CN109037627A - A kind of alkali metal base composite negative pole and its application - Google Patents
A kind of alkali metal base composite negative pole and its application Download PDFInfo
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- CN109037627A CN109037627A CN201810805334.4A CN201810805334A CN109037627A CN 109037627 A CN109037627 A CN 109037627A CN 201810805334 A CN201810805334 A CN 201810805334A CN 109037627 A CN109037627 A CN 109037627A
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- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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Abstract
The invention discloses a kind of alkali metal base composite negative pole and its applications, which includes alkali metal, and the fluorinated carbon material being uniformly distributed in alkali metal；The alkali metal base composite negative pole is prepared through infiltrated with molten metal method, and tiling shape is presented in the fluorinated carbon material in alkali metal.Fluorinated carbon material is introduced into alkali metal by the present invention, the fluoride of alkali metal can be formed in situ in charge and discharge process, the fluoride and carbon material form synergistic effect, uniform electric field is formed in charge and discharge process, to promote the uniform deposition of alkali metal, effectively inhibit the formation of alkali metal dendrite and the interfacial reaction of alkali metal and electrolyte, improves the security performance and cyclical stability of alkali metal battery.
Description
Technical field
The present invention relates to the technical fields of energy-storage battery, and in particular to a kind of alkali metal base composite negative pole and its application.
Background technique
Although lithium ion battery still occupies leading position in the secondary battery, as new-energy automobile is to lithium-ion electric
Energy density requirement in pond is higher and higher, and the energy density of traditional lithium ion battery based on insertion reaction has reached the limit, i.e.,
Bottleneck value is had been approached by the energy density of the lithium ion battery of cathode of graphite, exploitation is using lithium metal as the lithium battery (packet of cathode
Include lithium-sulfur cell, lithium sky battery) it is imperative.On the other hand, with the development of new-energy automobile, the consumption of lithium resource quickly,
But the reserves of lithium on earth are very limited, and in contrast, the reserves of sodium and potassium are relatively abundant, can satisfy large-scale use.
Therefore, it develops the novel battery based on sodium and potassium and has become the hot spot currently researched and developed.
It but a use of fatal problem of the battery that alkali metal is cathode is directly alkali metal meeting in charge and discharge cycles
Li dendrite is formed, the safety problem of battery is caused.In addition, the compatibility of alkali metal and liquid electrolyte and some solid electrolytes
Poor, long-term circulation will lead to the corrosion of alkali metal or the formation of interface passivation layer, to reduce the cycle life of battery.Cause
This, in order to improve safety and the service life of alkali metal battery, it is necessary to make protection processing to alkali metal.
Previous research concentrates on carbon material and fluoride protects alkali metal, such as Publication No. CN 108063218
A kind of preparation method of sheet metal lithium base cathode is disclosed in the Chinese patent literature of A, first copper foil current collector has been base to cathode
Bottom synthesizes single-layer graphene film on copper foil current collector surface using chemical vapour deposition technique, the graphene supported with this copper foil
For cathode, anode is made with rich lithium material or lithium salts and forms into lithium battery, then applying electric current keeps the lithium in rich lithium material or lithium salts heavy
Product obtains lithium metal/graphene composite negative, although can be obtained with this method relatively uniform in the graphene that copper foil supports
Composite negative pole is suitable for than relatively thin electrode, but when electrode is thicker, easily causes lithium to be distributed in graphene uneven, separately
Outside, although carbon material to inhibit Li dendrite effect it is preferable, electrode is protected, inhibit with the reaction effect of electrolyte compared with
It is weak.
It for another example authorizes in the Chinese patent literature of Publication No. CN 207441857U and discloses a kind of lithium metal/artificial nothing
Machine salt combination electrode, the combination electrode are obtained after metallic lithium surface deposited inorganic using magnetron sputtering method, the inorganic matter
Such as lithium fluoride, lithium bromide, lithium chloride, this method although available relatively uniform surface coating layer, but be equally suitable only for
In thin electrode, and it is not easy to realize large scale preparation, in addition, since inorganic matter conductivity is lower, simple inorganic compound
Introduce the decline that will cause electrode conductivity.
Summary of the invention
The invention discloses a kind of novel alkali metal base composite negative poles, and formation and the alkali of alkali metal dendrite can be effectively suppressed
The interfacial reaction of metal and electrolyte improves the security performance and cyclical stability of alkali metal battery.
Specific technical solution is as follows:
A kind of alkali metal base cathode, including alkali metal, and the fluorinated carbon material being uniformly distributed in alkali metal；
The alkali metal base composite negative pole is prepared through infiltrated with molten metal method；
Tiling shape is presented in the fluorinated carbon material in alkali metal.
