Fig. 4 is a CV curve of a nitrogen-phosphorus doped two-dimensional carbon/silicon composite in the present invention.
Fig. 5 is a graph of the cycle performance of nitrogen and phosphorus doped two-dimensional carbon/silicon composites of the present invention.
Fig. 6 is a graph of electrochemical rate performance of nitrogen-phosphorus doped two-dimensional carbon/silicon composite in the present invention.
Detailed Description
The invention is further described with reference to the following drawings and detailed description.
Example 1: preparation of nitrogen-phosphorus doped two-dimensional carbon/silicon composite
Step 1: dissolving 1g of glucose in 10mL of deionized water, carrying out ultrasonic treatment until the solution is uniform, then adding 50mg of elemental silicon with the size of 100nm, carrying out ultrasonic treatment until the solution is uniform, then adding 10g of NaCl solid powder, carrying out ultrasonic treatment until the solution is uniform, drying the mixture in a drying oven at 80 ℃ for 12 hours to obtain a massive solid, and grinding the massive solid into sufficiently fine powder in a mortar.
(2) And (2) placing the prepared powder in a burning boat in a tubular furnace, heating to 750 ℃ at a heating rate of 5 ℃/min by using nitrogen as a protective gas, calcining for 2h, cooling along with the furnace, etching the fired powder for 12h by using 200mL of deionized water to remove a NaCl template, and drying in a drying oven at 80 ℃ for 12h after suction filtration to obtain the two-dimensional carbon/silicon composite.
(3) Dispersing 100mg of two-dimensional carbon/silicon compound and 0.25g of melamine in 100ml of deionized water, then vigorously stirring for 1h, then adding 1ml of phytic acid, then vigorously stirring for 0.5h, carrying out suction filtration, drying for 12h in a drying oven at 60 ℃, then heating to 700 ℃ at the heating rate of 5 ℃/min by taking nitrogen as protective gas, calcining for 2h, and then cooling along with a furnace to obtain the nitrogen-phosphorus doped two-dimensional carbon/silicon compound.
Referring to fig. 1, a scanning and transmission electrostatographic analysis of a nitrogen-phosphorous doped two-dimensional carbon/silicon composite is shown:
the scanning picture a shows that the whole body is in a two-dimensional sheet shape, the scanning picture b shows that silicon particles are uniformly embedded in the scanning picture, the transmission picture c verifies the embedded distribution of silicon, the high-resolution transmission picture d shows the lattice stripes of the silicon, and the nitrogen-phosphorus-doped two-dimensional carbon/silicon composite structure is further verified.
Referring to fig. 2, mapping analysis is performed to demonstrate the doped nitrogen and phosphorus elements and their distribution, and the distribution of the doped elements can be seen from the figure.
Referring to fig. 3, XRD patterns of the silicon nanoparticles, the two-dimensional carbon/silicon composite and the nitrogen-phosphorus doped two-dimensional carbon/silicon composite show that:
28.4 degrees, 47.3 degrees and 56.1 degrees of the nitrogen-phosphorus doped two-dimensional carbon/silicon composite respectively correspond to crystal faces (111), (220) and (311) of pure silicon (JCPDS No. 27-1402). The carbon peak in XRD of the nitrogen-phosphorus doped two-dimensional carbon/silicon composite is stronger than that of the two-dimensional carbon/silicon composite because carbon is introduced again by phytic acid and melamine.
Referring to fig. 4, the CV curve of the nitrogen-phosphorus doped two-dimensional carbon/silicon composite can be seen as follows:
reversible storage performance of the nitrogen-phosphorus doped two-dimensional carbon/silicon compound: six voltammetric curves were tested at a sweep rate of 0.1mV/s and a voltage window of 0.01V-2V. The first cycle exhibited a broad cathodic peak in about 0.61V due to the formation of an irreversible SEI film, which disappeared in subsequent cycles. The subsequent cathodic scan showed a cathodic peak at about 0.22V due to the crystalline to amorphous transformation of the silicon structure. Peaks below 0.5V indicate coexistence of multiple LixSi phases. The anodic scan has oxidation peaks of about 0.3V and 0.55V, corresponding to the transition from amorphous LixSi to crystalline Si.
