CN107887553B - A kind of multi-functional lithium-sulfur cell diaphragm and preparation method thereof - Google Patents
A kind of multi-functional lithium-sulfur cell diaphragm and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
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- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
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- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
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Abstract
A kind of multi-functional lithium-sulfur cell diaphragm and preparation method thereof, belongs to technical field of energy material.The lithium-sulfur cell diaphragm is using the compound obtained composite material of graphene oxide of sodium lignin sulfonate and reduction as coating, solves the technical issues of simple graphite ene coatings have a single function, obtained composite material is coated on lithium-sulfur cell diaphragm, coating is under ionization, the region of electrification can be formed in the electrolytic solution, so that the side of diaphragm is negatively charged, according to the principle of homopolar-repulsion, electronegative diaphragm can obviously repel same electronegative polysulfide, effectively reduce a possibility that polysulfide is across diaphragm, reduce shuttle effect, improve battery performance.
Description
Technical field
The invention belongs to technical field of energy material, and in particular to a kind of diaphragm and its system for high-performance lithium-sulfur cell
Preparation Method.
Background technique
New-energy automobile is to alleviate China's Pressure on Energy, reply climate change, promote car industry and transportation that can hold
The important measure of supervention exhibition.In recent years, China's oil consumption external dependence degree reaches 60.6%, energy security, especially oil gas
The safety of resource, it has also become an important factor for restricting economic development, greatly developing renewable resource is to realize auto industry transition
The only way which must be passed, and maintenance Chinese energy safety strategic choice.However, renewable resource has uncontrollability and unstable
Property, need to match reliable energy-storage battery.Lithium ion battery is as currently used energy storage device, by itself storage volume
Limitation, be still difficult to meet requirement of the following power battery to energy-storage battery height ratio capacity and high-energy density.Therefore, research is opened
Sending out lithium ion battery high performance is particularly important.
Lithium-sulfur cell (Li-S) is one kind of lithium ion battery, and theoretical specific capacity is up to 1675mAh/g, theoretical specific energy
Reach 2600Wh/kg, be 5-10 times of traditional ferric phosphate lithium cell, and sulphur itself have many advantages, such as it is pollution-free, inexpensive so that
Li-S battery becomes international research hot spot, and is considered as the ideal chose (Nature of Future New Energy Source Vehicular dynamic battery
Mater.8,500,2009).However, the dissolution of polysulfide and its by the effect that shuttles caused by diaphragm in lithium-sulfur cell, right
The performance of lithium-sulfur cell and safety all bring serious challenge, so that commercialization lithium-sulfur cell develops slowly.
Shuttle effect in lithium-sulfur cell in order to prevent, is usually arranged diaphragm in the battery, which is being located at battery just
Between cathode, during charge and discharge cycles, playing prevents positive and negative anodes from contacting and short circuit occurs while allowing lithium ion free
The effect of migration.The superiority and inferiority of important component of the diaphragm as lithium-sulfur cell, performance has important shadow to the performance of battery
It rings.Currently, common lithium-sulfur cell diaphragm is traditional polypropylene diaphragm (PP), such diaphragm is although at low cost, but in battery
The shuttle that can not stop polysulfide in cyclic process be easy to cause serious capacitance loss, and lithium ion deposition is uneven, holds
Apparent Li dendrite easily is generated in cathode, meanwhile, heat resistance is very poor, easily rupturable generation battery short circuit, causes safety problem.
It is the hot spot of current lithium-sulfur cell diaphragm research, the report such as Huang by the performance that modified diaphragm improves lithium-sulfur cell
A kind of simple graphite ene coatings in road can be pressed down to a certain extent by coating one layer of graphene on common PP diaphragm
Shuttle effect processed improves circulating ring number and the load of battery；But since the functionalization degree of graphene is single, physics is only leaned on
Structure can not completely inhibit the shuttle of polysulfide, simultaneously as the thermal conductivity of single coating is poor, diaphragm is locally easy to produce
Heat is concentrated, and is formed " hot spot ", there are still certain hidden danger for lithium-sulfur cell security performance.It therefore, will by chemically synthesized method
For chemical group with certain function in conjunction with graphene, obtaining multi-functional graphite ene coatings is current diaphragm coating development
Inexorable trend.