Fluorinated carbon material is introduced into alkali metal by first passage infiltrated with molten metal method of the present invention, can be former in charge and discharge process
Position forms the fluoride of alkali metal, and since the fluoride and carbon material of alkali metal are in close contact, there are bondings or part bonding to make
With fluoride and carbon material form synergistic effect, uniform electric field are formed in charge and discharge process, to promote the equal of alkali metal
Even deposition effectively inhibits the formation of alkali metal dendrite to improve the safety of alkali metal battery；On the other hand, the fluorination being formed in situ
Effective protection alkali metal is inhibited reacting for alkali metal and organic bath or solid electrolyte, it is golden to improve alkali by object and carbon material
Belong to the cycle life that battery is improved with the interface stability of electrolyte；Furthermore the carbon material introduced in situ can be improved multiple
The conductivity for closing cathode, to reduce polarization of electrode.
So-called polarization, the absolute value of deviation from origin when referring to electrode charge or electric discharge.
It is found through experiment that when using the technical solution for being directly added into fluoride and carbon material, since fluoride is in carbon materials
It is difficult to realize bonding action that is evenly dispersed, being more difficult realization the two in material, cannot achieve the synergistic effect of the two to inhibit alkali golden
The formation and protection alkali metal, the Local enrichment of the fluoride of low conductivity for belonging to dendrite also will lead to the increase of electrode polarization, from
And cause the high polarization of electrode and short cycle life.
The alkali metal is selected from least one of lithium, sodium, potassium；
The fluorinated carbon material is soft selected from fluorinated nano carbon pipe, fluorinated carbon fiber, fluorinated graphene, fluorination hard carbon, fluorination
At least one of carbon, fluorinated fullerene, fluorographite.
Preferably, the weight ratio of the alkali metal base cathode, fluorinated carbon material and alkali metal is 1~20:100.
In the alkali metal base cathode, reasonable alkali metal and fluorination carbon content are conducive to adequately protect to alkali metal
In the case where without influence alkali metal cathode capacity and reversible degree.Further preferably, the weight of fluorinated carbon material and alkali metal
Than for 2.5~10:100.
In the alkali metal base cathode, too low fluorine content is unfavorable for that alkali metal is effectively protected, due to fluorination
The conductivity of carbon is lower, and excessively high fluorine content will reduce the conductivity of composite negative pole, to reduce the high rate performance and appearance of cathode
Amount.Preferably, in the fluorinated carbon material, fluorine content is 5~65%.Based on the commercialization situation of current fluorinated carbon material, directly
The fluorinated carbon material that commercially available fluorine content is 50% is selected in selecting, at this point, also raw material gross weight can be accounted for by adjusting fluorinated carbon material
Ratio fluorine content is adjusted.
Preferably, the fluorinated carbon material is powdered, having a size of 10nm~50 μm.Further preferably nanoscale material
Material, having a size of 10nm~500nm.So-called nano-scale, as long as the size for meeting at least one direction on three-dimensional is nanometer
Grade；Particle size is too small easy to reunite, particle size is excessive be unfavorable for it is evenly dispersed in alkali metal, and in conjunction with alkali metal
Power dies down.
Preferably, the fluorinated carbon material is selected from fluorinated nano carbon pipe, fluorinated carbon fiber or fluorinated graphene.
It is further preferred:
The fluorinated carbon material is selected from fluorinated nano carbon pipe or fluorinated graphene；
The weight ratio of the fluorinated carbon material and alkali metal is 2.5~5:100.
The diameter of the fluorinated nano carbon pipe is 30~60nm, and length is 500nm~2 μm, by weight, fluorinated nano carbon
Fluorine content is 50% in pipe；
The lateral dimension of the fluorinated graphene powder is 5~50 μm, and longitudinal number of plies is that single layer or a small number of layers (are lower than 10
Layer), fluorinated volume 50wt%.
It is found through experiment that with using the electricity of the alkali metal base composite negative pole assembling of the above-mentioned raw material preparation advanced optimized
Pond, polarization value can be down to 22mV.
Still further preferably, the fluorinated carbon material is selected from fluorinated nano carbon pipe, and alkali metal is selected from lithium metal or metallic sodium,
Polarization value can be down to 20mV.
Further preferably, the fluorinated carbon material is selected from fluorinated nano carbon pipe, and alkali metal is selected from metallic sodium, and polarization value can be down to
15mV。
The alkali metal base composite negative pole is prepared using simple infiltrated with molten metal method, and this method technics comparing is simple, due to
Alkali metal fusing point is lower, only by heating alkali metal heating melting then carbon fluoride powder need to be added to the alkali gold of melting
In category, alkali metal/fluorination carbon compound cathode is can be obtained in agitated and natural cooling, in the compound cathode of lithium obtained with this method
Fluorocarbons distribution is relatively uniform, is advantageously implemented the cycle life of Compound Negative extremely low polarization and length.
