CN112864527B - Preparation method of Mxene/PVDF lithium-sulfur battery diaphragm - Google Patents
Preparation method of Mxene/PVDF lithium-sulfur battery diaphragm Download PDFInfo
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Abstract
The invention discloses a preparation method of a Mxene/PVDF lithium-sulfur battery diaphragm, which comprises the step of etching Ti by etching liquid 3 AlC 2 Adding 0.2-0.5 mol/L CTAB, placing at-60 to-48 ℃ for freezing, adding deionized water for standing, taking the lower layer liquid for freeze drying to obtain Mxene, adding into distilled water, adding ferric nitrate nonahydrate, dopamine and amino acid, stirring for dissolving, transferring into a polytetrafluoroethylene reaction kettle, heating to 150-180 ℃ for reaction for 2-4 h, cooling, filtering, placing in a tubular furnace, firing at 200-300 ℃ for 2-3 h in the nitrogen atmosphere, and cooling for later use; and (3) adding the product obtained in the step (S3) into N, N-dimethylformamide, carrying out ultrasonic stirring and uniform dispersion, then adding polyvinylidene fluoride, heating to 50-60 ℃, carrying out magnetic stirring for 3-6 h, pouring the mixture into a grooved glass plate, carrying out blade coating to keep the thickness of the film at 1-3 mm, and finally carrying out vacuum drying in an oven at 70-80 ℃ for 3-5 h to obtain the diaphragm.
Description
Technical Field
The invention belongs to the technical field of lithium-sulfur batteries, and particularly relates to a preparation method of a Mxene/PVDF lithium-sulfur battery diaphragm.
Background
The lithium-sulfur battery is a lithium-sulfur secondary battery which takes metal lithium as a negative electrode and elemental sulfur as a positive electrode material, and the theoretical specific capacity of the material reaches 1672 mAh.g -1 The theoretical specific energy of the battery reaches 2600Wh/kg, and the actual energy density of the current lithium-sulfur battery reaches 390Wh/kg and is much higher than that of other LiFeO batteries 4 、LiMn 2 O 4 And the like, commercially available electrode materials.
The separator is an important component of a lithium-sulfur battery and serves to separate the positive and negative electrodes to prevent internal shorting of the battery while facilitating the transport of free lithium ions between the two electrodes. The lithium-sulfur battery separator is generally a non-polar film such as polypropylene/polyethylene (PP/PE). However, during discharge of the lithium-sulfur battery, elemental sulfur is reduced to S -2 In the process of (2), there are a plurality of intermediate states formed, among which Li 2 Sn (n is more than or equal to 4 and less than or equal to 8) is easily dissolved in organic electrolyte, shuttles from the sulfur anode to the lithium cathode through the diaphragm, forms an insulating layer on the lithium cathode, reduces the contact between the lithium cathode and the diaphragm, and prevents a transmission channel of lithium ions, thereby causing the problems of poor cyclicity, low coulombic efficiency, high self-discharge rate and the like of the lithium-sulfur battery.
Disclosure of Invention
For Li in the above lithium-sulfur battery 2 Sn (n is more than or equal to 4 and less than or equal to 8) is dissolved in electrolyte, and the diaphragm can not prevent the Sn from shuttling from a sulfur positive electrode to a lithium negative electrode, so that the problems of poor cyclicity, low coulombic efficiency, high self-discharge rate and the like of a lithium-sulfur battery are caused, and the invention aims to provide a preparation method of the Mxene/PVDF lithium-sulfur battery diaphragm, which comprises the following steps:
s1: adding LiF into hydrochloric acid solution containing chlorine salt, stirring uniformly to obtain etching solution, and adding Ti 3 AlC 2 The precursor is crushed and sieved by a sieve of 100 to 150 meshes, then is added into the etching solution, and then reacts for 3 to 6 hours at the temperature of 61 to 64 ℃ under the condition of the rotating speed of 500 to 550r/min for later use.
