CN111653753A - Preparation method of iron sulfide composite positive electrode material of sulfide all-solid-state battery - Google Patents
Preparation method of iron sulfide composite positive electrode material of sulfide all-solid-state battery Download PDFInfo
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- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
- H01M2300/0068—Solid electrolytes inorganic
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a sulfide all-solid-state battery iron sulfide composite positive electrode material2And then FeS2The carbon material and the sulfide solid electrolyte raw material are combined together by a high-temperature melting method, and then high-performance FeS is obtained by low-temperature tempering2And (3) compounding the positive electrode material. Compared with the traditional composite anode, the method improves the contact area of the anode material and the solid electrolyte, and accelerates the transmission rate of lithium ions at the interface; further enhancing the positive electrode,The contact tightness between the carbon material and the sulfide solid electrolyte promotes the uniform distribution of the carbon material and the sulfide solid electrolyte; the interface charge layer of the anode and the solid electrolyte can be effectively inhibited, and the interface impedance is reduced; the prepared composite anode material has higher density and can improve the energy density of the all-solid-state battery.
Description
Technical Field
The invention belongs to the field of all-solid-state batteries, and particularly relates to a preparation method of a sulfide all-solid-state battery iron sulfide composite positive electrode material.
Background
In recent years, new energy such as wind power, photovoltaic and the like is rapidly increased, and the installed scale of the new energy far exceeds the consumption capacity of a power grid while the new energy is greatly developed, so that more wind abandon and light abandon rates are caused. In addition, renewable energy sources such as wind power and photovoltaic have the characteristics of intermittence, volatility and the like, so that the power grid regulation and anti-interference capability are continuously reduced, and a series of major challenges are brought to the absorption of new energy sources, the internet surfing and the stable operation of the power grid. In the case of fluctuating power generation reaching such a high proportion, it is more challenging to ensure a real-time balance between power supply and demand. The energy storage device can be used for effectively managing the volatility and uncertainty related to high-proportion wind power generation and solar power generation. The electrochemical energy storage is a trend of large-scale energy storage development in the future due to the advantages of high energy density, good rate capability, low self-discharge rate, long service life, high energy conversion efficiency, high reaction speed and the like. However, the current electrochemical energy storage battery has a large safety problem, so that the battery has a certain distance from large-scale application.
The all-solid-state lithium ion battery can completely solve the safety problem of the battery because the all-solid-state lithium ion battery does not contain combustible organic electrolyte. The solid electrolyte may be classified into an inorganic solid electrolyte, an organic solid electrolyte, and a composite solid electrolyte, in which a sulfide solid electrolyte having a high normal-temperature ionic conductivity is considered to be one of the most promising solid electrolytes for industrialization. However, at present, sulfide all-solid-state batteries still face more problems, the biggest problem being the interface between the solid electrolyte and the electrode. Since there is no wetting of the liquid in the all-solid battery, the contact between the electrode and the electrolyte is a solid-solid contact, in fact a point-to-point contact, and the superior condition of the interfacial contact determines the electrochemical performance of the entire all-solid battery.
Disclosure of Invention
According to the inventionAims to overcome the defects of the prior art and provide a sulfide all-solid-state battery FeS2The preparation method of the composite anode material can greatly increase the contact area between the anode and the sulfide solid electrolyte and solve the problem of interface.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a sulfide all-solid-state battery iron sulfide composite positive electrode material comprises the following steps:
1) FeS is prepared2Ball milling the raw materials to obtain FeS2Powder;
2) under argon atmosphere, FeS2Mixing and ball-milling the powder and the carbon material to obtain FeS2A carbon/carbon composite;
3) FeS is prepared2Carbon/carbon composite material, Li2S and P2S5Mixing, placing in a container, sealing the container containing the mixed powder in a vacuum device, heat treating the vacuum device at high temperature, and immediately quenching in ice water when heating is finished;
4) cooling to normal temperature, heat treating the vacuum device again to crystallize the quenched glass solid electrolyte, cooling again, and opening the vacuum device in argon atmosphere to obtain FeS2And (3) compounding the positive electrode material.
Further, the rotation speed of the ball milling in the step 1) is 370 and 510rpm, and the ball milling time is 2-4 h.
Further, the carbon material is conductive carbon black, carbon fiber, carbon nanorod or carbon nanotube.
Further, the FeS2The mass ratio of the powder to the carbon material is (2.0-4.0): 1.
Further, the rotation speed of the ball milling in the step 2) is 120-.
Further, FeS in step 3)2Carbon/carbon composite material, Li2S and P2S5When mixed, Li2S and P2S5In a molar ratio of Li2S:P2S5＝(2.0～4.0) 1 adding FeS2Carbon/carbon composites with Li2S+P2S5The mass ratio of (1) to (3.0).
