High-ionic-conductivity lithium battery diaphragm with self-closing function and preparation method of high-ionic-conductivity lithium battery diaphragm

A technology of ionic conductivity and lithium battery diaphragm, which is applied in the direction of battery pack parts, circuits, electrical components, etc., can solve the problems of low ion conductivity, no self-shutdown function, and low thermal stability of lithium battery diaphragms, etc., to achieve High thermal sensitivity and thermal dimensional stability, high safety and performance, and wide application range

Pending Publication Date: 2021-11-02

SUZHOU UNIV

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AI-Extracted Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to solve the problems in the prior art that the ionic conductivity of the lithium battery diaphragm is not high, there is no self-shutdown function or the self-shutdown temperature is high, that is, the thermal sensitivity is not high and the thermal ...

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Abstract

The invention relates to a high-ionic-conductivity lithium battery diaphragm with a self-closing function and a preparation method of the high-ionic-conductivity lithium battery diaphragm. The method comprises the following steps of: (1) performing vacuum filtration on a conductive inorganic substance solution containing a viscous substance on one side of a micro-nano fiber membrane, and then performing vacuum drying; and (2) sequentially carrying out vacuum suction filtration on the two sides of the membrane obtained in the step (1) by using a ceramic nanoparticle solution containing a viscous substance, and carrying out vacuum drying after each suction filtration to obtain a composite membrane. The prepared lithium battery diaphragm is a composite membrane consisting of a ceramic nano-particle layer, a conductive inorganic substance layer, a micro-nano fiber membrane and a ceramic nano-particle layer in sequence along the thickness direction, the relative positions of the ceramic nanoparticles, the conductive inorganic matter and the micro-nanofiber membrane (made of pure poly(butylene succinate)) in the composite membrane are fixed by the viscous substance, and the porosity of the composite membrane is 50-56%. The high-ionic-conductivity lithium battery diaphragm has relatively high thermal sensitivity and thermal dimensional stability, so that a lithium battery is relatively high in safety and use performance, and the high-ionic-conductivity lithium battery diaphragm has a great application prospect.

Application Domain

Cell component detailsNon-woven fabrics

Technology Topic

Electrically conductiveIonic conductivity +8

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Examples

Experimental program(8)
Comparison scheme(4)

Example Embodiment

[0054] Example 1

[0055] A method for preparing a high ion conductivity lithium battery diaphragm having a self-turning off function, and the specific steps are as follows:

[0056] (1) Preparation of raw materials;

[0057] Preparation of conductive inorganic solution containing viscous substances:

[0058] According to the mass volume ratio of 0.5 mg / ml, the conductive inorganic (MXENE) is dispersed in an aqueous solution, and then mixed with aqueous solution containing a viscous material (butadiene rubber binder) to obtain a viscous material. Conductive inorganic solution; in a conductive inorganic solution containing viscous substance, the concentration of the viscous material is 0.001% by weight.

[0059] Preparation of ceramic nanoparticle solution containing viscous substance:

[0060] According to the mass volume ratio of 0.5 mg / ml, ceramic nanoparticles (hydrophilic nano SiO) 2 The particles, the average particle diameter is 7 nm) is dispersed in an aqueous solution, and then mixed with a water solution containing a viscous material (butadepylmine binder) to obtain a ceramic nanoparticle solution containing a viscous substance; a ceramic containing a viscous material In the nanoparticle solution, the concentration of the viscous substance was 0.001% by weight.

[0061] Preparation of micro-nanofibriometry:

[0062]The fiber membrane obtained by the electrospinning process was first carried out in a vacuum drie with a temperature of 12 h, and the pressure was 6 MPa, and the time was 2 min, and the micro-nanofibrosis was obtained.

[0063] The parameters of the electrospinning process are: the mass fraction of the solute (丁 diol ester) in the spinning liquid is 22% by weight (solvent is a mixture of hexafluoropropyl alcohol and chloroform having a mass ratio of 1: 4), The spinning applied voltage was 15 kV; the solution propulsion was 1.5 ml / h; the ambient temperature was 20 ° C, the ambient humidity was 44%, and the injection needle to the receiving plate was 15 cm;

[0064] The average diameter of the nanofibers in the obtained micro-nanofibers was 152 nm, and the average diameter of microfibers was 2.1 μm.