S2: and (2) adding 0.2-0.5 mol/L CTAB into the step S1, continuously stirring for 30-60 min, then placing at-60-48 ℃ for rapid freezing for 0.5-2 h, then taking out and placing at room temperature, carrying out ultrasonic treatment for 20-30 min when the internal temperature is raised to 1-3 ℃, carrying out freezing-ultrasonic circulation operation for 4-6 times, then adding deionized water, starting to stand for layering, taking out the liquid at the lower layer for freeze drying, and obtaining the Mxene material for later use.
S3: adding the Mxene material product obtained in the step S2 into distilled water, performing ultrasonic stirring to fully disperse the Mxene material product, then adding ferric nitrate nonahydrate, dopamine and amino acid, stirring to dissolve the mixture, transferring the mixture into a polytetrafluoroethylene reaction kettle, heating the mixture to 150-180 ℃, reacting for 2-4 h, cooling, filtering, placing the mixture into a tubular furnace, baking the mixture for 2-3 h at 200-300 ℃ in a nitrogen atmosphere, and cooling for later use.
S4: and (3) adding the product obtained in the step (S3) into N, N-dimethylformamide, carrying out ultrasonic stirring and uniform dispersion, then adding polyvinylidene fluoride, heating to 50-60 ℃, carrying out magnetic stirring for 3-6 h, pouring the mixture into a grooved glass plate, carrying out blade coating to keep the thickness of the film at 1-3 mm, and finally carrying out vacuum drying in an oven at 70-80 ℃ for 3-5 h to obtain the diaphragm.
Preferably, the above-mentioned LiF, hydrochloric acid solution and Ti 3 AlC 2 The mass-to-volume ratio of (1.88-2.69) g, (20-40) mL, (1.69-2.85) g.
Preferably, the mass-to-volume ratio of the Mxene material, ferric nitrate nonahydrate, dopamine, amino acid and distilled water is (3-5.5), (1.2-1.8), (0.96-1.28), (0.66-0.92) and (10-25) mL.
Preferably, the mass-to-volume ratio of the product obtained in the step S3 to the polyvinylidene fluoride to the N, N-dimethylformamide is (2.5-3.6) g, (7-15) g, (30-50) mL.
Compared with the prior art, the invention has the following beneficial effects:
in the invention, ti is etched step by step 3 AlC 2 The method comprises the steps of preparing the Mxene material, modifying the Mxene material by using ferric nitrate nonahydrate, dopamine and amino acid, calcining the Mxene material to ensure that Fe ions and nitrogen ions are rich between layers of the Mxene material, and preparing the diaphragm by compounding the Mxene material and polyvinylidene fluoride in a blade coating and tape casting mode, wherein polysulfide Li is compounded inside the diaphragm by compounding the Mxene material 2 S n (4. Ltoreq. N.ltoreq.8) through the "channels" of the membrane, and iron ions and nitrogen ions therein form Fe-N bonds to the polysulphide Li 2 S n Chemical anchoring effect is generated, and the shuttle of the lithium-sulfur battery can be effectively blocked from passing through the diaphragm, so that the cycle stability of the lithium-sulfur battery is improved.
Detailed Description
The following embodiments of the present invention are described in detail, and the embodiments are implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, it should be noted that, for those skilled in the art, a plurality of modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Example 1
A preparation method of a Mxene/PVDF lithium-sulfur battery diaphragm specifically comprises the following steps:
s1: adding LiF into hydrochloric acid solution containing chlorine salt, stirring uniformly to obtain etching solution, and adding Ti 3 AlC 2 The precursor is crushed and sieved by a 100-mesh sieve, and then the mixture is addedAdding into etching solution, and reacting at 61 deg.C and 500r/min for 3 hr.
S2: adding 0.2mol/L CTAB into the step S1, continuously stirring for 30min, then placing at-60 ℃ for fast freezing for 0.5h, then taking out and placing at room temperature, carrying out ultrasonic treatment for 20min when the internal temperature is raised to 1 ℃, carrying out freezing-ultrasonic circulation operation for 4 times, then adding deionized water, starting standing for layering, taking out the liquid at the lower layer, and carrying out freeze drying to obtain a Mxene material for later use; wherein LiF, hydrochloric acid solution and Ti 3 AlC 2 Mass to volume ratio of (1.88g).
