CN110165222A - A kind of preparation method and applications of high-performance lithium-sulfur cell composite current collector - Google Patents
A kind of preparation method and applications of high-performance lithium-sulfur cell composite current collector Download PDFInfo
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- CN110165222A CN110165222A CN201910574538.6A CN201910574538A CN110165222A CN 110165222 A CN110165222 A CN 110165222A CN 201910574538 A CN201910574538 A CN 201910574538A CN 110165222 A CN110165222 A CN 110165222A
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M4/663—Selection of materials containing carbon or carbonaceous materials as conductive part, e.g. graphite, carbon fibres
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- H—ELECTRICITY
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Abstract
The present invention provides a kind of preparation method and applications of high-performance lithium-sulfur cell composite current collector, belongs to battery material preparation technical field.The present invention uses simple chemical synthesis process, nano metal piece NiCo2O4 is combined with carbon nano-fiber, on the one hand, has the characteristics that polarity using metal oxide, the polysulfide generated in reaction is fixed on anode, it solves the technical issues of carbon nano-fiber polarity is weak, can not adsorb polysulfide, improves stability test；On the other hand, using NiCo2O4 metal receive piece contact site it is more, the strong advantage of electronic conduction ability, accelerate electronics conduction, the reaction speed of electrochemical reaction in battery is improved, compared to traditional collector, unit capacity improves 70%, cyclical stability improves 100%, and lithium-sulfur cell, high rate performance and capacity with higher will be prepared based on the collector.
Description
Technical field
The invention belongs to battery material preparation technical fields, and in particular to a kind of high-performance lithium-sulfur cell composite current collector
Preparation method and applications.
Background technique
Developing new-energy automobile is to alleviate Chinese energy pressure, reply climate change, promote car industry and transportation
The important measure of sustainable development.In recent years, China's oil consumption external dependence degree is up to 60.6%, energy security, especially
The safety of petroleum resources has become the major hidden danger of China's economic development, and greatly developing renewable energy is to realize China's vapour
The only way of vehicle industrial repositioning, and the strategic choice of maintenance Chinese energy safety.However, renewable energy uncontrollable and
Unstability needs to match reliable energy-storage battery.Conventional lithium ion battery as current most successful energy storage device it
One, it is limited by itself storage volume, is still difficult to meet the following power battery to energy-storage battery height ratio capacity and high-energy density
Requirement.Therefore, developing high performance lithium ion battery is the necessary ways for developing new-energy automobile.
The theoretical specific capacity of lithium-sulfur cell (Li-S) is up to 1675mAh/g, and theoretical specific energy reaches 2600 Wh/kg, is to pass
Five to ten times of system ferric phosphate lithium cell, and sulphur itself has pollution-free, inexpensive feature, so that Li-S battery has become and works as
Preceding international research hot spot, it is considered to be Future New Energy Source Vehicular dynamic battery ideal chose (Nature Mater.8,500,
2009).However, the dissolution of polysulfide causes, positive electrode is lost and polysulfide passes through the effect that shuttles caused by diaphragm
(Nature Mater.11,19,2012) etc., all makes the cyclical stability of lithium-sulfur cell very poor, actual use is far not achieved
It is required that commercialization lithium-sulfur cell development is more slow.
Collector as one of lithium-sulfur cell important component receives the concern of many researchers.Currently, Li-
S battery uses aluminium foil as collector more, because its have many advantages, such as it is light-weight, cheap；But aluminium foil functionalization is single, can not
Higher load is born, there are natural limitations as the collector of Li-S energy-storage battery.3D collector such as carbon cloth, nickel foam
Deng since there are a large amount of mesh spaces, a large amount of contact area can be provided for sulphur, thus, use it to produce the energy storage of high load
Battery is possibly realized.But 3D collector due to itself do not have absorption polarity polysulfide the characteristics of, in circulating battery process
The polysulfide of middle generation is easily dissolved out from collector, causes apparent capacitance loss；Also, tradition 3D collector conduction energy
Power is poor, is unable to satisfy quick cell reaction.