Specific step is as follows:
1) under inert atmosphere protection, by alkali metal heating and melting；
2) carbon fluoride powder is added in the alkali metal melted, does not stop to be stirred until homogeneous, alkali gold is obtained after cooled and solidified
Belong to base composite negative pole.
In step 1), the inert atmosphere is argon gas, nitrogen or helium, and preferably argon gas is prepared atmosphere.The temperature of thawing
There is no special provision, just alkali metal thawing to be advisable.
In step 2), the mixing speed does not have special regulation, in the alkali metal of melting uniformly by fluorocarbons
Dispersion is advisable.
In step 3), the cooling temperature does not have special regulation, and melt body solidification is advisable, to promote fluorocarbons to exist
It is uniformly dispersed, can melt repeatedly and is solidified repeatedly in alkali metal, so-called uniform, not stringent judgment criteria, with visually face
Color is uniform and microcosmic powers on subject to sem observation.
The invention also discloses the alkali metal base composite negative poles in alkali metal battery, alkali metal-sulphur battery, alkali gold
Application in category-air cell.
Compared with prior art, the present invention has the advantage that
1, alkali metal base cathode of the invention passes through simple infiltrated with molten metal using alkali metal and fluorinated carbon material as raw material
Fluorinated carbon material is dispersed in alkali metal by method, and the fluoride of alkali metal can be formed in situ in charge and discharge process, should
Fluoride and carbon material form synergistic effect, uniform electric field are formed in charge and discharge process, to promote the uniform of alkali metal
Deposition effectively inhibits the formation of alkali metal dendrite and the interfacial reaction of alkali metal and electrolyte, improves the safety of alkali metal battery
Performance and cyclical stability, meanwhile, conductivity can be improved in the carbon material being formed in situ, and reduces polarization of electrode.
2, the preparation process of alkali metal base cathode uses cheap raw material in the present invention, and simple process, consume energy low, cost
Small, the period is short, is conducive to large-scale production.
Detailed description of the invention
Fig. 1 is lithium/fluorinated graphene composite negative pole X-ray diffraction (XRD) map prepared by embodiment 1；
Fig. 2 is lithium/fluorinated graphene composite negative pole scanning electron microscope (SEM) photo prepared by embodiment 1；
Fig. 3 is the charging and discharging curve of the lithium/fluorinated graphene composite negative pole assembling Symmetrical cells prepared with embodiment 1；
Fig. 4 is the F1s x-ray photoelectron spectroscopy after lithium/fluorinated graphene composite negative pole charge and discharge prepared by embodiment 1
(XPS)；
Fig. 5 is the charging and discharging curve of the Symmetrical cells of the cathode of lithium assembling prepared with comparative example 1.
Specific embodiment
Present invention is further described in detail with reference to the accompanying drawings and embodiments, it should be pointed out that following embodiment
It is intended to convenient for the understanding of the present invention, and does not play any restriction effect to it.
Embodiment 1
Under argon atmosphere protection, lithium metal is melted by heating；The gold into melting is added in fluorinated graphene powder
Belong to lithium, the weight of fluorinated graphene and the weight ratio of lithium metal are 5%, and the fluorinated volume of fluorinated graphene is 50wt%, graphene
Powder lateral dimension is 5~50 μm, and longitudinal number of plies is single layer or a small number of layers (being lower than 10 layers)；The gold of fluorinated graphene will be impregnated with
Belong to lithium melt body cooled and solidified, obtains lithium metal/fluorinated graphene composite negative pole.
Fig. 1 is the XRD spectrum of composite negative pole manufactured in the present embodiment, from map it is found that diffraction maximum is lithium peak, fluorographite
There is not diffraction maximum since content is low, crystallinity is low in figure in alkene.
Fig. 2 is the SEM photograph of composite negative pole manufactured in the present embodiment, from photo it is found that fluorinated graphene is in lithium metal
Disperse it is relatively uniform, fluorinated graphene presented in alkali metal tiling shape, i.e. its position is parallel with lithium piece, and fluorinated graphene does not have
There is local agglomeration.
Fig. 3 is the charging and discharging curve of the Symmetrical cells assembled with composite negative pole manufactured in the present embodiment (with LiClO4Three
Glycol dimethyl ether (TEGDME) solution is electrolyte, and Celgard C480 film is diaphragm, as current density 0.5mA/cm2, hold
Amount is 1mAh/cm2When, by 200 hours, the polarization of Symmetrical cells is only 22 millivolts, as current density 1mA/cm2, capacity is
1mAh/cm2When, by 200 hours, the polarization of Symmetrical cells is only 91 millivolts, as current density 5mA/cm2, capacity is
1mAh/cm2When, by 100 hours, the polarization of Symmetrical cells is only 292 millivolts.Fig. 4 is Compound Negative manufactured in the present embodiment
F1s XPS map of the pole after charge and discharge, from map it is found that foring LiF.