S3: adding the Mxene material product obtained in the step S2 into distilled water, performing ultrasonic stirring to fully disperse the Mxene material product, then adding ferric nitrate nonahydrate, dopamine and amino acid, stirring to dissolve, transferring to a polytetrafluoroethylene reaction kettle, heating to 150 ℃ to react for 2 hours, cooling, filtering, then placing in a tubular furnace, baking at 200 ℃ for 2 hours in a nitrogen atmosphere, and cooling for later use; wherein the mass-volume ratio of the Mxene material, ferric nitrate nonahydrate, dopamine, amino acid and distilled water is 3 g.
S4: adding the product obtained in the step S3 into N, N-dimethylformamide, performing ultrasonic stirring to disperse uniformly, then adding polyvinylidene fluoride, heating to 50 ℃, performing magnetic stirring for 3 hours, pouring the mixture into a grooved glass plate, performing blade coating to keep the thickness of the film at 1mm, and finally performing vacuum drying in an oven at 70 ℃ for 3 hours to obtain the diaphragm; wherein the mass-to-volume ratio of the product obtained in the step S3 to the polyvinylidene fluoride to the N, N-dimethylformamide is 2.5g.
Example 2
A preparation method of a Mxene/PVDF lithium-sulfur battery diaphragm specifically comprises the following steps:
s1: adding LiF into hydrochloric acid solution containing chlorine salt, uniformly stirring to obtain etching solution, and adding Ti 3 AlC 2 The precursor is crushed, sieved by a 150-mesh sieve, added into etching liquid and then reacted for 6 hours at the temperature of 64 ℃ at the rotating speed of 550r/min for later use.
S2: adding 0.5mol/L CT to the step S1AB is continuously stirred for 60min, then placed at minus 48 ℃ for quick freezing for 2h, then taken out and placed at room temperature, ultrasonic treatment is carried out for 30min when the internal temperature is raised to 3 ℃, the freezing-ultrasonic circulation operation is carried out for 6 times, then deionized water is added, standing is started for layering, the liquid at the lower layer is taken out for freeze drying, and the Mxene material is obtained for standby; wherein LiF, hydrochloric acid solution and Ti 3 AlC 2 The mass-to-volume ratio of (2.69g).
S3: adding the Mxene material product obtained in the step S2 into distilled water, performing ultrasonic stirring to fully disperse the Mxene material product, then adding ferric nitrate nonahydrate, dopamine and amino acid, stirring to dissolve, transferring to a polytetrafluoroethylene reaction kettle, heating to 180 ℃ to react for 4 hours, cooling, filtering, then placing in a tubular furnace, baking at 300 ℃ for 3 hours in a nitrogen atmosphere, and cooling for later use; wherein the mass-volume ratio of the Mxene material, ferric nitrate nonahydrate, dopamine, amino acid and distilled water is 5.5g.
S4: adding the product obtained in the step S3 into N, N-dimethylformamide, performing ultrasonic stirring to disperse uniformly, then adding polyvinylidene fluoride, heating to 60 ℃, performing magnetic stirring for 6 hours, pouring the mixture into a grooved glass plate, performing blade coating to keep the thickness of the film at 3mm, and finally performing vacuum drying in an oven at 80 ℃ for 5 hours to obtain the diaphragm; wherein the mass-to-volume ratio of the product obtained in the step S3, polyvinylidene fluoride and N, N-dimethylformamide is 3.6 g.
Example 3
A preparation method of a Mxene/PVDF lithium-sulfur battery diaphragm specifically comprises the following steps:
s1: adding LiF into hydrochloric acid solution containing chlorine salt, stirring uniformly to obtain etching solution, and adding Ti 3 AlC 2 And crushing the precursor, sieving the crushed precursor with a 120-mesh sieve, adding the crushed precursor into etching liquid, and reacting for 4 hours at the temperature of 62 ℃ at the rotating speed of 520r/min for later use.