Summary of the invention
It cannot solve to wear caused by high-sulfur load and polysulfide simultaneously for existing collector present in background technique
The problems such as shuttle effect, the purpose of the present invention is to provide a kind of preparation method of high-performance lithium-sulfur cell composite current collector and its answers
With.The present invention uses simple chemical synthesis process, by nano metal piece NiCo2O4It is combined with carbon nano-fiber, on the one hand,
Have the characteristics that polarity using metal oxide, the polysulfide generated in reaction is fixed on anode, carbon is solved and receives
The technical issues of rice fiber polarity is weak, can not adsorb polysulfide, improves stability test；On the other hand, NiCo is utilized2O4
Metal receive piece contact site it is more, the strong advantage of electronic conduction ability, accelerate electronics conduction, promoted battery in electrochemical reaction it is anti-
Speed is answered, and then improves the high rate performance and capacity of battery.
To achieve the above object, technical scheme is as follows:
A kind of preparation method of high-performance lithium-sulfur cell composite current collector, comprising the following steps:
Step 1: nickel source, cobalt source and reaction additives being add to deionized water, after ultrasonic mixing, obtain solution A；
Step 2: 3D collector being soaked in the mixed solution B of the concentrated sulfuric acid and hydrogen peroxide, rushed after ultrasound with deionized water
It washes, 3D collector after being cleaned；
Step 3: by after cleaning 3D collector and solution A be collectively disposed in reaction vessel, in 140~150 DEG C of oil baths
5~6h reaction is heated, NiCo is generated2OH；
Step 4: after reaction, 3D collector is taken out, rinsed, vacuum drying removes moisture removal, then place it in 400~
In Muffle furnace at 500 DEG C, it is sintered 3~4h under air atmosphere, after natural cooling, the composite current collecting can be prepared
Body.
Further, nickel source described in step 1 is six water nickel nitrates or nickel sulfate hexahydrate etc., and the cobalt source is cobalt nitrate hexahydrate
Or CoCL2 6H2O etc., the reaction additives be hexamethylenetetramine and Sodium Citrate, usp, Dihydrate Powder or be hexamethylenetetramine and
Ascorbic acid etc..
Further, the quality of nickel source described in step 1 is 170~180mg, and the quality of cobalt source is 340~360mg, reaction
The quality of additive is 200~300mg.
Further, 3D collector described in step 2 is the collector with a large amount of mesh spaces, specially carbon cloth, foam
Nickel etc., the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is (3~1) in mixed solution B: 1.
Further, the actual conditions of vacuum drying described in step 4 are as follows: 1~2h of vacuum drying at 40~60 DEG C.
A kind of preparation method of high-performance lithium-sulfur cell, comprising the following steps:
Step 1: it is 0.5~1cm that above-mentioned composite current collector, which is cut to size,2；
Step 2: sulphur powder (S) is dissolved in carbon disulfide (CS2) in solution, obtain solution C；
Step 3: the composite current collector after cutting being soaked in 5~8min in solution C, then takes out collector, is placed in baking
1~3h is dried in case, for removing extra CS2Solution takes after collection liquid surface is covered with white crystalline sulfur granules object
Collector out；
Step 4: by step 3, treated that collector is laid in hydrothermal reaction kettle, keep the temperature 8 at 150~200 DEG C~
15h, after the white crystalline sulfur granules on collector uniformly melt, lithium-sulphur cell positive electrode can be prepared in natural cooling；
Step 5: the anode assembled battery described in step 4.
Further, the concentration of sulphur powder is 0.3~0.5g/ml in solution C described in step 2.
In conclusion by adopting the above-described technical solution, the beneficial effects of the present invention are:
Collector prepared by the present invention is NiCo2O4Metal oxide nanometer sheet is grown on 3D carbon fiber collector, the knot
Structure can adsorb the polysulfide generated in cell reaction and accelerate ionic conduction；Pass through the modification to 3D collector, hence it is evident that
The capacity and performance for improving battery, compared to traditional collector, unit capacity improves 70%, and cyclical stability improves
100%, the lithium-sulfur cell prepared based on the collector, high rate performance and capacity with higher.
Detailed description of the invention
Fig. 1 is CC@NiCo prepared by the embodiment of the present invention 12O4The SEM of composite current collector schemes.
Fig. 2 is CC@NiCo prepared by the embodiment of the present invention 12O4The NiCo on composite current collector surface2O4SEM figure.
