CN111943149A - General preparation method of transition metal nitride - Google Patents

General preparation method of transition metal nitride Download PDF

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CN111943149A
CN111943149A CN202010861136.7A CN202010861136A CN111943149A CN 111943149 A CN111943149 A CN 111943149A CN 202010861136 A CN202010861136 A CN 202010861136A CN 111943149 A CN111943149 A CN 111943149A
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transition metal
powder
nitride
metal oxide
general preparation
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王岩
崔桂荣
吴玉程
李洋
崔接武
秦永强
郑红梅
张勇
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Hefei University of Technology
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    • C01B21/062—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with chromium, molybdenum or tungsten
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    • C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
    • C01B21/0622—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with iron, cobalt or nickel
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Abstract

The invention discloses a general preparation method of transition metal nitride, which is characterized in that transition metal oxide powder and melamine powder are used as raw materials and are calcined together, so that nitrogen atoms replace oxygen atoms in the transition metal oxide, and the corresponding transition metal nitride is obtained. The transition metal nitride prepared by the invention can be used as a lithium ion battery cathode material, has excellent specific capacity, rate capability and cycling stability, and has simple process flow, convenient operation, no need of complex chemical modification and post-treatment in the process and universality.

Description

General preparation method of transition metal nitride
Technical Field
The invention belongs to the technical field of micro-nano functional material preparation, and particularly relates to a general preparation method of a transition metal nitride.
Background
Transition metal nitrides have properties of covalent compounds, ionic crystals and transition metals, have stable structures and excellent electrical conductivity, and are gradually a research hotspot in the field of energy storage in recent years. Compared with a carbon electrode material, the transition metal nitride has higher specific capacity and larger volume energy density (high tap density). Compared with the transition metal oxide electrode material, the transition metal nitride electrode material has high multiplying power and excellent cycle stability. Transition metal nitride also has a low and flat charge-discharge potential platform and good reversibility, and is widely applied to lithium ion battery cathode materials, such as: in MnO/TiN composites, TiN provides a conductive network and acts as a buffer for the volume expansion/contraction of the electrode material after Li insertion/de-insertion into MnO. Fe2N at a current density of 1A g-1The reversible capacity can reach 900mAh g-1At a current density of 6A g-1The capacity can still be kept to 76% of the capacity of the first circle after 300 circles of lower circulation.
In the prior reports, the methods for producing transition metal nitrides have been generally ball milling, sputtering, pyrolysis, electrochemical, solid state reaction, and the like. The ball milling method is a method for mixing and refining raw materials by ball milling under a certain atmosphere condition to finally obtain the transition metal nitride, and has the defects that the types of the prepared transition metal nitride are relatively few, most of the transition metal nitride cannot be prepared by ball milling, and the universality is poor. The sputtering method is a method of first vacuumizing the system, then introducing nitrogen or ammonia gas to keep the system at a certain low pressure, and finally converting the transition metal oxide into gas through a certain heat source to prepare the metal nitride. The pyrolysis method has low nitriding uniformity, and precursor agglomeration is easily caused in the nitriding process. The electrochemical process is selective to metal nitrides. The nitrided products obtained by the solid state reaction process have a residue of reactants.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a general preparation method of transition metal nitride, so that the transition metal nitride with high performance can be simply and efficiently obtained.
In order to realize the purpose of the invention, the following technical scheme is adopted:
a general preparation method of transition metal nitride is characterized in that: the transition metal oxide powder and melamine powder are used as raw materials, and co-calcination is carried out to enable nitrogen atoms to replace oxygen atoms in the transition metal oxide, so that the corresponding transition metal nitride is obtained.
Further, the transition metal oxide is molybdenum trioxide, cobaltosic oxide, vanadium pentoxide, ferric oxide or titanium dioxide. The transition metal oxide powder can be nanoscale powder or micron-sized powder, so that transition metal nitride materials with corresponding sizes can be obtained.
Furthermore, the dosage ratio of the transition metal oxide powder to the melamine powder is 0.1-1g: 0.05-2 g.
Further, the general preparation method comprises the following steps:
respectively putting transition metal oxide powder and melamine powder into two burning boats, and then putting the two burning boats into a tubular furnace, wherein the melamine powder is positioned at the upstream and the transition metal oxide powder is positioned at the downstream; under the protection of inert gas, the temperature in the tubular furnace is raised to 500-700 ℃, the heat preservation and the calcination are carried out for 2-4h, and then the transition metal nitride is obtained after the temperature is cooled to the room temperature along with the furnace.