Please refer to fig. 5 and 6, which are a cycle performance diagram of the two-dimensional carbon/silicon composite doped with nitrogen and phosphorus and an electrochemical rate performance diagram of the two-dimensional carbon/silicon composite doped with nitrogen and phosphorus, respectively.
The figure shows that the nitrogen-phosphorus doped two-dimensional carbon/silicon composite has excellent electrochemical rate capability and cycle performance, the initial charging specific capacity is 654mAh/g after 100 cycles of cycle under the current density of 0.2A/g, the charging specific capacity is 593mAh/g after 100 cycles of cycle, the capacity retention rate is 90.6%, the cycle stability is very good, and the high current also keeps good stability in a rate test, so that the material has good application prospect.
Example 2:
the difference from example 1 is that the carbon source was changed to starch, and a nitrogen-phosphorus doped two-dimensional carbon/silicon composite was obtained.
Example 3:
the difference from example 1 is that the carbon source was changed to citric acid to obtain a nitrogen-phosphorus doped two-dimensional carbon/silicon composite.
Example 4:
the difference from example 1 is that the silicon source was replaced by porous silicon to obtain a nitrogen-phosphorus doped two-dimensional carbon/silicon composite.
Example 5:
the difference from the embodiment 1 is that the mass ratio of the silicon source, the carbon source and the template NaCl in the embodiment is 1:15:200, so as to obtain the nitrogen-phosphorus doped two-dimensional carbon/silicon composite.
Example 6:
the difference from the embodiment 1 is that the mass ratio of the silicon source, the carbon source and the template NaCl in the embodiment is 1:10:200, so as to obtain the nitrogen-phosphorus doped two-dimensional carbon/silicon composite.
Example 7:
the difference from the embodiment 1 is that the calcination in the step 1 of the embodiment is heated to 900 ℃ at a heating rate of 10 ℃/min, the heat preservation time is 6h, and other steps are the same as the embodiment 1, so that the nitrogen-phosphorus doped two-dimensional carbon/silicon composite negative electrode material is obtained.
Example 8:
the difference from example 1 is that the protective gas in this example is argon.
Example 9:
the difference from example 1 is that the nitrogen source in this example is urea.
Example 10:
the difference from example 1 is that the phosphorous source in this example is sodium hypophosphite.
Example 11:
the difference from example 1 is that the calcination in step 3 of this example is heated to 800 ℃ at a heating rate of 10 ℃/min, and the holding time is 6 h.
While the invention has been particularly shown and described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of a nitrogen-phosphorus doped two-dimensional carbon/silicon compound is characterized by comprising the following steps:
step 1: dissolving a carbon source in deionized water, then adding a silicon source, uniformly mixing, adding NaCl, and uniformly mixing; drying the mixture in a drying oven to obtain a solid, and grinding the solid into powder;
step 2: placing the powder in a tubular furnace, calcining in protective gas, then removing a NaCl template by using deionized water for etching, and drying to obtain a two-dimensional carbon/silicon compound;
and step 3: dissolving the two-dimensional carbon/silicon compound and the nitrogen source in deionized water, and stirring; then adding a phosphorus source and stirring; and finally calcining in protective gas to obtain the nitrogen-phosphorus doped two-dimensional carbon/silicon compound.
2. The method for preparing the nitrogen-phosphorus-doped two-dimensional carbon/silicon composite according to claim 1, wherein in the step 3, a nitrogen source is dissolved in deionized water and stirred for 1-1.5 hours; adding a phosphorus source, and stirring for 0.5-1 h.
3. The method for preparing the nitrogen-phosphorus-doped two-dimensional carbon/silicon composite according to claim 1, wherein the carbon source is one or more of glucose, starch or citric acid.
4. The method for preparing the nitrogen-phosphorus-doped two-dimensional carbon/silicon composite as claimed in claim 1, wherein the silicon source is one or more of elemental silicon or porous silicon, and the particle diameter is 90nm-110 nm.