Summary of the invention
In view of the defects in the background art, the present invention proposes a kind of composite materials for lithium-sulfur cell diaphragm coating
Preparation method, by sodium lignin sulfonate (SL) and reduction graphene oxide (rGO) carry out it is compound, solve simple graphene
The technical issues of coating has a single function, obtained composite material are coated on lithium-sulfur cell diaphragm, can be effectively suppressed in battery
Shuttle effect improves the performance of battery.
Technical scheme is as follows:
A kind of preparation method of the composite material for lithium-sulfur cell diaphragm coating, comprising the following steps:
Step 1: dispersing graphene oxide (GO) in dimethylformamide (DMF), ultrasound, obtaining uniform concentration is
The graphene dispersing solution of 1~2mg/mL；
Step 2: hexamethylene diisocyanate (HDI) being added in dimethylformamide (DMF), is uniformly mixed, obtains
Mixed liquor heat 5min in 140~150 DEG C of oil baths；Wherein, in the mixed liquor hexamethylene diisocyanate concentration
For 3~5 μ L/mL；
Step 3: the graphene dispersing solution that step 1 obtains being slowly added to step 2 with the rate of 10~20mL/min and is handled
In mixed liquor afterwards, after being uniformly mixed, 30min is heated in 140~150 DEG C of oil baths, obtains mixed liquor A；
Step 4: sodium lignin sulfonate being added in dimethylformamide (DMF), being then heated to 80 DEG C makes sulfomethylated lignin
Sour sodium is completely dissolved, and the lignin sulfonic acid sodium solution that concentration is 0.7~1mg/mL can be obtained；
Step 5: the lignin sulfonic acid sodium solution that step 4 obtains is slowly added to step 3 with the rate of 10~20mL/min
In obtained mixed liquor A, obtained mixed liquid B under inert gas protection, keep 140~150 DEG C of thermotonuses 60~
120min；Wherein, the concentration of the graphene oxide restored in the mixed liquid B is 0.25~0.5mg/mL, sodium lignin sulfonate
Concentration be 0.5~0.7mg/mL；
Step 6: after the reaction was completed, to reaction solution cooled to room temperature, after taking out and using deionized water centrifuge washing,
By freeze-drying 12~for 24 hours, the composite material of the graphene oxide@sodium lignin sulfonate restored is as described to be used for
The composite material of lithium-sulfur cell diaphragm coating.
Further, inert gas described in step 5 is nitrogen, argon gas etc..
A kind of preparation method of the lithium-sulfur cell diaphragm obtained based on above-mentioned composite material, comprising the following steps:
Step 1: by the graphene oxide@sodium lignin sulfonate composite material of reduction obtained by the above method and conductive addition
After agent (carbon black, Ketjen black etc.), binder (Kynoar etc.) are according to the ratio mixing that mass ratio is 7:2:1, N- first is added
In base pyrrolidones (NMP), the concentration of graphene oxide@sodium lignin sulfonate (the rGO@SL) composite material restored is prepared
For the slurry of 30~100mg/mL, be ground to slurry in aterrimus it is thick after, continuously add N-Methyl pyrrolidone (NMP) into
Row dilution, makes the concentration of graphene oxide@sodium lignin sulfonate composite material of reduction be reduced to 5~20mg/mL, then grinds and make
It is completely dispersed；
Step 2: the slurry obtained after step 1 processing being formed on PP diaphragm using the method filtered, as diaphragm
The lithium-sulfur cell diaphragm can be obtained in coating.
