CN109860593B - Iron-nickel sulfide, preparation method thereof and sodium ion battery using iron-nickel sulfide as negative electrode - Google Patents
Iron-nickel sulfide, preparation method thereof and sodium ion battery using iron-nickel sulfide as negative electrode Download PDFInfo
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Abstract
The invention discloses a preparation method of an iron-nickel sulfide, which comprises the following steps of taking an iron organic acid salt, nickel nitrate and a carbon-nitrogen source organic matter according to the mass ratio of 1 (1-3) to (1-7), mixing and grinding to obtain a mixture A; the mixture A is subjected to heat treatment for 1 h-5 h at 500 ℃ -1200 ℃, the mixture A is taken out after cooling to obtain a product B, and the product B and a sulfur source are mixed and ground uniformly according to the mass ratio of 1 (5-10) to obtain a mixture C; the mixture C is subjected to heat treatment at 300-600 ℃ for 30 min-1 h, and is taken out after cooling to obtain a product D, namely the iron-nickel sulfide, wherein the iron-nickel sulfide prepared by the invention has a gourd-shaped structure of active particles coated by a continuous carbon layer; the active particles in the structure can keep nano size in the charging and discharging process, the coated carbon nano tube structure can protect the expansion process of the material, so that the structure of the active material is kept stable, the graphitized carbon nano tube structure can provide a high-speed conductive path, and the iron-nickel sulfide obtained by the invention can also be used as a cathode of a sodium ion battery.
Description
Technical Field
The invention belongs to the field of composite material synthesis, and particularly relates to an iron-nickel sulfide and a preparation method thereof, and also relates to a sodium ion battery adopting the iron-nickel sulfide as a battery negative electrode material.
Background
In recent years, due to the wide distribution and abundant reserves of sodium element in the earth, the development of room temperature sodium ion charge and discharge batteries has been considered as an effective way to replace lithium ion batteries in the fields of large-scale energy storage, particularly smart power grids and the like, so as to effectively solve the problems of low mineral reserves and high lithium source cost of the lithium ion batteries. Among the cathode material systems of sodium ion batteries, carbon, metal oxides or sulfides, and alloy-type materials such as Sn and Sb are the most interesting material systems. The metal sulfide has the advantages of high theoretical capacity, abundant resources, low toxicity, good conductivity and the like, and is a potential negative electrode material of the sodium-ion battery. Wherein the ferric sulfide is used as the electrode material of the sodium ion battery, is a stable, nontoxic and cheap material with simple preparation, and has high theoretical sodium intercalation capacity (894mAh/g) and volumetric specific capacity (2950 mAh/cm)3). However, the electrochemical sodium storage capacity of iron sulfide is greatly hindered by the defects of low conductivity, poor interface compatibility with organic electrolyte, large microscopic size of electrode material and low utilization rate of effective charge and discharge active sites. Meanwhile, because the resistivity of the iron sulfide is large, the voltage is reduced quickly during discharging, and particularly serious polarization phenomenon can be generated during large-current discharging of the battery, so that the service life of the battery is greatly shortened. Therefore, the improvement of the cycle capacity and sustainability of iron sulfide as a negative electrode material in sodium ion batteries is the direction to be studied intensively at present.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides an iron-nickel sulfide, a preparation method thereof and a sodium ion battery using the iron-nickel sulfide as a cathode.
In order to achieve the purpose, the invention adopts the technical scheme that the preparation method of the iron-nickel sulfide comprises the following steps:
step 1, mixing and grinding organic acid salts of iron, nickel nitrate and organic matters of carbon-nitrogen source according to the mass ratio of (1) - (3) to (1) - (7) to obtain a mixture A;
step 2, heat-treating the mixture A at 500-1200 ℃ for 1-5 h, cooling and taking out to obtain a product B,
step 3, mixing and grinding the product B and a sulfur source uniformly according to a mass ratio of 1 (5-10) to obtain a mixture C;
and 4, carrying out heat treatment on the mixture C at the temperature of 300-600 ℃ for 30 min-1 h, cooling and taking out to obtain a product D, namely the iron-nickel sulfide.
In step 1, the ferric organic acid salt is analytically pure, and the ferric organic acid salt comprises ferric citrate, ferric oxalate or ferric acetate.