Further, the inert gas is argon, the flow rate of the inert gas is 5-30sccm, and the flow direction in the tube furnace is from upstream to downstream.
Further, the heating rate is 5-10 ℃/min.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention adopts melamine with high nitrogen content as raw material, can provide sufficient nitrogen source in the calcining process, so that the transition metal oxide can be completely nitrided, and compared with the transition metal oxide before nitriding, the nitrided transition metal nitride has no great change in micro-morphology and no agglomeration phenomenon.
2. The transition metal nitride obtained by the invention has better conductivity than the oxide thereof, can be used as a lithium ion battery cathode material, and has excellent specific capacity, rate capability and cycling stability.
3. The method has the advantages of simple process flow, convenient operation, no need of complex chemical modification and post-treatment in the process, and universality.
Drawings
FIG. 1 is an X-ray photoelectron spectrum (FIG. 1a) and an X-ray diffraction pattern (FIG. 1b) of a nitride of molybdenum trioxide obtained in example 1;
FIG. 2 is a field emission scanning electron diagram (FIG. 2b) of the molybdenum trioxide starting material used in example 1 (FIG. 2a) and the resulting nitride of molybdenum trioxide;
FIG. 3 is a spectrum of the molybdenum trioxide nitride obtained in example 1;
FIG. 4 is an X-ray photoelectron spectrum (FIG. 4a) and an X-ray diffraction pattern (FIG. 4b) of a nitride of tricobalt tetraoxide obtained in example 2;
FIG. 5 is a field emission scanning electron diagram (FIG. 5b) of the cobaltosic oxide raw material used in example 2 (FIG. 5a) and the resulting nitride of cobaltosic oxide;
FIG. 6 is a spectrum diagram of the nitride of cobaltosic oxide obtained in example 2;
FIG. 7 is an X-ray photoelectron spectrum (FIG. 7a) and an X-ray diffraction pattern (FIG. 7b) of the nitride of vanadium pentoxide obtained in example 3;
FIG. 8 is a field emission scanning electron diagram (FIG. 8b) of the vanadium pentoxide material used in example 3 (FIG. 8a) and the resulting nitride of vanadium pentoxide;
FIG. 9 is a spectrum of a nitride of vanadium pentoxide obtained in example 3;
FIG. 10 is an X-ray photoelectron spectrum (FIG. 10a) and an X-ray diffraction pattern (FIG. 10b) of the nitride of iron sesquioxide obtained in example 4;
FIG. 11 is a field emission scanning electron diagram (FIG. 11b) of the iron sesquioxide starting material used in example 4 (FIG. 11a) and the resulting nitride of iron sesquioxide;
FIG. 12 is a graph showing an energy spectrum of a nitride of iron sesquioxide obtained in example 4;
FIG. 13 is an X-ray photoelectron spectrum (FIG. 13a) and an X-ray diffraction pattern (FIG. 13b) of a nitride of titanium dioxide obtained in example 5;
FIG. 14 is a field emission scanning electron image (FIG. 14b) of the titania starting material used in example 5 (FIG. 14a) and the resulting nitrides of titania;
FIG. 15 is a spectrum of the nitride of titanium dioxide obtained in example 5;
FIG. 16 shows the iron trioxide nitride and iron trioxide prepared in example 4 at different current densities (100-5000 mA g/g)-1) Graph of rate capability of (1) (FIG. 16a) and at 5000mA g-1Comparison graph of cycling stability at current density (fig. 16 b).
Detailed Description
In order to facilitate understanding of the present invention for those skilled in the art, the present invention will be further described with reference to the accompanying drawings and examples.
Example 1
In this embodiment, molybdenum trioxide powder and melamine powder are used as raw materials to prepare a nitride of molybdenum trioxide, and the specific steps are as follows:
step 1, weighing 0.5g of molybdenum trioxide powder and 1g of melamine powder, and respectively placing the molybdenum trioxide powder and the melamine powder in different burning boats.
And 2, placing the burning boat containing the molybdenum trioxide powder and the melamine powder into a tubular furnace, wherein the melamine powder is positioned at the upstream, the molybdenum trioxide powder is positioned at the downstream, and then introducing argon for 5min to remove air in the furnace.
And 3, under the protection of argon (the gas flow is 10sccm, the gas flow direction in the tube furnace is from upstream to downstream), raising the temperature in the tube furnace to 600 ℃ at the heating rate of 10 ℃/min, carrying out heat preservation and calcination for 2h, and then cooling to room temperature along with the furnace to obtain the molybdenum trioxide nitride, wherein the X-ray photoelectron spectrum of the molybdenum trioxide nitride is shown in figure 1a, the X-ray diffraction pattern of the molybdenum trioxide nitride is shown in figure 1b, the field emission scanning electron diagram of the molybdenum trioxide nitride is shown in figure 2b, and the energy spectrum diagram of the molybdenum trioxide nitride is shown in figure 3.
Example 2
In this embodiment, cobaltosic oxide powder and melamine powder are used as raw materials to prepare a nitride of cobaltosic oxide, and the specific steps are as follows:
step 1, weighing 0.1g of cobaltosic oxide powder and 0.05g of melamine powder, and respectively placing the cobaltosic oxide powder and the melamine powder in different burning boats.
And 2, placing the burning boat containing the cobaltosic oxide powder and the melamine powder into a tubular furnace, wherein the melamine powder is positioned at the upstream, the cobaltosic oxide powder is positioned at the downstream, and then introducing argon for 5min to remove air in the furnace.
And 3, under the protection of argon (the gas flow is 15sccm, the gas flow direction in the tube furnace is from upstream to downstream), raising the temperature in the tube furnace to 600 ℃ at the temperature rise rate of 5 ℃/min, carrying out heat preservation and calcination for 3h, and then cooling to room temperature along with the furnace to obtain the cobaltosic oxide nitride, wherein the X-ray photoelectron spectrum of the cobaltosic oxide nitride is shown in figure 4a, the X-ray diffraction pattern of the cobaltosic oxide nitride is shown in figure 4b, the field emission scanning electron diagram of the cobaltosic oxide nitride is shown in figure 5b, and the energy spectrum diagram of the cobaltosic oxide nitride.