S2: adding 0.3mol/L CTAB into the step S1, continuously stirring for 40min, rapidly freezing at-50 deg.C for 1h, taking out, standing at room temperature, and ultrasonic treating for 25min when the internal temperature is raised to 2 deg.C, soPerforming freezing-ultrasonic circulation operation for 5 times, then adding deionized water, starting standing for layering, taking the lower layer liquid for freeze drying to obtain the Mxene material for later use; wherein LiF, hydrochloric acid solution and Ti 3 AlC 2 The mass-to-volume ratio of (1.99g).
S3: adding the Mxene material product obtained in the step S2 into distilled water, performing ultrasonic stirring to fully disperse the Mxene material product, then adding ferric nitrate nonahydrate, dopamine and amino acid, stirring to dissolve, transferring to a polytetrafluoroethylene reaction kettle, heating to 160 ℃, reacting for 3 hours, cooling, filtering, then placing in a tubular furnace, baking for 2.5 hours at 250 ℃ in a nitrogen atmosphere, and cooling for later use; wherein the mass-volume ratio of the Mxene material, the ferric nitrate nonahydrate, the dopamine, the amino acid and the distilled water is 4 g.
S4: adding the product obtained in the step S3 into N, N-dimethylformamide, performing ultrasonic stirring to disperse uniformly, then adding polyvinylidene fluoride, heating to 55 ℃, performing magnetic stirring for 4 hours, pouring the polyvinylidene fluoride into a grooved glass plate, performing blade coating to keep the thickness of the film at 2mm, and finally performing vacuum drying in an oven at 75 ℃ for 4 hours to obtain the diaphragm; wherein the mass-volume ratio of the product obtained in the step S3 to the polyvinylidene fluoride to the N, N-dimethylformamide is 2.9g to 10g.
Example 4
A preparation method of an Mxene/PVDF lithium-sulfur battery diaphragm specifically comprises the following steps:
s1: adding LiF into hydrochloric acid solution containing chlorine salt, stirring uniformly to obtain etching solution, and adding Ti 3 AlC 2 And crushing the precursor, sieving the crushed precursor by a 140-mesh sieve, adding the crushed precursor into etching liquid, and reacting for 5 hours at the temperature of 63 ℃ at the rotating speed of 540r/min for later use.
S2: adding 0.4mol/L CTAB into the step S1, continuously stirring for 50min, then placing the mixture under the condition of-55 ℃ for quick freezing for 1.5h, then taking out the mixture and placing the mixture under the condition of room temperature, carrying out ultrasonic treatment for 30min when the internal temperature is raised to 3 ℃, carrying out freezing-ultrasonic circulation operation for 6 times, then adding deionized water, starting standing for layering, taking out the liquid at the lower layer for freeze drying, and obtaining the Mxene material for later use; wherein LiF, saltAcid solution and Ti 3 AlC 2 The mass-to-volume ratio of (2.44g).
S3: adding the Mxene material product obtained in the step S2 into distilled water, performing ultrasonic stirring to fully disperse the Mxene material product, then adding ferric nitrate nonahydrate, dopamine and amino acid, stirring to dissolve, transferring to a polytetrafluoroethylene reaction kettle, heating to 170 ℃, reacting for 4 hours, cooling, filtering, then placing in a tubular furnace, baking for 3 hours at 280 ℃ in a nitrogen atmosphere, and cooling for later use; wherein the mass-volume ratio of the Mxene material, ferric nitrate nonahydrate, dopamine, amino acid and distilled water is 5.6 g.
S4: adding the product obtained in the step S3 into N, N-dimethylformamide, performing ultrasonic stirring to disperse uniformly, then adding polyvinylidene fluoride, heating to 55 ℃, performing magnetic stirring for 5 hours, pouring the polyvinylidene fluoride into a grooved glass plate, performing blade coating to keep the thickness of the film at 3mm, and finally performing vacuum drying in an oven at 78 ℃ for 5 hours to obtain the diaphragm; wherein the mass-volume ratio of the product obtained in the step S3, polyvinylidene fluoride and N, N-dimethylformamide is 3.4g.