In step 1, the carbon-nitrogen source organic matter comprises urea, melamine, carbodiimide, cyanuric acid or trithiocyanuric acid.
In step 1, the grinding time is half an hour.
In the step 2, the heating rate of the heat treatment is 2-20 ℃/min, and the furnace is cooled.
In the step 3, one or more of sublimed sulfur, thioacetamide or trithiocyanuric acid is adopted as a sulfur source.
In step 4, the heating rate of the heat treatment is 5-10 ℃/min, and the furnace is cooled.
The iron-nickel sulfide particles prepared by the preparation method are in a continuous carbon layer coated particle structure.
According to another scheme, the iron-nickel sulfide is used as a negative electrode material of the sodium ion battery, and the iron-nickel sulfide maintains a nanoscale size in the charging and discharging processes.
Compared with the prior art, the invention has at least the following beneficial effects: the iron-nickel sulfide composite material is prepared by adopting a two-step synthesis method, the preparation method is simple and stable, the repeatability is strong, the raw material price is low, and the preparation cost of the material reported in the existing literature can be obviously reduced;
the nickel-iron has the function of synergistically catalyzing carbon graphitization to form a carbon tube, and in the heat treatment process, a carbon nanotube coated particle structure is formed under the combined catalysis of iron and nickel to form a nano composite structure so as to form a sodium ion battery cathode material, so that the electrochemical sodium storage performance of the iron sulfide cathode material is obviously improved;
the iron-nickel sulfide prepared by the invention has the advantages that the active particles coated by the continuous carbon layer are of a gourd-shaped structure; the active particles in the structure can keep nano-size in the charging and discharging process, the coated carbon nano tube structure can protect the expansion process of the material, so that the structure of the active material is kept stable, and the graphitized carbon nano tube structure can provide a high-speed conductive path, so that the material shows excellent rate performance.
Drawings
Fig. 1 is an XRD pattern of a bimetallic sulfide of iron and nickel.
Fig. 2 is a scanning electron micrograph of an iron nickel sulfide composite.
FIG. 3 is a diagram of the charge-discharge cycle performance of bimetallic iron-nickel sulfide.
Fig. 4 is a transmission view of an iron nickel sulfide composite.
FIG. 5 is a graph showing the rate cycle of bimetallic iron-nickel sulfide.
Detailed Description
The invention is explained in more detail below with reference to the figures and the examples.
1) Mixing and grinding analytically pure iron organic acid salt, nickel nitrate and carbon nitrogen organic compound in a glass mortar to obtain a mixture, wherein the mass ratio of an iron source to a nickel source to the organic compound in the mixture is 1 (1-3) to 1-7, and the mixture is marked as A; the ferric organic acid salt is ferric citrate, ferric oxalate or ferric acetate; the organic matter is urea, melamine, carbodiimide, cyanuric acid or trithiocyanuric acid;
2) performing heat treatment on the mixture A in a low-temperature tubular furnace, in the reaction process, catalyzing a carbon source by using an iron-nickel raw material together to form an iron-nickel separation particle externally coated graphitized carbon tube structure, cooling and taking out to obtain a product B, wherein the heat treatment temperature rise rate is 2-20 ℃/min, the heat treatment temperature is 500-1200 ℃, and the time is 1-5 h;
3) mixing and grinding the product B and a sulfur source in a glass mortar to obtain a mixture, wherein the mass ratio of the product B to the sulfur source is 1 (5-10), and the mixture is marked as C; the sulfur source may be sublimed sulfur, thioacetamide or trithiocyanuric acid;
4) and then the mixture C is subjected to heat treatment in a low-temperature tubular furnace, the heating rate of the heat treatment is 5-10 ℃/min, the heat treatment temperature is 300-800 ℃, the time is 30 min-1 h, and the mixture C is taken out after cooling to obtain a product D, namely the separated iron-nickel sulfide coated by the continuous carbon tube and having a calabash structure.