Fig. 3 is CC@NiCo prepared by the embodiment of the present invention 12O4The XRD diagram of composite current collector material.
Fig. 4 is CC@NiCo made from the embodiment of the present invention 12O4Composite current collector is used to assemble the cycle performance of lithium-sulfur cell
Figure.
Fig. 5 is CC@NiCo made from the embodiment of the present invention 12O4Composite current collector is for assembling lithium-sulfur cell in different charge and discharges
Performance map under electric current.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below with reference to embodiment and attached drawing, to this hair
It is bright to be described in further detail.
Embodiment 1
A kind of preparation method of high-performance lithium-sulfur cell composite current collector, comprising the following steps:
Step 1: by the six water nickel nitrate (Ni (NO of 175mg3)2·6H2O), the cobalt nitrate hexahydrate (Co (NO of 350mg3)2·
6H2O) be dissolved in 50ml deionized water, stir 30min, after it is completely dissolved again by the hexamethylenetetramine of 211mg,
Sodium Citrate, usp, Dihydrate Powder (the Na of 88mg3C6H5O7.2H2O it) is added and is dissolved with Ni (NO3)2·6H2O and Co (NO3)2·6H2The solution of O
In, ultrasonic 60min is completely dissolved all solids drug, and solution is purple, finally obtains to obtain solution A；
Step 2: by 2*2cm2The volume ratio that carbon cloth is soaked in 50ml is in the concentrated sulfuric acid of 1:1 and the mixed solution of hydrogen peroxide
30min then takes out and is rinsed 3 times with deionized water, to degrease and surface impurity；
Step 3: the carbon cloth after having cleaned and solution A are collectively disposed in there-necked flask, solution A is poured into, under protection of argon gas,
150 DEG C of condensation oil bath heating 6h are reacted, and NiCo is generated2OH；
Step 4: after reaction, carbon cloth being taken out, carbon cloth is rinsed using deionized water, rinses to deionized water without color
Afterwards, the vacuum drying 1h at 60 DEG C, to remove excessive moisture；The carbon cloth for taking out drying, places it in 500 DEG C of Muffle furnaces, empty
It is sintered in gas 3h (heating rate is 1 DEG C/min), after natural cooling, the composite current collector can be prepared.
NiCo is loaded on carbon cloth2O4Quality be about 0.3~0.4mg/cm2。
A kind of preparation method of high-performance lithium-sulfur cell, comprising the following steps:
Step 1: it is 0.6cm that above-mentioned composite current collector, which is cut to size,2；
Step 2: in draught cupboard, 0.5g sulphur powder being completely dissolved in 10ml CS2In solution, solution C is obtained；
Step 3: the composite current collector after cutting being soaked in 5min in solution C, collector is then taken out, is placed in baking oven
2h is dried at a temperature of 45 DEG C, for removing extra CS2Solution is covered with white crystalline sulfur granules object to collection liquid surface
Afterwards, collector is taken out；
Step 4: by step 3, treated that collector is laid in hydrothermal reaction kettle, 12h is kept the temperature at 170 DEG C, wait load
After uniformly melting with the white crystalline sulfur granules on collector, lithium-sulphur cell positive electrode can be prepared in natural cooling；
Step 5: the anode assembled battery described in step 4.
Sulphur loads about 1.2~1.8mg/cm in every anode of the lithium-sulfur cell2。
CC@NiCo manufactured in the present embodiment2O4The SEM figure of composite current collector is as shown in Figure 1；The Ni on composite current collector surface
Co2O4SEM figure it is as shown in Figure 2；CC@NiCo2O4The XRD diagram of composite current collector material is as shown in Figure 3；CC@NiCo obtained2O4
The cycle performance figure that composite current collector is used to assemble lithium-sulfur cell is as shown in Figure 4；Performance map such as Fig. 5 under different charging and discharging currents
It is shown.