Example 3
In the embodiment, vanadium pentoxide powder and melamine powder are used as raw materials to prepare vanadium pentoxide nitride, and the method comprises the following specific steps:
step 1, weighing 1g of vanadium pentoxide powder and 2g of melamine powder, and respectively placing the vanadium pentoxide powder and the melamine powder in different burning boats.
And 2, placing the burning boat containing the vanadium-molybdenum pentoxide powder and the melamine powder into a tubular furnace, wherein the melamine powder is positioned at the upstream and the vanadium pentoxide powder is positioned at the downstream, and then introducing argon for 5min to remove air in the furnace.
And 3, under the protection of argon (the gas flow is 20sccm, the gas flow direction in the tube furnace is from upstream to downstream), raising the temperature in the tube furnace to 700 ℃ at the heating rate of 10 ℃/min, carrying out heat preservation and calcination for 4h, and then cooling to room temperature along with the furnace to obtain the vanadium pentoxide nitride, wherein the X-ray photoelectron energy spectrum is shown in figure 7a, the X-ray diffraction pattern is shown in figure 7b, the field emission scanning electron diagram is shown in figure 8b, and the energy spectrum diagram is shown in figure 9.
Example 4
In this embodiment, iron sesquioxide powder and melamine powder are used as raw materials to prepare a nitride of iron sesquioxide, and the specific steps are as follows:
step 1, weighing 0.2g of ferric oxide powder and 0.1g of melamine powder, and respectively placing the ferric oxide powder and the melamine powder in different burning boats.
And 2, placing the burning boat filled with ferric oxide powder and melamine powder into a tubular furnace, wherein the melamine powder is positioned at the upstream, and the ferric oxide powder is positioned at the downstream, and then introducing argon for 5min to remove air in the furnace.
And 3, under the protection of argon (the gas flow is 10sccm, the gas flow direction in the tube furnace is from upstream to downstream), raising the temperature in the tube furnace to 500 ℃ at the heating rate of 10 ℃/min, carrying out heat preservation and calcination for 2h, and then cooling to room temperature along with the furnace to obtain the nitride of the ferric oxide, wherein the X-ray photoelectron spectrum of the nitride is shown as figure 10a, the X-ray diffraction pattern is shown as figure 10b, the field emission scanning electron diagram is shown as figure 11b, and the energy spectrum diagram is shown as figure 12.
Example 5
In this embodiment, titanium dioxide powder and melamine powder are used as raw materials to prepare a nitride of titanium dioxide, and the specific steps are as follows:
step 1, weighing 0.1g of titanium dioxide powder and 0.1g of melamine powder, and respectively placing the titanium dioxide powder and the melamine powder in different burning boats.
And 2, placing the burning boat containing the titanium dioxide powder and the melamine powder into a tubular furnace, wherein the melamine powder is positioned at the upstream and the titanium dioxide powder is positioned at the downstream, and then introducing argon for 5min to remove air in the furnace.
And 3, under the protection of argon (the gas flow is 10sccm, the gas flow direction in the tube furnace is from upstream to downstream), raising the temperature in the tube furnace to 600 ℃ at the temperature rise rate of 5 ℃/min, carrying out heat preservation and calcination for 2h, and then cooling to room temperature along with the furnace to obtain the nitride of the titanium dioxide, wherein the X-ray photoelectron spectrum of the nitride of the titanium dioxide is shown in figure 13a, the X-ray diffraction pattern of the nitride of the titanium dioxide is shown in figure 13b, the field emission scanning electron diagram of the nitride of the titanium dioxide is shown in figure 14b, and the energy spectrum diagram of the nitride of.
To test the performance of the materials obtained in the above examples as electrochemical energy storage materials, the materials obtained in example 4 were assembled into batteries and subjected to electrochemical tests as follows: preparing the material synthesized in the embodiment 4, carbon black and polyvinylidene fluoride (PVDF) into slurry according to the mass ratio of 8:1:1, and coating the slurry on a copper foil to prepare an electrode plate; 1.0mol L of Ethylene Carbonate (EC) and dimethyl carbonate (DMC) (volume ratio of 1:1) dissolved in-1LiPF6Is an electrolyte; a2320 type polypropylene microporous membrane is taken as a diaphragm, and the diaphragm is assembled into a 2032 type button battery in an argon glove box. The LAND CT-2001A test system is adopted to test the voltage of 100-5000 mA g in the voltage range of 0.01-3.0V at room temperature-1Constant current charge and discharge tests were performed at the current density of (1).
FIG. 16 shows the iron trioxide nitride and iron trioxide prepared in example 4 at different current densities (100-5000 mAg)-1) Performance of (c) is compared with the graph. The result shows that the nitride electrode material prepared in the example 4 has more excellent electrochemical performance, and the electrochemical performance is 5000mA g-1The specific capacity under the current density can reach 100mA g-1About 60 percent of the total weight of the product, and has high rate capability. At 5000m ag-1The specific capacity is improved by 25% after circulating for 2000 circles under the current density, and the lithium ion battery has excellent circulating stability and pseudocapacitance characteristics and can be used as an ideal lithium ion battery cathode material.