Further, the container containing the mixed powder in the step 3) is sealed in a vacuum device, and the vacuum degree of the vacuum device is lower than 0.1 MPa.
Further, the temperature of the high-temperature heat treatment of the vacuum device in the step 3) is 650-.
Further, the temperature of the heat treatment in the step 4) is 240-260 ℃, and the time is controlled to be 1-3 h.
Further, the argon atmosphere is realized through an argon glove box, and O in the argon glove box2Content less than 0.1ppm, H2The O content is less than 0.1 ppm.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention prepares the FeS of the sulfide all-solid-state battery by a high-temperature quenching method2The composite cathode material has quite obvious advantages, and the most important advantages are as follows: (1) the method improves FeS2The contact area of the anode material and the solid electrolyte is changed from point contact between solids in the original mechanical cold pressing process into surface contact, so that the transmission rate of lithium ions at an interface is increased; (2) the method enhances the contact tightness among the anode, the carbon material and the sulfide solid electrolyte, and the melting method promotes the uniform distribution of the anode, the carbon material and the sulfide solid electrolyte in the composite anode; (3) the positive electrode material prepared by the method can effectively inhibit the interface charge layer of the positive electrode and the solid electrolyte, and reduce the interface impedance; (4) compared with the positive electrode material pressed by the conventional method, the positive electrode material prepared by the method has higher density, and the density of the positive electrode material in the battery can be improved, so that the energy density of the battery is improved.
Drawings
FIG. 1 is a conventional FeS2Schematic representation of composite positive electrode material;
FIG. 2 shows FeS prepared according to the present invention2Schematic diagram of composite positive electrode material.
Wherein 1 is FeS2A positive electrode material; 2 is a carbon material; 3 is a sulfide solidAn electrolyte.
Detailed Description
Embodiments of the invention are described in further detail below:
sulfide all-solid-state battery FeS2The preparation method of the composite anode material comprises the steps of firstly, preparing FeS2The raw materials are placed in a ball milling tank, and FeS is reduced by high-energy ball milling2The ball milling speed is 370 plus 510rpm, the ball milling time is 2 to 4 hours, and the FeS is obtained2And (3) powder. Taking a proper amount of prepared FeS under the argon atmosphere2The powder and carbon materials (carbon materials such as conductive carbon black, carbon fibers, carbon nanorods, carbon nanotubes and the like) are placed in a ball milling tank according to the mass ratio of (2.0-4.0) to 1 for mixing, the ball milling rotation speed is 120 plus 180rpm at normal temperature, and the ball milling time is 1-3h, so that FeS is obtained2A carbon/carbon composite material. Then, FeS is added2Carbon and Li2S、P2S5Mixing at a certain ratio, wherein Li is added2S and P2S5In a molar ratio of Li2S:P2S5＝(2.0～4.0):1，FeS2Carbon and Li2S+P2S5The mass ratio of the two is 1 (1.0-3.0), the mixed powder is placed in a stainless steel container, then the stainless steel container containing the mixed powder is sealed in a vacuum quartz tube, and the vacuum degree of the vacuum quartz glass tube is lower than 0.1 Mpa. Heat-treating the quartz tube at 650-. After cooling to normal temperature, the quartz tube is thermally treated again for 1-3h at the temperature of 240-260 ℃ to crystallize the glass solid electrolyte obtained by quenching. After cooling, the quartz tube was opened in an argon glove box, O in which2Content less than 0.1ppm, H2The content of O is less than 0.1ppm, thus obtaining FeS2FIG. 2 shows FeS prepared by the present invention2The schematic diagram of the composite cathode material shows FeS in the composite cathode material prepared by the high-temperature quenching method2The contact among the anode material 1, the carbon material 2 and the sulfide solid electrolyte 3 is more compact and is uniformly distributed, the contact area among the materials is increased, and the transmission of lithium ions is widenedA channel. By contrast, FIG. 1 is a conventional FeS2According to the schematic diagram of the composite cathode material, larger pores exist among the cathode materials, and the contact area is very small.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. The present invention is described in further detail below with reference to examples:
example 1
Firstly, 2.0g of FeS is taken2The raw materials are placed in a ball milling tank, and FeS is reduced by high-energy ball milling2The ball milling speed is 370rpm, and the ball milling time is 4.0 h. In a glove box (O)2<0.1ppm,H2O<0.1ppm), taking FeS with reduced particle size22.0g of the powder and 1.0g of the conductive carbon black are mixed in a ball milling tank, and the mixture is ball milled for 3.0h at the rotating speed of 120rpm at normal temperature to obtain FeS2Conductive carbon black composite. Then, Li was weighed in a glove box2S mass 0.9827g, P2S5Mass 2.0173g, FeS23.0g of the conductive carbon black composite material was mixed together, the mixed powder was placed in a stainless steel container, and then the stainless steel container containing the mixed powder was sealed in a vacuum quartz tube having a degree of vacuum of less than 0.1 MPa. And (3) carrying out high-temperature heat treatment on the vacuum quartz tube, wherein the heat treatment temperature is 650 ℃, and the sintering time is controlled to be 3.0 h. After the heating was completed, the hot quartz tube was immediately quenched in ice water below zero degrees. And cooling to normal temperature, then carrying out heat treatment on the quartz tube for a period of time again, controlling the temperature of the secondary heat treatment at 240 ℃ and the sintering time at 3.0h, and carrying out recrystallization on the quenched glass solid electrolyte crystal. After cooling, opening the quartz tube in the argon atmosphere, taking out the sample, and grinding the sample into powder to obtain FeS2And (3) compounding the positive electrode material.
