CN110212161B - Lithium ion battery cathode and preparation method thereof - Google Patents

Lithium ion battery cathode and preparation method thereof Download PDF

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CN110212161B
CN110212161B CN201910546249.5A CN201910546249A CN110212161B CN 110212161 B CN110212161 B CN 110212161B CN 201910546249 A CN201910546249 A CN 201910546249A CN 110212161 B CN110212161 B CN 110212161B
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substrate
nanowire array
lithium ion
ion battery
nise
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CN110212161A (en
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王佳莹
王志明
余鹏
马翠苹
童鑫
林峰
巫江
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University of Electronic Science and Technology of China
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00—Selenium; Tellurium; Compounds thereof
    • C01B19/007—Tellurides or selenides of metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/04—Processes of manufacture in general
    • H01M4/0402—Methods of deposition of the material
    • H01M4/0421—Methods of deposition of the material involving vapour deposition
    • H01M4/0423—Physical vapour deposition
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/04—Processes of manufacture in general
    • H01M4/0402—Methods of deposition of the material
    • H01M4/0421—Methods of deposition of the material involving vapour deposition
    • H01M4/0423—Physical vapour deposition
    • H01M4/0426—Sputtering
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/04—Processes of manufacture in general
    • H01M4/049—Manufacturing of an active layer by chemical means
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • 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 lithium ion battery cathode which comprises a substrate, wherein an electrode film layer is deposited on the substrate, and the electrode film layer is of a nanowire array structure. The electrode film layer with the nanowire array structure is deposited on the substrate by adopting electron beam evaporation, can be firmly attached to the substrate material without using an adhesive, and avoids the performance influence of the adhesive on the cathode active material. The application also provides a preparation method of the lithium ion battery cathode.

Description

Lithium ion battery cathode and preparation method thereof
Technical Field
The invention relates to the technical field of lithium batteries, in particular to a lithium ion battery cathode and a preparation method thereof.
Background
With the wide application of lithium ion batteries in daily life of people, research and development of new lithium ion battery technologies are put into great numbers of colleges, research institutions and enterprises. The method aims to improve the specific capacity, the cycle life and other performances of the lithium ion battery.
The negative electrode of the lithium ion battery is one of the factors which play a decisive role in the performance of the battery, and the performance of the negative electrodes of the batteries prepared by adopting different materials has great difference. Experiments show that NiSe is adopted2The specific discharge capacity of the lithium ion battery with the material as the negative electrode can reach 800 mAh.g-1Much higher than the LiFePO widely used at present4(170mAh·g-1) Has great application prospect.
The problem is that NiSe2In the preparation process of the lithium ion battery with the negative electrode, a binder is generally adopted to mix electrochemical active materials and then coat the electrochemical active materials on a negative electrode substrate. The negative active material is soaked in the binder for a long time, is easy to cause pulverization and peeling of the active material, and is dissolved in the binder, so that the negative active material which can participate in charge-discharge reaction is reduced, and irreversible loss of charge-discharge capacity of the lithium ion battery is caused.
Disclosure of Invention
In view of this, the present application provides a lithium ion battery cathode, which employs electron beam evaporation to deposit an electrode film layer with a nanowire array structure on a substrate, and can be stably attached to the substrate material without using an adhesive, thereby avoiding the performance influence of the adhesive on the cathode active material. The application also provides a preparation method of the lithium ion battery cathode.
In order to solve the technical problems, the technical scheme provided by the invention is that the lithium ion battery cathode comprises a substrate, wherein an electrode film layer is deposited on the substrate, and the electrode film layer is of a nanowire array structure.
Preferably, the nanowire array structure and the substrate form an included angle of 8-15 degrees.
Preferably, the electrode film layer is NiSe2A nanowire array of material.
Preferably, the substrate is a stainless steel sheet, and an 80-120nm Ti layer is arranged between the substrate and the electrode film layer.
The invention also provides a preparation method of the lithium ion battery cathode, which comprises the following steps:
pretreating a substrate;
NiSe formation on a substrate2And (3) preparing an electrode film layer of the nanowire array.
Preferably, the step of pretreating the substrate specifically comprises:
taking a stainless steel sheet as a substrate;
cleaning the stainless steel sheet, wherein the cleaning agent is at least one of acetone or ethanol;
and arranging a Ti layer with the thickness of 80-120nm on the stainless steel sheet by adopting magnetron sputtering.
Preferably, the NiSe is formed on a substrate2The method comprises the following steps of preparing an electrode film layer of the nanowire array:
depositing a Ni nanowire array on a substrate through electron beam evaporation;
selenizing Ni nanowire array into NiSe2A nanowire array of material.