Embodiment 2
A kind of preparation method of high-performance lithium-sulfur cell composite current collector, comprising the following steps:
Step 1: by the six water nickel nitrate (Ni (NO of 180mg3)2·6H2O), the cobalt nitrate hexahydrate (Co (NO of 360mg3)2·
6H2O) be dissolved in 50ml deionized water, stir 30min, after it is completely dissolved again by the hexamethylenetetramine of 200mg,
Sodium Citrate, usp, Dihydrate Powder (the Na of 35mg3C6H5O7.2H2O it) is added and is dissolved with Ni (NO3)2·6H2O and Co (NO3)2·6H2The solution of O
In, ultrasonic 60min is completely dissolved all solids drug, and solution is purple, finally obtains to obtain solution A；
Step 2: by 2*2cm2The volume ratio that carbon cloth is soaked in 50ml is in the concentrated sulfuric acid of 1:1 and the mixed solution of hydrogen peroxide
30min then takes out and is rinsed 3 times with deionized water, to degrease and surface impurity；
Step 3: the carbon cloth after having cleaned and solution A are collectively disposed in there-necked flask, solution A is poured into, under protection of argon gas,
150 DEG C of condensation oil bath heating 6h are reacted, and NiCo is generated2OH；
Step 4: after reaction, carbon cloth being taken out, carbon cloth is rinsed using deionized water, rinses to deionized water without color
Afterwards, the vacuum drying 1h at 60 DEG C, to remove excessive moisture；The carbon cloth for taking out drying, places it in 400 DEG C of Muffle furnaces, empty
It is sintered in gas 4h (heating rate is 1 DEG C/min), after natural cooling, the composite current collector can be prepared.
Embodiment 3
A kind of preparation method of high-performance lithium-sulfur cell composite current collector, comprising the following steps:
Step 1: by the six water nickel nitrate (Ni (NO of 170mg3)2·6H2O), the cobalt nitrate hexahydrate (Co (NO of 340mg3)2·
6H2O) be dissolved in 50ml deionized water, stir 30min, after it is completely dissolved again by the hexamethylenetetramine of 220mg,
Sodium Citrate, usp, Dihydrate Powder (the Na of 65mg3C6H5O7.2H2O it) is added and is dissolved with Ni (NO3)2·6H2O and Co (NO3)2·6H2The solution of O
In, ultrasonic 60min is completely dissolved all solids drug, and solution is purple, finally obtains to obtain solution A；
Step 2: by 2*2cm2The volume ratio that carbon cloth is soaked in 50ml is in the concentrated sulfuric acid of 1:1 and the mixed solution of hydrogen peroxide
30min then takes out and is rinsed 3 times with deionized water, to degrease and surface impurity；
Step 3: the carbon cloth after having cleaned and solution A are collectively disposed in there-necked flask, solution A is poured into, under protection of argon gas,
150 DEG C of condensation oil bath heating 6h are reacted, and NiCo is generated2OH；
Step 4: after reaction, carbon cloth being taken out, carbon cloth is rinsed using deionized water, rinses to deionized water without color
Afterwards, the vacuum drying 1h at 60 DEG C, to remove excessive moisture；The carbon cloth for taking out drying, places it in 450 DEG C of Muffle furnaces, empty
It is sintered in gas 4h (heating rate is 1 DEG C/min), after natural cooling, the composite current collector can be prepared.
A kind of preparation method of high-performance lithium-sulfur cell, comprising the following steps:
Step 1: it is 0.6cm that above-mentioned composite current collector, which is cut to size,2；
Step 2: in draught cupboard, 0.3g sulphur powder being completely dissolved in 10ml CS2In solution, solution C is obtained；
Step 3: the composite current collector after cutting being soaked in 5min in solution C, collector is then taken out, is placed in baking oven
2h is dried at a temperature of 45 DEG C, for removing extra CS2Solution is covered with white crystalline sulfur granules object to collection liquid surface
Afterwards, collector is taken out；
Step 4: by step 3, treated that collector is laid in hydrothermal reaction kettle, 12h is kept the temperature at 170 DEG C, wait load
After uniformly melting with the white crystalline sulfur granules on collector, lithium-sulphur cell positive electrode can be prepared in natural cooling；
Step 5: the anode assembled battery described in step 4.
From fig. 1, it can be seen that the flake nano NiCo that embodiment 1 obtains2O4It is uniformly covered in the surface of carbon fiber, compared to
Traditional carbon nano-fiber, sulphur is in NiCo2O4Surface has more contact sites and load point, has polarity NiCo2O4It receives
Rice piece can effectively adsorb polysulfide during cell reaction, its dissolution be avoided, to improve the stable circulation of battery
Property.Figure it is seen that NiCo2O4Structure in the form of sheets is grown on matrix surface, increases contact area.
