CN111883754A - Iron nitride-ordered mesoporous carbon composite material and preparation method and application thereof - Google Patents
Iron nitride-ordered mesoporous carbon composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a ferric nitride-ordered mesoporous carbon composite material, which takes ordered mesoporous carbon as a carrier, and ferric nitride nano particles are uniformly distributed on the surface and in the inner pore canal of the ordered mesoporous carbon. The invention also discloses a preparation method of the iron nitride-ordered mesoporous carbon composite material and application of the iron nitride-ordered mesoporous carbon composite material as a negative electrode active substance of a lithium ion battery. According to the invention, the high specific capacity of the iron nitride is combined with the cycling stability of the ordered mesoporous carbon to prepare the composite material of the iron nitride and the ordered mesoporous carbon, so that the problem of low specific capacity of the lithium ion battery cathode material is effectively solved.
Description
Technical Field
The invention relates to the technical field of lithium ion battery cathode materials, in particular to a ferric nitride-ordered mesoporous carbon composite material and a preparation method and application thereof.
Background
With the rapid development of global economy, the current society faces many problems to be solved, such as energy shortage, environmental pollution, climate deterioration, etc. Therefore, people are more eagerly expected to research clean recyclable energy, and lithium ion batteries are more and more concerned by people due to the characteristics of cleanness, no pollution, convenience in carrying, stable cycle performance and the like. The cathode material is one of four materials of the lithium ion battery, and has important significance. The main function of the negative electrode material is to provide a chemical reaction active site for lithium ion intercalation, directly determine the energy density of the lithium ion battery, and pay more and more attention to the demand of people on a high-energy-density power supply, so that the research on the high-capacity negative electrode material is particularly important for the lithium ion battery.
The traditional commercial negative electrode material of the lithium ion battery mainly takes graphite or carbon material as a main material, although the negative electrode cycling performance of the carbon material as the lithium ion battery material is very stable, the theoretical capacity of the negative electrode material is only 372 mAh/g. It is the lower gram volume of carbon materials that limits their use in high energy density power supplies.
With the continuous development of science and technology, people continuously deepen the understanding of lithium ion battery cathode materials, and silicon-based materials, metal oxides and metal nitrides are sequentially used as the cathode materials of the lithium ion battery. Silicon in the silicon-based material can form Li with lithium4.4The lithium storage capacity of the Si alloy can reach 4200mAh/g theoretically, which is equivalent to 10 times of the graphite capacity. But silicon-based materials have an extremely fatal drawback: formation of Li from silicon and lithium4.4When the Si alloy is used, the volume expansion is up to 320%, and the huge volume change easily causes the active substances to fall off from the current collector, so that the electrical contact between the active substances and the current collector is reduced, and the cycle performance of the electrode is rapidly reduced. The metal nitride has high specific capacity and good electrochemical performance, and lithium ions can be combined with N to form a lithium intercalation compound Li3N, has good conductivity. Wherein the transition metal nitride Fe2N has high lithium storage capacity as the negative electrode material of the lithium ion battery if single Fe is used2The N material is used as the cathode of the lithium ion battery, and the active material Fe can be generated by the insertion and the extraction of lithium ions in the battery circulation process2The volume expansion of N becomes large, so that the structure of the negative electrode material collapses and fails, and the cycle performance is influenced.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a ferric nitride-ordered mesoporous carbon composite material and a preparation method and application thereof.
The invention provides a ferric nitride-ordered mesoporous carbon composite material, which takes ordered mesoporous carbon as a carrier, and ferric nitride nano particles are uniformly distributed on the surface and in the inner pore canal of the ordered mesoporous carbon.
Preferably, the preparation method of the ordered mesoporous carbon material comprises the following steps: the preparation method comprises the steps of uniformly dispersing the ordered mesoporous silica template in water, adding a water-soluble carbon source to dissolve the ordered mesoporous silica template completely to obtain a mixed solution, carrying out freeze drying on the mixed solution, carrying out high-temperature carbonization in a protective atmosphere, and removing the ordered mesoporous silica template to obtain the composite material.
Preferably, the mass ratio of the ordered mesoporous silica template to the water-soluble carbon source is 1 (0.5-1.5), and the mass ratio of the ordered mesoporous silica template to the water is 1: (10-50).
Preferably, the water-soluble carbon source is a water-soluble saccharide substance, preferably glucose or sucrose; the ordered mesoporous silica template is a KIT-6 template or an SBA-15 template.