Further, in the lithium-sulfur cell diaphragm that step 2 obtains, the coating with a thickness of 20~50 μm.
The invention has the benefit that
1, compared to single graphite ene coatings, the coating that rGO SL provided by the invention is formed is under ionization, meeting
The region of electrification is formed in the electrolytic solution, so that the side of diaphragm is negatively charged, according to the principle of homopolar-repulsion, electronegative diaphragm
Same electronegative polysulfide can obviously be repelled, a possibility that polysulfide is across diaphragm is effectively reduced, reduce shuttle
Effect improves battery performance.
2, the present invention combines dendritic sodium lignin sulfonate by chemical bond with graphene, has further expanded graphite
The space structure of alkene；Obtained rGO@SL composite material will form 3D porous structure after being coated on diaphragm, increase sulphur and conduction
The attaching space of additive effectively improves the electric conductivity and capacity of battery.
3, the coating that the rGO@SL composite material that the present invention obtains is formed has good thermal conductivity, under high temperature environment work
When making, the diaphragm for coating the coating is not easy to produce hot spot, effectively increases the heat resistance of diaphragm, optimizes the safety of battery
Performance.
Detailed description of the invention
Fig. 1 is graphene oxide (GO) and the graphene oxide@sodium lignin sulfonate composite material (rGO@SL) of reduction
XPS figure；
The SEM that Fig. 2 is GO schemes；
Fig. 3 is that the SEM of rGO@SL composite material schemes；
Fig. 4 is that the rGO@SL composite material (b) that conventional graphite alkene (a) is obtained with the embodiment of the present invention is soaked in Li-S electrolysis
The zeta potential diagram tested in liquid；
Fig. 5 be not coated piece of PP diaphragm (PP), in background technique the PP diaphragm (GO/PP) with graphite ene coatings and this
The chemical property of the lithium-sulfur cell of PP diaphragm (rGO@SL/PP) production of the invention based on rGO@SL coating；It (a) is forthright again
Can, (b-c) is the cycle performance of different multiplying.
Specific embodiment
With reference to the accompanying drawings and examples, technical solution of the present invention is described in detail.
A kind of preparation method of the composite material for lithium-sulfur cell diaphragm coating, comprising the following steps:
Step 1: dispersing 100~200mg graphene oxide (GO) in 100mL dimethylformamide (DMF), ultrasound 10
~30min obtains the graphene dispersing solution that uniform concentration is 1~2mg/mL；
Step 2: 100mL dimethylformamide (DMF) is added in 300~500 μ L hexamethylene diisocyanates (HDI)
In, it is uniformly mixed, condensation heating keeps the temperature 5min to 140~150 DEG C to obtained mixed liquor in oil bath；Wherein, the mixed liquor
The concentration of middle hexamethylene diisocyanate is 3~5 μ L/mL；In the process, graphene oxide (GO) is reduced to reduction
Graphene oxide (rGO)；
Step 3: the graphene dispersing solution that step 1 obtains being slowly added to step 2 with the rate of 10~20mL/min and is handled
In mixed liquor afterwards, after being uniformly mixed, 30min is heated in 140~150 DEG C of oil baths, obtains mixed liquor A；
Step 4: 200~300mg sodium lignin sulfonate being added in 300mL dimethylformamide (DMF), is then heated to
80 DEG C are completely dissolved sodium lignin sulfonate, and the lignin sulfonic acid sodium solution that concentration is 0.7~1mg/mL can be obtained；
Step 5: the lignin sulfonic acid sodium solution that step 4 obtains is slowly added to step 3 with the rate of 10~20mL/min
In obtained mixed liquor A, obtained mixed liquid B under protection of argon gas, keeps 140~150 DEG C of 60~120min of thermotonus；Its
In, the concentration of the graphene oxide restored in the mixed liquid B is 0.25~0.5mg/mL, and the concentration of sodium lignin sulfonate is
0.5~0.7mg/mL；
Step 6: after the reaction was completed, to reaction solution cooled to room temperature, take out, using deionized water as detergent,
After continuous centrifugal washing three times, by freeze-drying 12~for 24 hours, rGO@SL composite material is obtained, it is as described for lithium sulphur electricity
The composite material of pond diaphragm coating.