[0065] (2) The conductive inorganic solution containing the viscous substance was vacuum filtration on one side of the micro-nanofiber film, and then dried in vacuo (60 ° C drying temperature of 60 ° C); when filtered, the conductive inorganic inorganic in which the adhesive substance was filtered. The volume of the solution is 6ml;

[0066] (3) The ceramic nanoparticle solution containing the viscous substance was vacuum filtration in both sides of the film obtained by the film (2), each filtered, and the drying temperature was 60 ° C, the time was 55min. The composite film is obtained; the volume of ceramic nanoparticle solution containing viscous substance is 5 mL each time it is filtered.

[0067] A high ion conductivity lithium battery diaphragm having self-turning off function, is made of ceramic nanoparticles (hydrophilic nano SiO) 2 Particles), conductive inorganic (MXENE) and micro-nanofibers (material are pteroidal polybut dikalate); the four layers are ceramics in turn along the thickness direction of the composite film Nanoparticle layer, conductive inorganic layer, micro-nano-fiber film and ceramic nanoparticle layer; the relative position between ceramic nanoparticles, conductive inorganic materials, and micro-nanofibers in the composite film (butadienyl) ) Fixed; the porosity of the composite film is 52.4%. On the composite film, the density of the conductive inorganic material is 0.08mg / cm 2 , The density of ceramic nanoparticles is 0.159mg / cm 2 The suction rate of the composite film on the Litfsi electrolyte is 439%; the ionic conductivity is 3.31 × 10 -3 S / CM, the composite film closed in the melting point (115 ° C) of the polybutadic acid butne glycol ester (PBS), invisible when the temperature of 300 ° C, such as figure 1 As shown, a microscopic plan view of the rear surface of the diaphragm (composite film) at 110 ° C and 120 ° C, respectively.

Example Embodiment

[0081] Example 2

[0082] A method for preparing a high ion conductivity lithium battery diaphragm having a self-turning off function, and the specific steps are as follows:

[0083] (1) Preparation of raw materials;

[0084] Preparation of conductive inorganic solution containing viscous substances:

[0085] According to the mass volume ratio of 0.5 mg / ml, the conductive inorganic (MXENE) is dispersed in an aqueous solution, and then mixed with aqueous solution containing a viscous material (butadiene rubber binder) to obtain a viscous material. Conductive inorganic solution; in a conductive inorganic solution containing viscous substance, the concentration of the viscous material is 0.001% by weight.

[0086] Preparation of ceramic nanoparticle solution containing viscous substance:

[0087] According to the mass volume ratio of 0.5 mg / ml, ceramic nanoparticles (hydrophilic nano SiO) 2 The particles, the average particle diameter is 10 nm) is dispersed in aqueous solution, and then mixed with aqueous solution containing a viscous substance (butadiene rubber binder) to obtain a ceramic nanoparticle solution containing a viscous substance; a ceramic containing a viscous material In the nanoparticle solution, the concentration of the viscous substance was 0.001% by weight.

[0088] Preparation of micro-nanofibriometry:

[0089] The fiber membrane obtained by the electrospinning process was first carried out in a vacuum drie with a temperature of 12 h, and the pressure was 6 MPa, and the time was 2 min, and the micro-nanofibrosis was obtained.

[0090] The parameters of the electrospinning process are: the mass fraction of the solute (丁 diol ester) in the spinning liquid is 22% by weight (solvent is a mixture of hexafluoropropyl alcohol and chloroform having a mass ratio of 1: 4), The spinning applied voltage is 15 kV; the solution propulsion is 1.5 ml / h; the ambient temperature is 20 ° C, the environmental humidity is 41%, the injection needle to the receiving plate is 15 cm;

[0091] The average diameter of the nanofibers in the obtained micro-nanofibers was 135 nm, and the average diameter of microfibers was 1.8 μm.

[0092] (2) Vacuum filtration of the conductive inorganic inorganic substance containing the viscous material was vacuum filtered on one side of the micro-nanofiber film, and then dried in vacuo (drying temperature of 60 ° C, time was 56min); when filtered, the conductive inorganic inorganic The volume of the substance is 8 mL;

[0093] (3) The ceramic nanoparticle solution containing the viscous substance was vacuum filtration in both sides of the film obtained by the step (2), each filtered, and the drying temperature was 60 ° C, the time was 56 min). The composite film is obtained; the volume of ceramic nanoparticle solution containing viscous substance is 5 mL each time it is filtered.