As can be seen from Figure 3, the material of matrix surface growth is really NiCo2O4, multiple peak positions such as (220), (311) are and PDF
The peak position of card 02-1074 is consistent.
As can be seen from Figure 4, by CC@NiCo2O4The lithium-sulfur cell of/S positive electrode preparation has the initial capacity of 670mAh/g,
After the circle of circulation 200, the 90% of initial capacity is still maintained, and coulombic efficiency is close to absolutely.
As can be seen from Figure 5, NiCo2O4Can not only make battery stablize circulation, under various current conditions (0.2C, 0.5C, 1C,
2C) all there is good cyclical stability；Also, even if still having the considerable appearance of 400mAh/g under the conditions of high current (2C)
Amount.
The above description is merely a specific embodiment, any feature disclosed in this specification, except non-specifically
Narration, can be replaced by other alternative features that are equivalent or have similar purpose；Disclosed all features or all sides
Method or in the process the step of, other than mutually exclusive feature and/or step, can be combined in any way.
Claims (7)
1. a kind of preparation method of high-performance lithium-sulfur cell composite current collector, which comprises the following steps:
Step 1: nickel source, cobalt source and reaction additives being added in deionized water, after ultrasonic mixing, obtain solution A；
Step 2: 3D collector being soaked in the mixed solution B of the concentrated sulfuric acid and hydrogen peroxide, rinsed, obtained with deionized water after ultrasound
3D collector after to cleaning；
Step 3: by after cleaning 3D collector and solution A be collectively disposed in reaction vessel, react 5 in 140~150 DEG C of oil baths
~6h；
Step 4: after reaction, taking out 3D collector, rinse, vacuum drying removes moisture removal, then places it in 400~500
In Muffle furnace at DEG C, it is sintered 3~4h under air atmosphere, after natural cooling, the composite current collector can be prepared.
2. the preparation method of high-performance lithium-sulfur cell composite current collector according to claim 1, which is characterized in that step 1
The nickel source is six water nickel nitrates or nickel sulfate hexahydrate, and the cobalt source is cobalt nitrate hexahydrate or CoCL2 6H2O, and the reaction adds
Agent is added to be hexamethylenetetramine and Sodium Citrate, usp, Dihydrate Powder mixture or be hexamethylenetetramine and ascorbic acid mixture.
3. the preparation method of high-performance lithium-sulfur cell composite current collector according to claim 1, which is characterized in that step 1
The quality of the nickel source is 170~180mg, and the quality of cobalt source is 340~360mg, the quality of reaction additives is 200~
300mg。
4. the preparation method of high-performance lithium-sulfur cell composite current collector according to claim 1, which is characterized in that step 2
The 3D collector is the collector with mesh space, specially carbon cloth, nickel foam；The concentrated sulfuric acid and dioxygen in mixed solution B
The volume ratio of water is (3~1): 1.
5. the preparation method of high-performance lithium-sulfur cell composite current collector according to claim 1, which is characterized in that step 4
The actual conditions of the vacuum drying are as follows: 1~2h of vacuum drying at 40~60 DEG C.
6. a kind of side of the composite current collector preparation high-performance lithium-sulfur cell obtained based on any the method for Claims 1 to 5
Method, which comprises the following steps:
Step 1: it is 0.5~1cm that above-mentioned composite current collector, which is cut to size,2；
Step 2: sulphur powder being dissolved in carbon disulfide solution, solution C is obtained；
Step 3: the composite current collector after cutting being soaked in 5~8min in solution C, collector is then taken out, is placed in baking oven
1~3h is dried, after collection liquid surface is covered with white crystalline sulfur granules object, takes out collector；
Step 4: by step 3, treated that collector is laid in hydrothermal reaction kettle, and 8~15h is kept the temperature at 150~200 DEG C, to
After white crystalline sulfur granules on collector uniformly melt, lithium-sulphur cell positive electrode can be prepared in natural cooling；
Step 5: the anode assembled battery described in step 4.
7. the preparation method of high-performance lithium-sulfur cell according to claim 6, which is characterized in that sulphur in solution C described in step 2
The concentration of powder is 0.3~0.5g/ml.
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