A kind of preparation method of the lithium-sulfur cell diaphragm obtained based on above-mentioned composite material, comprising the following steps:
Step 1: by rGO@SL composite material obtained by the above method and conductive additive (carbon black, Ketjen black etc.), bonding
After agent (Kynoar etc.) is according to the ratio mixing that mass ratio is 7:2:1, it is added in 500 μ lN- methyl pyrrolidones (NMP),
It prepares and obtains the slurry that the concentration of rGO@SL composite material is 30~100mg/mL, grind 30 minutes, it is viscous in aterrimus to slurry
After thick shape, continuously add N-Methyl pyrrolidone (NMP) and be diluted, make the concentration of rGO@SL composite material be reduced to 5~
20mg/mL, then grinding 30 minutes is completely dispersed it；
Step 2: conventional PP diaphragm being cut to the small cube of 5cm × 5cm, common pumping is placed in after infiltrating using NMP
Filter flask mouth, then by obtained slurry after step 1 processing by Suction filtration device suction filtration to PP diaphragm, as the coating of diaphragm,
The lithium-sulfur cell diaphragm can be obtained.
Further, in the lithium-sulfur cell diaphragm that step 2 obtains, the coating with a thickness of 20~50 μm.
Embodiment
A kind of preparation method of lithium-sulfur cell diaphragm, specifically includes the following steps:
Step 1 after being cleaned by ultrasonic 30g water removal molecular sieve 5 times using alcohol, is toasted for 24 hours, with complete in 100 DEG C of baking ovens
Moisture in full removal molecular sieve；
Step 2 goes step 1 molecular sieve after moisture removal to be put into 800mL dimethylformamide (DMF), removes in DMF
Moisture, the DMF after being removed water；When taking water removal DMF, supernatant liquid is drawn using liquid-transfering gun, the DMF in subsequent step
Solution is water removal DMF；
100mg graphene oxide (GO) is slowly added in 100mL dimethylformamide (DMF) by step 3, ultrasound
30min obtains uniform graphene oxide dispersion；
Step 4 350 μ L hexamethylene diisocyanates (HDI) is added in 100mL dimethylformamide (DMF), mixing
Uniformly, condensation heating keeps the temperature 5min to 140 DEG C to the mixed liquor obtained in oil bath；
Step 5, the temperature for keeping mixed liquor are 140 DEG C, and the graphene dispersing solution that step 3 is obtained is with the speed of 20mL/min
Rate is slowly added to, and constant temperature 30min obtains mixed liquor A；In the process, graphene oxide (GO) is reduced to the oxidation of reduction
Graphene (rGO)；
Step 6 takes 300mg sodium lignin sulfonate powder in beaker, dries for 24 hours, completely in 80 DEG C of vacuum ovens
Remove contained humidity in powder；Then, the sodium lignin sulfonate after drying is added in 300mL dimethylformamide (DMF), so
After be heated to 80 DEG C and be completely dissolved sodium lignin sulfonate, the lignin sulfonic acid sodium solution that concentration is 1mg/mL can be obtained；
Above-mentioned lignin sulfonic acid sodium solution is slowly added to the mixed liquor that step 5 obtains with the rate of 10mL/min by step 7
In A, obtained mixed liquid B under protection of argon gas, keeps 140 DEG C of thermotonus 120min；
Step 8, after the reaction was completed is taken out to reaction solution cooled to room temperature, using deionized water as detergent,
After continuous centrifugal washing three times, extra sodium lignin sulfonate is removed, for 24 hours finally by freeze-drying, it is compound to obtain rGO@SL
Material；
Step 9 mixes 21mg rGO@SL composite material, 6mg carbon black, 3mg Kynoar according to the ratio of 7:2:1
After be added 500 μ l N-Methyl pyrrolidone (NMP) solution, prepare and obtain the slurry that the concentration of rGO@SL composite material is 60mg/mL
Material is ground 30 minutes, and after slurry is thick in aterrimus, N-Methyl pyrrolidone (NMP) progress for continuously adding 2.5mL is dilute
It releases, so that the concentration of rGO@SL composite material is reduced to 10mg/mL, then grinding 30 minutes is completely dispersed it；
Step 10, the small cube that conventional PP diaphragm is cut to 5cm × 5cm, it is general using being placed in after 1mL NMP infiltration
It is logical to filter bottleneck, above-mentioned slurry is then drawn using liquid-transfering gun and is added dropwise on PP diaphragm, 1.5mL slurry is inhaled every time, passes through suction filtration
Device is filtered onto PP diaphragm, and as the coating of diaphragm, coating layer thickness is 20 μm, and the lithium-sulfur cell diaphragm can be obtained.