[0094] A high ion conductivity lithium battery diaphragm having self-turning off function, is made of ceramic nanoparticles (hydrophilic nano SiO) 2 Particles), conductive inorganic (MXENE) and micro-nanofibers (material are pteroidal polybut dikalate); the four layers are ceramics in turn along the thickness direction of the composite film Nanoparticle layer, conductive inorganic layer, micro-nano-fiber film and ceramic nanoparticle layer; the relative position between ceramic nanoparticles, conductive inorganic materials, and micro-nanofibers in the composite film (butadienyl) Fixed; the porosity of the composite film is 55.5%. On the composite film, the density of the conductive inorganic material is 0.159mg / cm 2 , The density of ceramic nanoparticles is 0.159mg / cm 2 The suction rate of the composite film on the Litfsi electrolyte is 567%; the ionic conductivity is 3.59 × 10 -3 S / cm; the composite film is closed at the melting point of the polybut dikalelic acid hyethylamate (PBS), which is invisible at the temperature of 300 ° C.

Example Embodiment

[0095] Example 3

[0096] A method for preparing a high ion conductivity lithium battery diaphragm having a self-turning off function, and the specific steps are as follows:

[0097] (1) Preparation of raw materials;

[0098] Preparation of conductive inorganic solution containing viscous substances:

[0099] According to the mass volume ratio of 0.5 mg / ml, the conductive inorganic (MXENE) is dispersed in an aqueous solution, and then mixed with aqueous solution containing a viscous material (butadiene rubber binder) to obtain a viscous material. Conductive inorganic solution; in a conductive inorganic solution containing viscous substance, the concentration of the viscous material is 0.001% by weight.

[0100] Preparation of ceramic nanoparticle solution containing viscous substance:

[0101] According to the mass volume ratio of 0.5 mg / ml, ceramic nanoparticles (hydrophilic nano SiO) 2 The particles, the average particle diameter is 20 nm) is dispersed in an aqueous solution, and then mixed with a water solution containing a viscous substance (butadepylmine binder) to obtain a ceramic nanoparticle solution containing a viscous material; a ceramic containing a viscous substance In the nanoparticle solution, the concentration of the viscous substance was 0.001% by weight.

[0102] Preparation of micro-nanofibriometry:

[0103] The fiber membrane obtained by the electrospinning process was first carried out in a vacuum drie with a temperature of 12 h, and the pressure was 6 MPa, and the time was 2 min, and the micro-nanofibrosis was obtained.

[0104]The parameters of the electrospinning process are: the mass fraction of the solute (丁 diol ester) in the spinning liquid is 22% by weight (solvent is a mixture of hexafluoropropyl alcohol and chloroform having a mass ratio of 1: 4), The spinning applied voltage was 15 kV; the solution propulsion was 1.5 ml / h; the ambient temperature was 20 ° C, the ambient humidity was 43%, and the injection needle to the receiving plate was 15 cm;

[0105] The average diameter of the nanofibers in the obtained micro-nanofibers was 146 nm, and the average diameter of microfibers was 1.9 μm.

[0106] (2) The conductive inorganic solution containing the viscous substance was vacuum filtered on one side of the micro-nanofiber film, and then dried in vacuo (60 ° C drying temperature of 60 ° C); when filtered, the conductive inorganic inorganic containing viscous substance The volume of the substance is 8 mL;

[0107] (3) EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc A composite film is obtained; the volume of ceramic nanoparticle solution containing viscous substance is 8 mL each time it is filtered.

[0108] A high ion conductivity lithium battery diaphragm having self-turning off function, is made of ceramic nanoparticles (hydrophilic nano SiO) 2 Particles), conductive inorganic (MXENE) and micro-nanofibers (material are pteroidal polybut dikalate); the four layers are ceramics in turn along the thickness direction of the composite film Nanoparticle layer, conductive inorganic layer, micro-nano-fiber film and ceramic nanoparticle layer; the relative position between ceramic nanoparticles, conductive inorganic materials, and micro-nanofibers in the composite film (butadienyl) ) Fixed; the porosity of the composite film is 54.3%. On the composite film, the density of the conductive inorganic material is 0.159mg / cm 2 The density of ceramic nanoparticles is 0.318 mg / cm 2 The suction rate of the composite film on the Litfsi electrolyte is 650%; the ionic conductivity is 3.86 × 10 -3 S / cm; the composite film is closed at the melting point of the polybut dikalelic acid hyethylamate (PBS), which is invisible at the temperature of 300 ° C.

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PUM

Property	Measurement	Unit
The average particle size	7.0 ~ 40.0	nm
The average diameter	100.0 ~ 200.0	nm
The average diameter	1.5 ~ 3.0	µm
tensile		MPa
Particle size		Pa
strength	10

Description & Claims & Application Information

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Classification and recommendation of technical efficacy words

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AI-Extracted Technical Summary

Problems solved by technology

Abstract

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Examples

Example Embodiment

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Example Embodiment

PUM

Description & Claims & Application Information

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