Example 1:
the process for preparing the iron-nickel sulfide according to the mass ratio of the reactants of 1:1:2 is as follows:
1) taking 2g of analytically pure ferric citrate, 2g of nickel nitrate and 4g of urea, and mixing and grinding in a glass mortar to obtain a mixture A;
2) heating the mixture A to 800 ℃ at the speed of 2 ℃/min in a low-temperature tube furnace, preserving the temperature for 3h, cooling and taking out to obtain a product B;
3) mixing and grinding the product B and sublimed sulfur with the mass of 5 times of that of the product B in a glass mortar to obtain a mixture C;
4) and then heating the mixture C to 400 ℃ at the speed of 5 ℃/min in a low-temperature tubular furnace, calcining for 1h, cooling and taking out to obtain a product D, namely the iron-nickel bimetallic sulfide nano material.
The product was analyzed by means of a Japanese science D/max2000 PCX-ray diffractometer, and the XRD of the product obtained in example 1 is shown in FIG. 1, and it can be seen from FIG. 1 that the product is a bimetallic sulfide of iron and nickel; preparing the obtained product into a button type sodium ion battery, and specifically packaging the button type sodium ion battery by the following steps: the product is directly sliced and then assembled into a sodium ion half cell, a Xinwei electrochemical workstation is adopted to perform constant current charge and discharge test on the cell, the test voltage is 0.01V-3.0V, the obtained material is assembled into a button cell to test the performance of the sodium ion cell cathode material, as shown in figure 3, the cell shows the capacity of 400mAh/g under the current density of 100mA/g, the cell still has the capacity of more than 300mAh/g after being circulated for 100 circles, and the visible material has excellent cycle performance as shown in figure 3.
Example 2:
the process for preparing the iron-nickel sulfide according to the mass ratio of the reactants of 1:1:3 is as follows:
1) taking 2g of analytically pure ferric oxalate, 2g of nickel nitrate and 6g of melamine, and mixing and grinding in a glass mortar to obtain a mixture, wherein the mixture is marked as A;
2) heating the mixture A to 500 ℃ at the speed of 8 ℃/min in a low-temperature tube furnace, preserving the heat for 1h, cooling and taking out to obtain a product B;
3) mixing and grinding the product B and thioacetamide with the mass being 4 times that of the product B in a glass mortar to obtain a mixture C;
4) heating the mixture C to 300 ℃ at the speed of 6 ℃/min in a low-temperature tubular furnace, calcining for 0.5h, cooling and taking out to obtain a product D, namely the iron-nickel bimetallic sulfide;
fig. 2 is a high-power Scanning Electron Microscope (SEM) photograph of the iron-nickel sulfide composite, and the product thereof is randomly oriented and densely grown by observing the morphology of the iron-nickel sulfide composite through a Scanning Electron Microscope (SEM) model S-4800 of japan electronics, and fig. 4 is a transmission diagram of the iron-nickel sulfide composite, and it can be seen that the product thereof is in a hollow coating shape, and a graphitized carbon layer is generated under the concerted catalysis of nickel and an iron source, and the structure can improve the stability and conductivity of the material.
Example 3:
the process for preparing the iron-nickel sulfide according to the mass ratio of the reactants of 1:1:1 is as follows:
1) taking 2g of analytically pure ferric acetate, 2g of nickel nitrate and 2g of carbodiimide, mixing and grinding in a glass mortar to obtain a mixture, and marking the mixture as A;
2) heating the mixture A to 900 ℃ at a speed of 12 ℃/min in a low-temperature tube furnace, preserving the heat for 4h, cooling and taking out to obtain a product B;
3) mixing and grinding the product B and 3 times of trithiocyanuric acid in mass in a glass mortar to obtain a mixture C;
4) heating the mixture C to 500 ℃ at the speed of 8 ℃/min in a low-temperature tubular furnace, calcining for 0.5h, cooling and taking out to obtain a product D, namely the iron-nickel bimetallic sulfide;
the sample is tested by electrochemical performance, the rate performance of the sample is shown in figure 5, and as can be seen from figure 5, the sample can still keep the sodium storage capacity close to 200mAh/g at the charge-discharge rate of 5A/g, has excellent performance and has great potential as a cathode material of a sodium-ion battery.