Fig. 1 is graphene (GO) and the XPS of rGO@SL composite material schemes；As shown in Figure 1, the rGO@SL that the present invention obtains is multiple
Condensation material (rGO@SL) has apparent N, and S chemical bond shows that the graphene oxide of sodium lignin sulfonate and reduction has passed through chemistry
Bond is closed；Meanwhile O key obviously dies down, and shows that graphene oxide has been reduced to the graphene oxide of reduction.
Fig. 3 is the SEM figure for the rGO@SL composite material that the present invention obtains；From the figure 3, it may be seen that the rGO@SL that the present invention obtains is multiple
Condensation material surface is a large amount of dendritic structure, which not only can effectively prevent the shuttle of polysulfide, moreover it is possible to mention for electronics
For a large amount of transmission channel, and then improve the stability and capacity of battery.
Fig. 4 is that the rGO@SL composite material (b) that conventional graphite alkene (a) is obtained with the embodiment of the present invention is soaked in Li-S electrolysis
The zeta potential diagram tested in liquid；As shown in Figure 4, compared with conventional graphite alkene, the rGO@SL composite material that embodiment obtains exists
The characteristics of negative electricity is rendered obvious by electrolyte.
Fig. 5 be not coated piece of PP diaphragm (PP), in background technique the PP diaphragm (GO/PP) with graphite ene coatings and this
The chemical property of the lithium-sulfur cell of PP diaphragm (rGO@SL/PP) production of the invention based on rGO@SL coating；It (a) is forthright again
Can, (b-c) is the cycle performance of different multiplying.Show that the present invention is based on the lithium-sulfur cells that the PP diaphragm of rGO@SL coating makes
With good high rate performance and cycle performance.
Claims (4)
1. a kind of preparation method of the composite material for lithium-sulfur cell diaphragm coating, comprising the following steps:
Step 1: dispersing graphene oxide in dimethylformamide, ultrasound, obtain the graphene point that concentration is 1~2mg/mL
Dispersion liquid；
Step 2: hexamethylene diisocyanate is added in dimethylformamide, is uniformly mixed, obtained mixed liquor 140~
5min is heated in 150 DEG C of oil baths；Wherein, the concentration of hexamethylene diisocyanate is 3~5 μ L/mL in the mixed liquor；
Step 3: with the rate of 10~20mL/min step 2 is added treated mixing in the graphene dispersing solution that step 1 is obtained
In liquid, after being uniformly mixed, 30min is heated in 140~150 DEG C of oil baths, obtains mixed liquor A；
Step 4: sodium lignin sulfonate being added in dimethylformamide, being then heated to 80 DEG C keeps sodium lignin sulfonate completely molten
The lignin sulfonic acid sodium solution that concentration is 0.7~1mg/mL can be obtained in solution；
Step 5: the lignin sulfonic acid sodium solution that step 4 obtains is mixed with what the rate addition step 3 of 10~20mL/min obtained
It closes in liquid A, obtained mixed liquid B under inert gas protection, keeps 140~150 DEG C of 60~120min of thermotonus；Wherein,
The concentration of the graphene oxide restored in the mixed liquid B is 0.25~0.5mg/mL, the concentration of sodium lignin sulfonate is 0.5~
0.7mg/mL；
Step 6: after the reaction was completed, to reaction solution cooled to room temperature, after taking out and using deionized water centrifuge washing, passing through
Freeze-drying 12~for 24 hours, the composite material of the graphene oxide@sodium lignin sulfonate restored is as described to be used for lithium sulphur
The composite material of battery diaphragm coating.