Preferably, the carbonization temperature is 400-1000 ℃, and the heating rate is 1-5 ℃/min; the method for removing the ordered mesoporous silica template comprises the following steps: and washing by adopting a hydrofluoric acid solution with the mass fraction of 1-20%.
The preparation method of the iron nitride-ordered mesoporous carbon composite material comprises the following steps:
s1, uniformly dispersing the ordered mesoporous carbon in water, adding a water-soluble iron source to dissolve completely, and then drying to obtain a precursor;
and S2, performing high-temperature ammoniation on the precursor in an ammonia atmosphere to obtain the ferric nitride-ordered mesoporous carbon composite material.
The mass ratio of the ordered mesoporous carbon to the water-soluble iron source is 1: (1-10), wherein the mass ratio of the ordered mesoporous carbon to the water is 1: (10-200); preferably, the mass ratio of the ordered mesoporous carbon to the water-soluble iron source is 1: 5.
Preferably, the iron source is a trivalent soluble iron salt.
Preferably, in the step S2, the flow rate of the ammonia gas for high-temperature ammoniation is 50-200 mL/S, the temperature is 400-1000 ℃, and the temperature rise rate is 1-5 ℃/min.
The application of the iron nitride-ordered mesoporous carbon composite material as a negative active material of a lithium ion battery.
The invention has the following beneficial effects:
the invention combines the high specific capacity of the iron nitride with the cycling stability of the ordered mesoporous carbon to prepare the composite material of the iron nitride and the ordered mesoporous carbon, and the ordered mesoporous carbon has larger specific surface area and abundant pore channel structures and can provide abundant attachment sites for the iron nitride, so that the iron nitride is uniformly distributed on the surface and in the internal pore channels in a nanometer size, and the prepared composite material has the following advantages: on one hand, the ferric nitride has extremely high lithium storage capacity, and can improve the gram capacity of the composite material, so that the composite material has larger specific capacity; on the other hand, the structure of the ordered mesoporous carbon is stable, the volume change of the composite material caused by the insertion and the extraction of lithium ions can be restricted when the negative plate is charged and discharged, and the problem of volume expansion of the material caused by iron nitride is solved, so that the cycle performance of the composite material is improved.
Drawings
FIG. 1 shows Ordered Mesoporous Carbon (OMC) and iron nitride (Fe)2N) sample Fe2N@OMC-1、 Fe2N @ OMC-2 and Fe2XRD pattern of N @ OMC-3, which is from top to bottom: fe2N@OMC-3、Fe2N@OMC-2、Fe2N@OMC-1、Fe2N、OMC；
FIG. 2 shows Fe in sample2SEM image of N @ OMC-2.
FIG. 3 shows Ordered Mesoporous Carbon (OMC) and Fe sample2N@OMC-1、Fe2N @ OMC-2 and Fe2TEM image of N @ OMC-3, where FIG. 3(a) is TEM image of OMC and FIG. 3(b) is Fe2TEM image of N @ OMC-1, FIG. 3(c) is Fe2TEM image of N @ OMC-2, FIG. 3(d) is Fe2TEM image of N @ OMC-3, FIG. 3(e) is Fe2HRTEM image of N @ OMC-2.
FIG. 4 shows Ordered Mesoporous Carbon (OMC) and iron nitride (Fe)2N) sample Fe2N@OMC-1、 Fe2N @ OMC-2 and Fe2N of N @ OMC-32Adsorption/desorption isotherm graph (a) and pore size distribution profile (b).
FIG. 5 shows the sample Fe2N @ OMC-2 is a cycle diagram of a button cell assembled by a negative pole piece prepared by a negative active material.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
Preparing ordered mesoporous carbon:
ultrasonically dispersing 1g of KIT-6 template in 20mL of deionized water for 2h, then adding 1g of sucrose to completely dissolve to obtain a mixed solution, carrying out vacuum freeze drying on the mixed solution in a freeze dryer for 24h, then grinding the mixed solution into powder, heating the powder to 900 ℃ at the heating rate of 2 ℃/min in a tubular furnace in the nitrogen atmosphere with the flow rate of 40mL/s, preserving the temperature for 2h to carry out carbonization, cooling, stirring in 5 wt% of hydrofluoric acid solution for 24h to remove the KIT-6 template, and then drying in a constant-temperature drying oven at the temperature of 80 ℃ for 12h to obtain the composite material.