Example 2
Firstly, 3.0g of FeS is taken2The raw materials are placed in a ball milling tank, and FeS is reduced by high-energy ball milling2The rotation speed of ball milling is 450rpm, and the ball milling time is 3.0 h. In a glove box (O)2<0.1ppm,H2O<0.1ppm), taking FeS with reduced particle size23.0g of powder and 1.0g of carbon fiber are mixed in a ball milling tank, and the mixture is ball milled for 2.0h at the rotating speed of 150rpm at normal temperature to obtain FeS2A composite material of carbon fiber. Then, Li was weighed in a glove box2S mass 1.1554g, P2S5Mass 1.8445g, FeS21.5g of the carbon fiber/carbon fiber composite material was mixed together, the mixed powder was placed in a stainless steel container, and then the stainless steel container containing the mixed powder was sealed in a vacuum quartz tube having a degree of vacuum of less than 0.1 MPa. And (3) carrying out high-temperature heat treatment on the vacuum quartz tube, wherein the heat treatment temperature is 750 ℃, and the sintering time is controlled to be 2.0 h. After the heating was completed, the hot quartz tube was immediately quenched in ice water below zero degrees. And cooling to normal temperature, then carrying out heat treatment on the quartz tube for a period of time again, controlling the temperature of the secondary heat treatment at 250 ℃ and the sintering time at 2.0h, and carrying out recrystallization on the quenched glass solid electrolyte crystal. After cooling, opening the quartz tube in the argon atmosphere, taking out the sample, and grinding the sample into powder to obtain FeS2And (3) compounding the positive electrode material.
Example 3
Firstly, 4.0g of FeS is taken2The raw materials are placed in a ball milling tank, and FeS is reduced by high-energy ball milling2The rotation speed of ball milling is 510rpm, and the ball milling time is 2.0 h. In a glove box (O)2<0.1ppm,H2O<0.1ppm), taking FeS with reduced particle size24.0g of powder and 1.0g of carbon nano tube are mixed in a ball milling tank, and the mixture is ball milled for 1.0h at the rotating speed of 180rpm at normal temperature to obtain FeS2A composite material of carbon nano tube. Then, Li was weighed in a glove box2S mass 1.358g, P2S5Mass 1.642g, FeS21.0g of the carbon nanotube composite material was mixed together, the mixed powder was placed in a stainless steel container, and then the stainless steel container containing the mixed powder was sealed in a vacuum quartz tube having a low degree of vacuumAt 0.1 MPa. And (3) carrying out high-temperature heat treatment on the vacuum quartz tube, wherein the heat treatment temperature is 800 ℃, and the sintering time is controlled to be 1.0 h. After the heating was completed, the hot quartz tube was immediately quenched in ice water below zero degrees. And cooling to normal temperature, then carrying out heat treatment on the quartz tube for a period of time again, controlling the temperature of the secondary heat treatment at 260 ℃ and the sintering time at 1.0h, and carrying out recrystallization on the quenched glass solid electrolyte crystal. After cooling, opening the quartz tube in the argon atmosphere, taking out the sample, and grinding the sample into powder to obtain FeS2And (3) compounding the positive electrode material.
According to the method, the sulfide solid electrolyte material, the carbon material and the anode material are combined together through a melting method, so that the interface contact area is increased, the interface impedance is reduced, and the density of the anode is further improved, so that the energy density of the all-solid-state battery is improved.
In the embodiments provided in the present application, the technical content disclosed mainly aims at the preparation method of the sulfide composite positive electrode material of the all-solid-state battery, the above is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by a person skilled in the art within the technical scope disclosed in the present invention, or equivalent structures or equivalent flow transformations made by the contents of the present specification and the drawings, or directly or indirectly applied to other related technical fields, should be covered within the scope of the present invention.