Preferably, the step of depositing the nanowire array made of the Ni material on the substrate by electron beam evaporation specifically includes:
the substrate is arranged obliquely, the Ni material evaporated by the electron beam is deposited on the substrate by adopting a grazing angle, and the deposition angle of the grazing angle is 8-15 degrees; the deposition rate of the Ni nanowire array is 0.25-0.35nm · s-1The deposition thickness on the substrate was 450-550 nm.
Preferably, the Ni nanowire array is selenized into NiSe2The method comprises the following steps of preparing a nanowire array, specifically:
moving the substrate deposited with the Ni material nanowire array into a selenization cavity;
3-4g of Se nanoparticles are put into the selenization cavity;
introduction of N2And H2The Se nanoparticles are brought into an inductively coupled plasma region;
at 14-16 deg.C/min-1The rate of (a) is to raise the temperature from room temperature to 400 ℃ and maintain it;
low-temperature plasma in inductive coupling plasma region promotes selenization of Ni material nanowire array to generate NiSe2A nanowire array of material.
Preferably, said introduction of N2And H2The step of bringing the Se nanoparticles into the inductively coupled plasma region comprises the following specific steps: n is a radical of2And H2The aeration ratio of (1) is 2:3, and the flow rate of the mixed gas is 90-110 ml.min-1。
Compared with the prior art, the application has the beneficial effects that:
a layer of nanowire array structure is generated on the substrate through electron beam evaporation and is firmly attached to the substrate through deposition, and an adhesive is not needed, so that the influence of the adhesive on the performance of the active negative electrode material is avoided.
A certain included angle exists between the nanowire array structure and the substrate, so that the nanowire array structure is stably attached to the substrate, a larger reaction area is kept, and electrochemical reaction can be better carried out.
The Ti layer is arranged on the substrate of the stainless steel sheet, and the stainless steel sheet and the negative active material are isolated, so that the substrate is used as a bearing structural member and does not participate in the reaction of the lithium ion battery, and the stable performance of the lithium ion battery is ensured.
Drawings
FIG. 1 is a schematic structural diagram of a negative electrode of a lithium ion battery according to the present invention;
FIG. 2 is a scanning electron microscope characterization pattern of a lithium ion battery cathode of the present invention;
FIG. 3 is a schematic view of a process for preparing a lithium ion battery cathode according to the present invention;
FIG. 4 is a first charge-discharge curve diagram of a lithium ion battery according to the present invention;
fig. 5 is a graph of cycle performance of a lithium ion battery of the present invention.
Reference numerals: the plasma processing device comprises a substrate 1, a Ti layer 2, an electrode film layer 3, a selenization cavity 4, an inductively coupled plasma coil 5 and an inductively coupled plasma region 51.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the accompanying drawings and specific embodiments.
Referring to fig. 1 and fig. 2, an embodiment of the invention provides a negative electrode of a lithium ion battery, including a substrate 1 made of a stainless steel sheet. An electrode film layer 3 is deposited on the substrate 1, and the electrode film layer 3 is NiSe2A nanowire array structure of material. The nanowire array structure and the substrate 1 form an included angle of 8-15 degrees. A Ti layer of 80-120nm is arranged between the substrate 1 and the electrode film layer 3.
Referring to fig. 3, the present invention further provides a method for preparing the negative electrode of the lithium ion battery, including the following steps:
taking a stainless steel sheet as a substrate 1;
cleaning the stainless steel sheet, wherein the cleaning agent is at least one of acetone or ethanol;
arranging a Ti layer 2 with the thickness of 80-120nm on the stainless steel sheet by adopting magnetron sputtering;
depositing a Ni nanowire array on the substrate 1 provided with the Ti layer 2 through electron beam evaporation to serve as an electrode film layer 3; the substrate 1 is obliquely arranged, an included angle theta is formed between the substrate 1 and a vertical plane, the Ni material evaporated by the electron beam is deposited on the substrate 1 in a glancing angle, and the deposition angle theta of the glancing angle is8-15 degrees; the deposition rate of the Ni nanowire array is 0.25-0.35nm · s-1The deposition thickness on the substrate 1 is 450-550 nm;
moving the substrate 1 deposited with the Ni material nanowire array into a selenization cavity 4;
3-4g of Se nano particles are put into the selenization cavity 4;
introduction of N2And H2Mixed gas of (2), N2And H2The aeration ratio of (1) is 2:3, and the flow rate of the mixed gas is 90-110 ml.min-1(ii) a The mixed gas brings Se nano-particles into the inductively coupled plasma coils 5 which are arranged in pairs; an inductive coupling plasma area 51 is arranged between the inductive coupling plasma coils 5 which are arranged in pairs, and the generated low-temperature plasma can selenize the Ni nanowire array; the low temperature in this embodiment means 400 ℃ and the plasma is a Se element.