Claims (6)

1. A general method for preparing a transition metal nitride, characterized by: the transition metal oxide powder and melamine powder are used as raw materials, and co-calcination is carried out to enable nitrogen atoms to replace oxygen atoms in the transition metal oxide, so that the corresponding transition metal nitride is obtained.
2. The general preparation method according to claim 1, characterized in that: the transition metal oxide is molybdenum trioxide, cobaltosic oxide, vanadium pentoxide, ferric oxide or titanium dioxide.
3. The general preparation method according to claim 1, characterized in that: the dosage ratio of the transition metal oxide powder to the melamine powder is 0.1-1g: 0.05-2 g.
4. The general preparation method according to claim 1, 2 or 3, characterized in that it comprises the following steps:
respectively putting transition metal oxide powder and melamine powder into two burning boats, and then putting the two burning boats into a tubular furnace, wherein the melamine powder is positioned at the upstream and the transition metal oxide powder is positioned at the downstream; under the protection of inert gas, the temperature in the tubular furnace is raised to 500-700 ℃, the heat preservation and the calcination are carried out for 2-4h, and then the transition metal nitride is obtained after the temperature is cooled to the room temperature along with the furnace.
5. The general preparation method according to claim 4, characterized in that: the inert gas is argon, the flow rate is 5-30sccm, and the flow direction in the tube furnace is from upstream to downstream.
6. The general preparation method according to claim 4, characterized in that: the heating rate is 5-10 ℃/min.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113851332A (en) * 2021-08-26 2021-12-28 合肥工业大学 Niobium oxynitride with adjustable nitrogen-oxygen atom ratio and preparation method and energy storage application thereof
CN113968739A (en) * 2021-10-12 2022-01-25 中国原子能科学研究院 Preparation method of mixed nitride powder
CN114023936A (en) * 2021-10-29 2022-02-08 格林美股份有限公司 Nitride/graphitized carbon nanosheet coated ternary cathode material and preparation method thereof

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CN113851332A (en) * 2021-08-26 2021-12-28 合肥工业大学 Niobium oxynitride with adjustable nitrogen-oxygen atom ratio and preparation method and energy storage application thereof
CN113851332B (en) * 2021-08-26 2022-08-30 合肥工业大学 Niobium oxynitride with adjustable nitrogen-oxygen atom ratio, preparation method and energy storage application thereof
CN113968739A (en) * 2021-10-12 2022-01-25 中国原子能科学研究院 Preparation method of mixed nitride powder
CN114023936A (en) * 2021-10-29 2022-02-08 格林美股份有限公司 Nitride/graphitized carbon nanosheet coated ternary cathode material and preparation method thereof

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