Claims (10)
1. A preparation method of a sulfide all-solid-state battery iron sulfide composite positive electrode material is characterized by comprising the following steps:
1) FeS is prepared2Ball milling the raw materials to obtain FeS2Powder;
2) under argon atmosphere, FeS2Mixing and ball-milling the powder and the carbon material to obtain FeS2A carbon/carbon composite;
3) FeS is prepared2Carbon/carbon composite material, Li2S and P2S5Mixing, placing in a container, sealing the container containing the mixed powder in a vacuum device, and heat treating at high temperatureThe vacuum device is used for immediately placing the hot vacuum device in ice water for quenching when heating is finished;
4) cooling to normal temperature, heat treating the vacuum device again to crystallize the quenched glass solid electrolyte, cooling again, and opening the vacuum device in argon atmosphere to obtain FeS2And (3) compounding the positive electrode material.
2. The method for preparing the iron sulfide composite cathode material for the sulfide all-solid-state battery as claimed in claim 1, wherein the rotation speed of the ball milling in the step 1) is 370-510rpm, and the ball milling time is 2-4 h.
3. The method for preparing the iron sulfide composite cathode material for the sulfide all-solid battery, according to claim 1, wherein the carbon material is conductive carbon black, carbon fiber, carbon nanorod or carbon nanotube.
4. The method for preparing the iron sulfide composite positive electrode material of the sulfide all-solid-state battery according to claim 1, wherein the FeS is2The mass ratio of the powder to the carbon material is (2.0-4.0): 1.
5. The method for preparing the iron sulfide composite cathode material for the sulfide all-solid-state battery as claimed in claim 1, wherein the rotation speed of the ball milling in the step 2) is 120-180rpm, and the ball milling time is 1-3 h.
6. The method for preparing the iron sulfide composite positive electrode material of the sulfide all-solid-state battery according to claim 1, wherein FeS is used in the step 3)2Carbon/carbon composite material, Li2S and P2S5When mixed, Li2S and P2S5In a molar ratio of Li2S:P2S51 part of FeS is added in the formula (2.0-4.0)2Carbon/carbon composites with Li2S+P2S5The mass ratio of (1) to (3.0).
7. The method for preparing the iron sulfide composite cathode material for the sulfide all-solid battery according to claim 1, wherein the container containing the mixed powder in the step 3) is sealed in a vacuum device, and the vacuum degree of the vacuum device is lower than 0.1 Mpa.
8. The method for preparing the iron sulfide composite cathode material for the sulfide all-solid-state battery as claimed in claim 1, wherein the temperature of the high-temperature heat treatment of the vacuum device in the step 3) is 650-800 ℃, and the time is controlled to be 1-3 h.
9. The method for preparing the iron sulfide composite cathode material for the sulfide all-solid-state battery as claimed in claim 1, wherein the temperature of the heat treatment in the step 4) is 240-260 ℃, and the time is controlled to be 1-3 h.
10. The method for preparing the iron sulfide composite cathode material for the sulfide all-solid-state battery according to claim 1, wherein the argon atmosphere is realized through an argon glove box, and O in the argon glove box2Content less than 0.1ppm, H2The O content is less than 0.1 ppm.
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| CN202010598568.3A CN111653753A (en) | 2020-06-28 | 2020-06-28 | Preparation method of iron sulfide composite positive electrode material of sulfide all-solid-state battery |
| PCT/CN2021/100601 WO2022001681A1 (en) | 2020-06-28 | 2021-06-17 | Preparation method for iron sulfide composite positive electrode material of sulfide all-solid-state battery |
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| US20210028440A1 (en) * | 2018-03-16 | 2021-01-28 | University Of Maryland, College Park | All solid-state sodium-sulfur or lithium-sulfur battery prepared using cast-annealing method |
| WO2022001681A1 (en) * | 2020-06-28 | 2022-01-06 | 中国华能集团清洁能源技术研究院有限公司 | Preparation method for iron sulfide composite positive electrode material of sulfide all-solid-state battery |
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| CN116646503A (en) * | 2023-07-27 | 2023-08-25 | 河南师范大学 | Preparation method of carbon-coated transition metal telluride and application of carbon-coated transition metal telluride in water-based zinc ion battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20210028440A1 (en) * | 2018-03-16 | 2021-01-28 | University Of Maryland, College Park | All solid-state sodium-sulfur or lithium-sulfur battery prepared using cast-annealing method |
| US11949092B2 (en) * | 2018-03-16 | 2024-04-02 | University Of Maryland, College Park | All solid-state sodium-sulfur or lithium-sulfur battery prepared using cast-annealing method |
| WO2022001681A1 (en) * | 2020-06-28 | 2022-01-06 | 中国华能集团清洁能源技术研究院有限公司 | Preparation method for iron sulfide composite positive electrode material of sulfide all-solid-state battery |
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| WO2022001681A1 (en) | 2022-01-06 |
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