At 14-16 deg.C/min-1The rate of (a) is to raise the temperature from room temperature to 400 ℃ and maintain it;
the low-temperature plasma of the inductive coupling plasma area 51 promotes the selenization of the Ni material nanowire array to generate NiSe2A nanowire array of material.
Example one
The embodiment provides a preparation method of a lithium ion battery cathode, which comprises the following steps:
taking a stainless steel sheet as a substrate 1; in the present embodiment, a square stainless steel sheet having a side of 1cm is preferable;
cleaning a stainless steel sheet, wherein the cleaning agent is acetone;
arranging a Ti layer 2 with the thickness of 80nm on a stainless steel sheet by adopting magnetron sputtering;
depositing a Ni nanowire array on the substrate 1 provided with the Ti layer 2 through electron beam evaporation to serve as an electrode film layer 3; the substrate 1 is obliquely arranged, an included angle theta is formed between the substrate 1 and a vertical plane, the Ni material evaporated by electron beams is deposited on the substrate 1 in a glancing angle, and the glancing angle deposition angle theta is 8 degrees; the deposition rate of the Ni nanowire array is 0.25nm s-1The deposition thickness on the substrate 1 was 450 nm;
moving the substrate 1 deposited with the Ni material nanowire array into a selenization cavity 4;
3g of Se nanoparticles are put into the selenization cavity 4;
introduction of N2And H2Mixed gas of (2), N2And H2The aeration ratio of (2: 3) and the flow rate of the mixed gas of 90 ml/min-1(ii) a The mixed gas brings the Se nanoparticles into the inductively coupled plasma region 51;
at 14 ℃ min-1The rate of raising the temperature from room temperature to 400 ℃ and maintaining it;
selenizing the Ni nanowire array by the low-temperature plasma in the inductively coupled plasma region 51 to generate NiSe2A nanowire array of material.
Example two
The invention also provides a preparation method of the lithium ion battery cathode, which comprises the following steps:
taking a stainless steel sheet as a substrate 1; in the present embodiment, a square stainless steel sheet having a side of 2cm is preferable;
cleaning the stainless steel sheet, wherein the cleaning agent is ethanol;
arranging a Ti layer 2 with the thickness of 120nm on the stainless steel sheet by adopting magnetron sputtering;
depositing a Ni nanowire array on the substrate 1 provided with the Ti layer 2 through electron beam evaporation to serve as an electrode film layer 3; the substrate 1 is obliquely arranged, an included angle theta is formed between the substrate 1 and a vertical plane, the Ni material evaporated by electron beams is deposited on the substrate 1 in a glancing angle, and the deposition angle theta of the glancing angle is 15 degrees; the deposition rate of the Ni nanowire array is 0.35nm s-1The deposition thickness on the substrate 1 was 550 nm;
moving the substrate 1 deposited with the Ni material nanowire array into a selenization cavity 4;
putting 4g of Se nanoparticles into the selenization cavity 4;
introduction of N2And H2Mixed gas of (2), N2And H2The aeration ratio of (2: 3) and the flow rate of the mixed gas of 110 ml/min-1(ii) a The mixed gas brings the Se nanoparticles into the inductively coupled plasma region 51;
at 16 ℃ min-1Rate ofRaising the temperature from room temperature to 400 ℃ and maintaining;
selenizing the Ni nanowire array by the low-temperature plasma in the inductively coupled plasma region 51 to generate NiSe2A nanowire array of material.
EXAMPLE III
The embodiment provides a preparation method of a lithium ion battery cathode, which comprises the following steps:
taking a stainless steel sheet as a substrate 1;
cleaning a stainless steel sheet, wherein the cleaning agent is ethanol;
arranging a Ti layer 2 with the thickness of 100nm on a stainless steel sheet by adopting magnetron sputtering;
depositing a Ni nanowire array on the substrate 1 provided with the Ti layer 2 through electron beam evaporation to serve as an electrode film layer 3; the substrate 1 is obliquely arranged, an included angle theta is formed between the substrate 1 and a vertical plane, the Ni material evaporated through electron beams is deposited on the substrate 1 in a glancing angle mode, and the glancing angle deposition angle theta is 10 degrees; the deposition rate of the Ni nanowire array is 0.3nm s-1The deposition thickness on the substrate 1 was 500 nm;
moving the substrate 1 deposited with the Ni material nanowire array into a selenization cavity 4;
3g of Se nanoparticles are put into the selenization cavity 4;
introduction of N2And H2Mixed gas of (2), N2And H2The aeration ratio of (2: 3) and the flow rate of the mixed gas of 100 ml/min-1(ii) a The mixed gas brings the Se nanoparticles into the inductively coupled plasma region 51;
at 15 ℃ in min-1The rate of (a) is to raise the temperature from room temperature to 400 ℃ and maintain it;
selenizing the Ni nanowire array by the low-temperature plasma in the inductively coupled plasma region 51 to generate NiSe2A nanowire array of material.