Preparing a ferric nitride-ordered mesoporous carbon composite material:
s1, ultrasonically dispersing 0.1g of the prepared ordered mesoporous carbon in 20mL of deionized water for 2 hours, and then adding 0.25g of FeCl3·6H2Stirring for 8h, then placing in a constant-temperature drying oven at 80 ℃ for drying for 12h, and grinding into powder to obtain a precursor;
s2, heating to 800 ℃ at the heating rate of 5 ℃/min in a tubular furnace under the ammonia atmosphere with the flow rate of 100mL/S, performing heat preservation and ammoniation for 2h to obtain the ferric nitride-ordered mesoporous carbon composite material, and marking as a sample Fe2N@OMC-1。
Example 2
The difference between example 2 and example 1 is: 0.5g FeCl was added3·6H2And O. Example 2 the composite of iron nitride and ordered mesoporous carbon prepared in example 2 was recorded as sample Fe2N@OMC-2。
Example 3
The difference between example 3 and example 1 is: adding 1g FeCl3·6H2And O. Example 3 iron nitrideThe composite material with the ordered mesoporous carbon is recorded as sample Fe2N@OMC-3。
Example 4
Preparing ordered mesoporous carbon:
ultrasonically dispersing 1g of KIT-6 template in 10mL of deionized water for 2h, adding 0.5g of cane sugar to completely dissolve the template to obtain a mixed solution, carrying out vacuum freeze drying on the mixed solution in a freeze dryer for 24h, grinding the mixed solution into powder, heating the mixed solution to 400 ℃ at the heating rate of 1 ℃/min in a nitrogen atmosphere with the flow rate of 40mL/s in a tubular furnace, preserving the temperature for 2h for carbonization, cooling, stirring the cooled mixed solution in 1 wt% of hydrofluoric acid solution for 24h to remove the KIT-6 template, and drying the obtained product in a constant-temperature drying oven at the temperature of 80 ℃ for 12h to obtain the composite material.
Preparing a ferric nitride-ordered mesoporous carbon composite material:
s1, ultrasonically dispersing 0.1g of the prepared ordered mesoporous carbon in 1mL of deionized water for 2 hours, and then adding 0.1g of FeCl3·6H2Stirring for 8h, then placing in a constant-temperature drying oven at 80 ℃ for drying for 12h, and grinding into powder to obtain a precursor;
s2, heating to 400 ℃ at a heating rate of 1 ℃/min in a tubular furnace in an ammonia gas atmosphere with a flow rate of 50mL/S, performing heat preservation and ammoniation for 2h to obtain the ferric nitride-ordered mesoporous carbon composite material, and recording the ferric nitride-ordered mesoporous carbon composite material as a sample Fe2N@OMC-4。
Example 5
Preparing ordered mesoporous carbon:
ultrasonically dispersing 1g of SBA-15 template in 50mL of deionized water for 2h, adding 1.5g of glucose to dissolve completely to obtain a mixed solution, carrying out vacuum freeze drying on the mixed solution in a freeze dryer for 24h, grinding the mixed solution into powder, heating the mixed solution to 1000 ℃ at the heating rate of 5 ℃/min in a tubular furnace under the nitrogen atmosphere with the flow rate of 40mL/s, preserving the temperature for 2h for carbonization, cooling, stirring in 20 wt% of hydrofluoric acid solution for 24h to remove the KIT-6 template, and drying in a constant-temperature drying oven at the temperature of 80 ℃ for 12h to obtain the template.
Preparing a ferric nitride-ordered mesoporous carbon composite material:
s1, ultrasonically dispersing 0.1g of the prepared ordered mesoporous carbon in 10mL of deionized water for 2h, and then adding 1gFeCl3·6H2Stirring for 8h, then placing in a constant-temperature drying oven at 80 ℃ for drying for 12h, and grinding into powder to obtain a precursor;
s2, heating to 1000 ℃ at the heating rate of 5 ℃/min in a tubular furnace in the ammonia gas atmosphere with the flow rate of 200mL/S, and performing heat preservation and ammoniation for 2h to obtain the ferric nitride-ordered mesoporous carbon composite material, wherein the sample is marked as Fe2N@OMC-5。
Comparative example 1
Preparing ordered mesoporous carbon:
ultrasonically dispersing 1g of KIT-6 template in 20mL of deionized water for 2h, then adding 1g of sucrose to completely dissolve to obtain a mixed solution, carrying out vacuum freeze drying on the mixed solution in a freeze dryer for 24h, then grinding the mixed solution into powder, heating the powder to 900 ℃ at the heating rate of 2 ℃/min in a tubular furnace in the nitrogen atmosphere with the flow rate of 40mL/s, preserving the temperature for 2h to carry out carbonization, cooling, stirring in 5 wt% of hydrofluoric acid solution for 24h to remove the KIT-6 template, and then drying in a constant-temperature drying oven at the temperature of 80 ℃ for 12h to obtain the product.