Example 4:
the process for preparing the iron-nickel sulfide according to the mass ratio of the reactants of 1:3:7 is as follows:
1) taking 1g of analytically pure ferric oxalate, 3g of nickel nitrate and 7g of carbodiimide, and mixing and grinding in a glass mortar to obtain a mixture, wherein the mixture is marked as A;
2) heating the mixture A to 1200 ℃ at a speed of 20 ℃/min in a low-temperature tube furnace, preserving the temperature for 5h, cooling and taking out to obtain a product B;
3) mixing and grinding the product B and sublimed sulfur with 2 times of the mass of the product B in a glass mortar to obtain a mixture C;
4) and then heating the mixture C to 600 ℃ at a speed of 10 ℃/min in a low-temperature tubular furnace, calcining for 1h, cooling and taking out to obtain a product D, namely the iron-nickel bimetallic sulfide.
Example 5:
the process for preparing the iron-nickel sulfide according to the mass ratio of the reactants of 1:2:4 is as follows:
1) taking 1g of analytically pure ferric citrate, 2g of nickel nitrate and 4g of urea, mixing and grinding in a glass mortar to obtain a mixture, wherein the mixture is marked as A;
2) heating the mixture A to 600 ℃ at a speed of 10 ℃/min in a low-temperature tube furnace, preserving the heat for 2h, cooling and taking out to obtain a product B;
3) mixing and grinding the product B and thioacetamide with the mass of 5 times of the product B in a glass mortar to obtain a mixture C;
4) and heating the mixture C to 400 ℃ at the speed of 6 ℃/min in a low-temperature tubular furnace, calcining for 1h, cooling and taking out to obtain a product D, namely the iron-nickel bimetallic sulfide.
Example 6:
the process for preparing the iron-nickel sulfide according to the mass ratio of the reactants of 1:3:6 is as follows:
1) taking 1g of analytically pure ferric acetate, 3g of nickel nitrate and 6g of urea, mixing and grinding in a glass mortar to obtain a mixture, and marking the mixture as A;
2) heating the mixture A to 700 ℃ at a speed of 12 ℃/min in a low-temperature tube furnace, preserving the temperature for 2h, cooling and taking out to obtain a product B;
3) mixing and grinding the product B and trithiocyanuric acid with the mass of 5 times of the product B in a glass mortar to obtain a mixture C;
4) and heating the mixture C to 450 ℃ at the speed of 7 ℃/min in a low-temperature tubular furnace, calcining for 0.5h, cooling and taking out to obtain a product D, namely the iron-nickel bimetallic sulfide.
Example 7:
the process for preparing the iron-nickel sulfide according to the mass ratio of the reactants of 1:2:3 is as follows:
1) taking 1g of analytically pure ferric citrate, 2g of nickel nitrate and 3g of carbodiimide, and mixing and grinding in a glass mortar to obtain a mixture, wherein the mixture is marked as A;
2) heating the mixture A to 900 ℃ at a speed of 15 ℃/min in a low-temperature tube furnace, preserving the heat for 1h, cooling and taking out to obtain a product B;
3) mixing and grinding the product B and trithiocyanuric acid with the mass of 4 times of that of the product B in a glass mortar to obtain a mixture C;
4) and heating the mixture C to 350 ℃ at the speed of 6 ℃/min in a low-temperature tubular furnace, calcining for 1h, cooling and taking out to obtain a product D, namely the iron-nickel bimetallic sulfide.
Example 8:
the process for preparing the iron-nickel sulfide according to the mass ratio of the reactants of 1:1:6 is as follows:
1) taking 1g of analytically pure ferric oxalate, 1g of nickel nitrate and 6g of urea, mixing and grinding in a glass mortar to obtain a mixture, wherein the mixture is marked as A;
2) heating the mixture A to 1000 ℃ at a speed of 20 ℃/min in a low-temperature tube furnace, preserving the temperature for 1h, cooling and taking out to obtain a product B;
3) mixing and grinding the product B and trithiocyanuric acid with the mass of 4 times of that of the product B in a glass mortar to obtain a mixture C;
4) and heating the mixture C to 300 ℃ at the speed of 5 ℃/min in a low-temperature tubular furnace, calcining for 2h, cooling and taking out to obtain a product D, namely the iron-nickel bimetallic sulfide.