Comparative example 1
Commercial Nafion battery separator.
Examples of the experiments
Performance test, namely assembling the lithium-sulfur battery diaphragm prepared in the embodiment 1-4 into a battery, wherein the positive electrode is sublimed sulfur, super P and a binder, and the mixture is ground and then added into N-methyl pyrrolidone according to the mass ratio of 6; the negative electrode is a lithium metal sheet, the electrolyte is a mixed solution of lithium salt and 1,3-dioxolane/glycol dimethyl ether, wherein the lithium salt is 1M LiTFSI, the mixed solution contains 1wt.% of lithium nitrate as an additive, the lithium-sulfur battery is tested by adopting a Wuhan blue electric test system, the charge-discharge voltage range is 1.7-2.8V, the current density is 0.2C, the test results are shown in Table 1,
table 1. Test results:
it can be seen from table 1 that the first specific discharge capacity of the lithium-sulfur battery assembled from the separator materials prepared in examples 1 to 4 of the present invention is 969.4mAh/g, the specific discharge capacity of the lithium-sulfur battery still remains 919.3mAh/g after 100 cycles of cycling, and the specific discharge capacity of the lithium-sulfur battery assembled from the separator materials of 200 cycles of cycling is 851.1mAh/g, which is superior to the separator material of comparative example 1 in terms of specific discharge capacity and cycling stability.
Claims (1)
1. A preparation method of a Mxene/PVDF lithium-sulfur battery diaphragm is characterized by comprising the following steps:
s1: adding LiF into hydrochloric acid solution containing chlorine salt, stirring uniformly to obtain etching solution, and adding Ti 3 AlC 2 Crushing the precursor, sieving the crushed precursor with a sieve of 100 to 150 meshes, adding the crushed precursor into etching solution, and reacting the obtained product for 3 to 6 hours at the temperature of 61 to 64 ℃ at the rotating speed of 500 to 550r/min for later use;
s2: adding 0.2-0.5 mol/L CTAB into the step S1, continuously stirring for 30-60 min, then placing at-60-48 ℃ for rapid freezing for 0.5-2 h, then taking out and placing at room temperature, carrying out ultrasonic treatment for 20-30 min when the internal temperature is raised to 1-3 ℃, carrying out freezing-ultrasonic circulation operation for 4-6 times, then adding deionized water, starting to stand for layering, taking out the liquid at the lower layer for freeze drying, and obtaining the Mxene material for later use;
s3: adding the Mxene material product obtained in the step S2 into distilled water, performing ultrasonic stirring to fully disperse the Mxene material product, then adding ferric nitrate nonahydrate, dopamine and amino acid, stirring to dissolve the mixture, transferring the mixture into a polytetrafluoroethylene reaction kettle, heating the mixture to 150-180 ℃, reacting for 2-4 h, cooling, filtering, placing the mixture into a tubular furnace, baking the mixture for 2-3 h at 200-300 ℃ in a nitrogen atmosphere, and cooling for later use;
s4: adding the product obtained in the step S3 into N, N-dimethylformamide, performing ultrasonic stirring to disperse uniformly, then adding polyvinylidene fluoride, heating to 50-60 ℃, performing magnetic stirring for 3-6 h, pouring the mixture into a grooved glass plate, performing blade coating to keep the thickness of the film at 1-3 mm, and finally performing vacuum drying in an oven at 70-80 ℃ for 3-5 h to obtain the diaphragm;
wherein, the LiF, the hydrochloric acid solution and the Ti 3 AlC 2 The mass volume ratio of (1.88-2.69) g, (20-40) mL, (1.69-2.85) g; the mass volume ratio of the Mxene material, ferric nitrate nonahydrate, dopamine, amino acid and distilled water is (3-5.5) g, (1.2-1.8) g, (0.96-1.28) g, (0.66-0.92) g, (10-25) mL; the mass-volume ratio of the product obtained in the step S3, polyvinylidene fluoride and N, N-dimethylformamide is (2.5-3.6), (7-15), (30-50) mL.
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