Comparative example 2
Preparing iron nitride:
1g of FeCl3·6H2Placing the O in a constant-temperature drying oven at 80 ℃ for drying for 12h, and grinding into powder to obtain anhydrous FeCl3Powder of the anhydrous FeCl3Uniformly spreading the powder at the bottom of the porcelain boat, placing the porcelain boat in a tube furnace, heating to 800 ℃ at the heating rate of 5 ℃/min under the ammonia gas atmosphere with the flow rate of 100mL/s, and performing heat preservation and ammoniation for 2h to obtain the iron nitride.
Fe was added to each of the samples obtained in examples 1, 2 and 32N @ OMC-1, sample Fe2N @ OMC-2, sample Fe2N @ OMC-3 and the ordered mesoporous carbon and iron nitride prepared in comparative examples 1 and 2 were subjected to XRD, TEM and N2Physical adsorption and desorption test, and Fe sample2N @ OMC-2 was subjected to SEM testing.
FIG. 1 shows sample Fe2N @ OMC-1, sample Fe2N @ OMC-2, sample Fe2XRD patterns of the ordered mesoporous carbon prepared by N @ OMC-3 and the comparative example 1 and the iron nitride prepared by the comparative example 2. From the spectrum of FIG. 1, it can be seen that iron nitride,Fe2N@OMC-1、Fe2N @ OMC-2 and Fe2N @ OMC-3 has distinct characteristic peaks at 2 θ ═ 37.4, 40.9, 43.0, 56.9, 68.0, and 76.0 °, which correspond to Fe, respectively2The (021), (200), (121), (221), (023) and (321) crystal planes of the N phase (JC-PDS #50-0958) demonstrate Fe2N @ OMC-1, sample Fe2N @ OMC-2, sample Fe2Fe in N @ OMC-32The presence of N. In the XRD spectrum of the ordered mesoporous carbon, two distinct characteristic peaks corresponding to the (002) and (100) crystal planes of the graphitized carbon at 2 θ of 23.8 and 43.6 ° can be observed.
FIG. 2 shows Fe in sample2SEM image of N @ OMC-2, FIG. 3 is (a): ordered mesoporous carbon, (b): sample Fe2N @ OMC-1, (c): sample Fe2N @ OMC-2 and (d): sample Fe2TEM image of N @ OMC-3; (e) the method comprises the following steps Sample Fe2HRTEM image of N @ OMC-2. As can be seen from FIG. 2, sample Fe2The N @ OMC-2 material surface was uniformly attached with nano-sized particles, as can be seen in the high power transmission microscope in fig. 3 e: the lattice spacing of the particles was 0.21 and 0.44nm, respectively, which corresponds to orthorhombic Fe2The (102) and (200) crystal planes of the N phase (JC-PDS #50-0958), which indicates Fe in nanometer size2The N particles are uniformly attached to the ordered mesoporous carbon material.
FIG. 4 shows Fe in sample2N @ OMC-1, sample Fe2N @ OMC-2, sample Fe2N @ OMC-3, the ordered mesoporous carbon prepared in comparative example 1, and the N2 adsorption/desorption isotherm graph and the pore size distribution map of the iron nitride prepared in comparative example 2, the specific surface areas of which are respectively Fe samples2N@OMC-11232m2G, sample Fe2N@OMC-2919m2G, sample Fe2N@OMC-3583m2Per g, ordered mesoporous carbon 1609m from comparative example 12Iron nitride 62m from comparative example 22(ii) in terms of/g. From the comparison of the specific surface area data of the materials, the following results are obtained: the composite material still maintains a larger specific surface area, which can provide more storage space for the electrolyte, and is beneficial to the cycle life of the battery.