2. the preparation method of the composite material according to claim 1 for lithium-sulfur cell diaphragm coating, which is characterized in that
Inert gas described in step 5 is argon gas.
3. a kind of preparation method of the lithium-sulfur cell diaphragm of the composite material obtained based on preparation method described in claim 1, packet
Include following steps:
Step 1: the graphene oxide@sodium lignin sulfonate composite material for the reduction that preparation method described in claim 1 is obtained
After being mixed with conductive additive, binder according to the ratio that mass ratio is 7:2:1, it is added in N-Methyl pyrrolidone, with obtained
The slurry that concentration to the graphene oxide@sodium lignin sulfonate composite material of reduction is 30~100mg/mL, is ground to slurry
In aterrimus it is thick after, continuously add N-Methyl pyrrolidone (NMP) and be diluted, make reduction graphene oxide@it is wooden
The concentration of plain sodium sulfonate composite material is reduced to 5~20mg/mL, then grinding is completely dispersed it；
Step 2: obtained slurry after step 1 processing is formed on PP diaphragm using the method filtered, as the coating of diaphragm,
The lithium-sulfur cell diaphragm can be obtained.
4. the preparation method of lithium-sulfur cell diaphragm according to claim 3, which is characterized in that the lithium-sulfur cell that step 2 obtains
In diaphragm, the coating with a thickness of 20~50 μm.
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| CN108963152B (en) * | 2018-06-28 | 2021-05-25 | 肇庆市华师大光电产业研究院 | g-C applied to lithium-sulfur battery diaphragm3N4Preparation method of/RGO coating |
| CN108987755A (en) * | 2018-08-28 | 2018-12-11 | 南京工业大学 | Method for applying lignosulfonate as binder to lithium-sulfur battery and application of lignosulfonate |
| CN110571390A (en) * | 2019-08-23 | 2019-12-13 | 华南师范大学 | Method for compositely modifying lithium-sulfur battery diaphragm by salinized graphene and carbon nano tube |
| CN111370620A (en) * | 2020-02-26 | 2020-07-03 | 华中科技大学 | Functional diaphragm of lithium-sulfur battery and preparation method thereof |
| CN112259927A (en) * | 2020-10-23 | 2021-01-22 | 青岛大学 | Lithium-sulfur battery diaphragm compounded with redox graphene and preparation method thereof |
| CN113206255A (en) * | 2021-05-06 | 2021-08-03 | 中国铁塔股份有限公司四川省分公司 | High-performance lithium-sulfur battery composite positive electrode material and preparation method thereof |
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| CN104979561A (en) * | 2015-05-23 | 2015-10-14 | 保定金阳光能源装备科技有限公司 | Graphene coating agent and preparation method for producing super lead-acid storage battery negative electrode plate from graphene coating agent |
| CN106654215A (en) * | 2016-12-30 | 2017-05-10 | 温州大学 | Small biological molecule and graphene composite material functional film and preparation method thereof |
| CN107069033A (en) * | 2017-03-21 | 2017-08-18 | 中国科学院福建物质结构研究所 | A kind of battery electrode of graphene-containing fiber and its preparation method and application |
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