Example 9:
the process for preparing the iron-nickel sulfide according to the mass ratio of the reactants of 1:2:4 is as follows:
1) taking 1g of analytically pure ferric citrate, 2g of nickel nitrate and 4g of melamine, and mixing and grinding in a glass mortar to obtain a mixture, wherein the mixture is marked as A;
2) heating the mixture A to 650 ℃ at the speed of 5 ℃/min in a low-temperature tube furnace, preserving the heat for 3h, cooling and taking out to obtain a product B;
3) mixing and grinding the product B and trithiocyanuric acid with the mass of 2 times of the product B in a glass mortar to obtain a mixture C;
4) and heating the mixture C to 400 ℃ at the speed of 6 ℃/min in a low-temperature tubular furnace, calcining for 3h, cooling and taking out to obtain a product D, namely the iron-nickel bimetallic sulfide.
Claims (10)
1. The preparation method of the iron-nickel sulfide is characterized by comprising the following steps of:
step 1, mixing and grinding organic acid salts of iron, nickel nitrate and organic matters of carbon-nitrogen source according to the mass ratio of (1) - (3) to (1) - (7) to obtain a mixture A;
step 2, carrying out heat treatment on the mixture A at 500-1200 ℃ for 1-5 h, cooling and taking out to obtain a product B,
step 3, mixing and grinding the product B and a sulfur source uniformly according to a mass ratio of 1 (5-10) to obtain a mixture C;
and 4, carrying out heat treatment on the mixture C at the temperature of 300-600 ℃ for 30 min-1 h, cooling and taking out to obtain a product D, namely the iron-nickel sulfide.
2. The method according to claim 1, wherein in step 1, the organic acid salt of iron is analytically pure, and the organic acid salt of iron comprises ferric citrate, ferric oxalate or ferric acetate.
3. The method for producing iron-nickel sulfide as claimed in claim 1, wherein in step 1, the organic carbon-nitrogen source includes urea, melamine, carbodiimide, cyanuric acid or trithiocyanuric acid.
4. The method of claim 1, wherein the milling time in step 1 is half an hour.
5. The method for preparing iron-nickel sulfide according to claim 1, wherein in the step 2, the temperature rise rate of the heat treatment is 2-20 ℃/min, and the iron-nickel sulfide is cooled along with the furnace.
6. The method for preparing iron-nickel sulfide according to claim 1, wherein in the step 3, one or more of sublimed sulfur, thioacetamide or trithiocyanuric acid is used as the sulfur source.
7. The method for preparing iron-nickel sulfide according to claim 1, wherein in the step 4, the temperature rise rate of the heat treatment is 5 ℃/min to 10 ℃/min, and the iron-nickel sulfide is cooled along with the furnace.
8. An iron-nickel sulfide prepared by the preparation method according to any one of claims 1 to 7, wherein the iron-nickel sulfide particles have a continuous carbon layer-coated particle structure.
9. A sodium ion battery, characterized in that the iron-nickel sulfide as claimed in claim 8 is used as a battery negative electrode material.
10. The sodium ion battery of claim 9, wherein the iron nickel sulfide maintains nanoscale dimensions during charging and discharging.
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| CN110224126B (en) * | 2019-06-14 | 2020-12-29 | 陕西科技大学 | Iron-nickel sulfide nano material and preparation method and application thereof |
| CN111312999A (en) * | 2020-02-20 | 2020-06-19 | 肇庆市华师大光电产业研究院 | Preparation method of graphene-coated nickel-iron bimetallic sulfide sodium-ion battery negative electrode material |
| CN111900385B (en) * | 2020-07-29 | 2022-04-26 | 肇庆市华师大光电产业研究院 | Novel negative electrode material of potassium ion battery and preparation method thereof |
| CN112408496A (en) * | 2020-11-09 | 2021-02-26 | 邵阳学院 | Nitrogen and sulfur co-doped carbon @ FeS nanotube and preparation method and application thereof |
| CN113224303B (en) * | 2021-05-08 | 2022-08-05 | 陕西科技大学 | Preparation method of iron cyanamide material for realizing graphitized carbon coating by in-situ autocatalysis |
| CN113548700A (en) * | 2021-07-26 | 2021-10-26 | 河南师范大学 | Preparation method of iron-nickel-nitrogen-carbon nano material |
| CN113793760A (en) * | 2021-08-19 | 2021-12-14 | 江苏工程职业技术学院 | Preparation method of one-step electro-deposition nickel-iron sulfide nano composite electrode |
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