Respectively mixing the samples Fe2N @ OMC-1, sample Fe2N @ OMC-2, sample Fe2N @ OMC-3, the ordered mesoporous carbon prepared in the comparative example 1 and the ferric nitride prepared in the comparative example 2 are used as negative active materials to prepare a negative pole piece, wherein in the negative pole piece, the negative active materials are as follows: conductive agent (carbon black): binder (polytetrafluoroethylene) 90:5: 5. And respectively assembling the obtained negative pole pieces into button cells, and carrying out charge and discharge tests, wherein the counter electrode is a lithium piece.
Wherein, sample Fe2N @ OMC-1, sample Fe2N @ OMC-2, sample Fe2The first reversible capacities of the button cell prepared by using the ordered mesoporous carbon prepared in N @ OMC-3 and the comparative example 1 and the ferric nitride prepared in the comparative example 2 as the negative electrode active materials are respectively as follows: sample Fe2N @ OMC-1481mAh/g and sample Fe2N @ OMC-2582mAh/g and sample Fe2N @ OMC-3510mAh/g, 321mAh/g of ordered mesoporous carbon prepared in comparative example 1, and 410mAh/g of iron nitride prepared in comparative example 2. Wherein, sample Fe2The first capacity exertion of N @ OMC-2 is far better than that of single OMC or Fe2And (3) N material. For sample Fe2The button cell made by N @ OMC-2 was subjected to 100 cycles of the test as shown in FIG. 5, from which it was seen that it had excellent cycle stability.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The ferric nitride-ordered mesoporous carbon composite material is characterized in that ordered mesoporous carbon is used as a carrier, and ferric nitride nano particles are uniformly distributed on the surface and in the inner pore canal of the ordered mesoporous carbon.
2. The ferric nitride-ordered mesoporous carbon composite material according to claim 1, wherein the ordered mesoporous carbon material is prepared by the following steps: the preparation method comprises the steps of uniformly dispersing the ordered mesoporous silica template in water, adding a water-soluble carbon source to dissolve the ordered mesoporous silica template completely to obtain a mixed solution, carrying out freeze drying on the mixed solution, carrying out high-temperature carbonization in a protective atmosphere, and removing the ordered mesoporous silica template to obtain the composite material.
3. The ferric nitride-ordered mesoporous carbon composite material of claim 2, wherein the mass ratio of the ordered mesoporous silica template to the water-soluble carbon source is 1 (0.5-1.5), and the mass ratio of the ordered mesoporous silica template to the water is 1: (10-50).
4. The iron nitride-ordered mesoporous carbon composite according to claim 2 or 3, wherein the water-soluble carbon source is a water-soluble carbohydrate, preferably glucose or sucrose; the ordered mesoporous silica template is a KIT-6 template or an SBA-15 template.
5. The diiron nitride-ordered mesoporous carbon composite material according to any one of claims 2 to 4, wherein the carbonization temperature is 400 to 1000 ℃, and the temperature rise rate is 1 to 5 ℃/min; the method for removing the ordered mesoporous silica template comprises the following steps: and washing by adopting a hydrofluoric acid solution with the mass fraction of 1-20%.
6. A method for preparing a diiron nitride-ordered mesoporous carbon composite material according to any one of claims 1 to 5, comprising the steps of:
s1, uniformly dispersing the ordered mesoporous carbon in water, adding a water-soluble iron source to dissolve completely, and then drying to obtain a precursor;
and S2, performing high-temperature ammoniation on the precursor in an ammonia atmosphere to obtain the ferric nitride-ordered mesoporous carbon composite material.
7. The method for preparing the iron nitride-ordered mesoporous carbon composite material according to claim 6, wherein the mass ratio of the ordered mesoporous carbon to the water-soluble iron source is 1: (1-10), wherein the mass ratio of the ordered mesoporous carbon to the water is 1: (10-200); preferably, the mass ratio of the ordered mesoporous carbon to the water-soluble iron source is 1: 5.
8. The method of preparing a di-iron nitride-ordered mesoporous carbon composite according to claim 6 or 7, wherein the iron source is a trivalent soluble iron salt.
9. The preparation method of the iron nitride-ordered mesoporous carbon composite material according to any one of claims 6 to 8, wherein in the step S2, the flow rate of the ammonia gas for high-temperature ammoniation is 50-200 mL/S, the temperature is 400-1000 ℃, and the temperature rise rate is 1-5 ℃/min.
10. Use of the ferric nitride-ordered mesoporous carbon composite material according to any of claims 1 to 5 as a negative active material for lithium ion batteries.
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