Example four
Taking the negative electrode of the lithium ion battery prepared in the third example as a negative electrode, taking a metal lithium sheet as a counter electrode, and adding 1mol of LiPF6Dissolving in mixed solution of ethylene carbonate and diethyl carbonate in the volume ratio of 1:1 to obtain electrolyteAnd (4) obtaining the CR2032 type lithium ion battery.
Referring to fig. 4, the battery prepared in this example was tested for constant current charging and discharging at room temperature, with a voltage range of 0.01-3.0V. When the current density is 0.5A · g-1The first charge and discharge capacity are 741.6 and 745.3mAh g-1. Referring to FIG. 5, when the current density is 1A g-1In this case, 694.2mAh g was still retained after 1000 cycles of charging and discharging in the lithium ion battery prepared in this example-1The discharge capacity of (2).
According to the lithium ion battery cathode and the preparation method thereof, Ni is evaporated by electron beams and is deposited on a substrate 1 in a glancing angle, and then selenization is carried out in an inductively coupled plasma region 51 formed by the inductively coupled plasma coils 5 arranged oppositely to prepare NiSe2And (4) nanowire arrays. The preparation of the battery cathode can be realized without depending on a binder, and the influence of the binder on the performance of the cathode active material is avoided. Experiments show that the lithium ion battery prepared by the lithium ion battery cathode provided by the application has good charge and discharge performance and cycling stability, and has good electrochemical performance.
The above is only a preferred embodiment of the present invention, and it should be noted that the above preferred embodiment should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and these modifications and adaptations should be considered within the scope of the invention.

Claims (6)

1. The lithium ion battery cathode comprises a substrate, and is characterized in that an electrode film layer is deposited on the substrate and has a nanowire array structure;
an included angle of 8-15 degrees is formed between the nanowire array structure and the substrate;
the electrode film layer is NiSe2A nanowire array of material;
NiSe2preparation of nanowire arrays of materialsThe method specifically comprises the following steps:
moving the substrate deposited with the Ni nanowire array into a selenization cavity;
3-4g of Se nano particles are put into the selenization cavity;
introduction of N2And H2The Se nanoparticles are brought into an inductively coupled plasma region;
at 14-16 deg.C/min-1The rate of raising the temperature from room temperature to 400 ℃ and maintaining it;
low-temperature plasma in inductive coupling plasma region promotes selenization of Ni material nanowire array to generate NiSe2A nanowire array of material;
the substrate is a stainless steel sheet, and a Ti layer with the thickness of 80-120nm is arranged between the substrate and the electrode film layer.
2. The preparation method of the lithium ion battery cathode according to claim 1, characterized by comprising the following steps:
pretreating a substrate;
NiSe formation on a substrate2And (3) preparing an electrode film layer of the nanowire array.
3. The method for preparing the negative electrode of the lithium ion battery according to claim 2, wherein the step of pretreating the substrate specifically comprises:
taking a stainless steel sheet as a substrate;
cleaning the stainless steel sheet, wherein the cleaning agent is at least one of acetone or ethanol;
and arranging a Ti layer with the thickness of 80-120nm on the stainless steel sheet by adopting magnetron sputtering.
4. The method of claim 2, wherein the forming NiSe on a substrate is performed by a negative electrode of a lithium ion battery2The method comprises the following steps of preparing an electrode film layer of the nanowire array:
depositing a Ni nanowire array on a substrate through electron beam evaporation;
selenizing Ni nanowire array into NiSe2Nanowire arrays of materials。
5. The method for preparing the negative electrode of the lithium ion battery according to claim 4, wherein the step of depositing the nanowire array of the Ni material on the substrate by electron beam evaporation specifically comprises:
the substrate is arranged obliquely, the Ni material evaporated by the electron beam is deposited on the substrate by adopting a grazing angle, and the deposition angle of the grazing angle is 8-15 degrees; the deposition rate of the Ni nanowire array is 0.25-0.35nm · s-1The deposition thickness on the substrate was 450-550 nm.
6. The method for preparing the negative electrode of the lithium ion battery according to claim 4, wherein N is introduced2And H2The step of bringing the Se nanoparticles into the inductively coupled plasma region comprises the following specific steps: n is a radical of2And H2The aeration ratio of (2: 3) and the flow rate of the mixed gas is 90-110 ml/min-1。
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