5. The method for preparing the nitrogen-phosphorus-doped two-dimensional carbon/silicon composite according to any one of claims 1 to 4, wherein the mass ratio of the silicon source to the carbon source to the NaCl is 1: (10-20): 200.
6. the preparation method of the nitrogen-phosphorus-doped two-dimensional carbon/silicon composite as claimed in claim 1, wherein the calcination in the step 2 is performed at a heating rate of 5 ℃/min to 10 ℃/min to 750 ℃ to 900 ℃ and a holding time of 2h to 6 h.
7. The method for preparing the nitrogen-phosphorus-doped two-dimensional carbon/silicon composite according to claim 1, wherein the protective gas in the steps 2 and 3 is nitrogen or argon; in the step 3, the nitrogen source is one or more of melamine or urea; in the step 3, the phosphorus source is one or more of phytic acid and sodium hypophosphite; in the step 3, the calcination is heated to 700-800 ℃ at the heating rate of 5-10 ℃/min, and the heat preservation time is 2-6 h.
8. The preparation method of the nitrogen-phosphorus-doped two-dimensional carbon/silicon composite according to claim 1, wherein the drying temperature of the drying oven in the step 1 and the drying oven in the step 2 is 60-85 ℃, and the drying time is 11-13 h.
9. A nitrogen-phosphorus-doped two-dimensional carbon/silicon composite, which is prepared by the preparation method of any one of claims 1 to 8.
10. The use of the nitrogen-phosphorus doped two-dimensional carbon/silicon composite of claim 9 as a negative electrode material for a lithium ion battery.
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| CN113363455A (en) * | 2021-06-04 | 2021-09-07 | 广东工业大学 | Composite two-dimensional micron-sized silicon wafer and preparation method thereof |
| CN113745509A (en) * | 2021-08-09 | 2021-12-03 | 华侨大学 | Phosphorus-nitrogen doped biomass hard carbon material and preparation method and application thereof |
| CN113816384A (en) * | 2021-08-30 | 2021-12-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of phosphorus-doped porous carbon-coated silica material and product thereof |
| CN114105149A (en) * | 2021-10-12 | 2022-03-01 | 湖南金硅科技有限公司 | Carbon-coated nitrogen-phosphorus double-doped silicon monoxide composite material, preparation method thereof and application thereof in lithium ion battery |
| CN114156457A (en) * | 2021-11-18 | 2022-03-08 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of nitrogen-phosphorus co-doped porous carbon-coated silicon-based material |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113363455A (en) * | 2021-06-04 | 2021-09-07 | 广东工业大学 | Composite two-dimensional micron-sized silicon wafer and preparation method thereof |
| CN113745509A (en) * | 2021-08-09 | 2021-12-03 | 华侨大学 | Phosphorus-nitrogen doped biomass hard carbon material and preparation method and application thereof |
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| CN113816384A (en) * | 2021-08-30 | 2021-12-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of phosphorus-doped porous carbon-coated silica material and product thereof |
| CN113816384B (en) * | 2021-08-30 | 2023-07-18 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of phosphorus-doped porous carbon-coated silicon oxide material and product thereof |
| CN114105149A (en) * | 2021-10-12 | 2022-03-01 | 湖南金硅科技有限公司 | Carbon-coated nitrogen-phosphorus double-doped silicon monoxide composite material, preparation method thereof and application thereof in lithium ion battery |
| CN114105149B (en) * | 2021-10-12 | 2023-09-22 | 湖南金硅科技有限公司 | Carbon-coated nitrogen-phosphorus double-doped silicon oxide composite material, preparation method thereof and application thereof in lithium ion battery |
| CN114156457A (en) * | 2021-11-18 | 2022-03-08 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of nitrogen-phosphorus co-doped porous carbon-coated silicon-based material |
| CN114566637A (en) * | 2022-02-08 | 2022-05-31 | 泾河新城陕煤技术研究院新能源材料有限公司 | Preparation method of heteroatom doped silicon-carbon negative electrode material and material thereof |
| CN114566637B (en) * | 2022-02-08 | 2024-02-02 | 泾河新城陕煤技术研究院新能源材料有限公司 | Preparation method of heteroatom doped silicon-carbon anode material and material thereof |
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