Comparative example 1
The preparation of electrode and the assembly such as embodiment 1 of battery, except that fluorographite is not added in lithium metal
Alkene, electro-chemical test show (current density 0.5mA/cm2, capacity 1mAh/cm2When, by 200 hours), it polarizes as 34 millis
Volt, is shown in Fig. 5.
Comparative example 2
The preparation of electrode and the assembly such as embodiment 1 of battery, except that the general of identical weight is added in lithium metal
Logical graphene, rather than fluorinated graphene, electro-chemical test show (current density 0.5mA/cm2, capacity 1mAh/cm2When, pass through
200 hours), under identical testing conditions, polarizing is 30 millivolts.
Comparative example 3
The preparation of electrode and the assembly such as embodiment 1 of battery, except that lithium fluoride and graphite are added in lithium metal
The mole of carbon and fluorine is identical in fluorinated graphene in the mole with embodiment of fluorine in alkene, graphene and lithium fluoride.Electrochemistry
Test shows (current density 0.5mA/cm under identical testing conditions2, capacity 1mAh/cm2When, by 200 hours),
Polarization is 31 millivolts.
Embodiment 2
The preparation of electrode and the assembly such as embodiment 1 of battery, except that by fluorinated graphene change into equal additive amounts,
The identical fluorinated nano carbon pipe of fluorinated volume, electro-chemical test show (current density 0.5mA/cm under identical testing conditions2,
Capacity is 1mAh/cm2When, by 200 hours), polarizing is 20 millivolts.
Embodiment 3
Under argon atmosphere protection, metallic sodium is melted by heating；Fluorinated nano carbon pipe powder is penetrated into melting
Metallic sodium, the weight of fluorinated nano carbon pipe and the weight ratio of metallic sodium are 2.5%, and the fluorinated volume of fluorinated graphene is 50wt%；
It will be impregnated with the metallic sodium melt body cooled and solidified of fluorinated nano carbon pipe, obtains metallic sodium/fluorinated nano carbon pipe composite negative pole.Product warp
XRD characterization is metallic sodium, and fluorinated nano carbon pipe diffraction maximum does not occur since content is low, crystallinity is low in figure.Product is through SEM
Characterization, fluorinated nano carbon pipe disperses relatively uniform in metallic sodium.Electro-chemical test shows (current density 0.5mA/cm2, capacity
For 1mAh/cm2When, by 200 hours), be only using metallic sodium/fluorinated nano carbon pipe as the polarization of the Symmetrical cells of electrode
15mV。
Embodiment 4
Under argon atmosphere protection, by heating metal kali fusion；Fluorinated carbon fiber powder is penetrated into the gold into melting
Belong to potassium, the weight of fluorinated carbon fiber and the weight ratio of metallic potassium are 10%, and the fluorinated volume of fluorinated carbon fiber is 50wt%；It will be impregnated with
The metallic potassium melt body cooled and solidified of fluorinated carbon fiber, obtains metallic potassium/fluorinated carbon fiber composite negative pole.Product is through XRD characterization
There is not diffraction maximum since content is low, crystallinity is low in figure in metallic potassium, fluorinated carbon fiber.Product is characterized through SEM, fluorocarbons
Fiber disperses relatively uniform in metallic potassium.Electro-chemical test shows (current density 0.5mA/cm2, capacity 1mAh/cm2When,
By 200 hours), it is only 25mV by the polarization of the Symmetrical cells of electrode of metallic potassium/fluorinated carbon fiber.
Claims (9)
1. a kind of alkali metal base composite negative pole, which is characterized in that including alkali metal, and the fluorination being uniformly distributed in alkali metal
Carbon material；
The alkali metal base composite negative pole is prepared through infiltrated with molten metal method；
Tiling shape is presented in the fluorinated carbon material in alkali metal.
2. alkali metal base composite negative pole according to claim 1, it is characterised in that:
The alkali metal is selected from least one of lithium, sodium, potassium；
The fluorinated carbon material is selected from fluorinated nano carbon pipe, fluorinated carbon fiber, fluorinated graphene, fluorination hard carbon, fluorination soft carbon, fluorine
Change at least one of fullerene, fluorographite.
3. alkali metal base composite negative pole according to claim 1, which is characterized in that in the fluorinated carbon material, fluorine content
It is 5~65%；
The fluorinated carbon material be it is powdered, having a size of 10nm~50 μm.
4. alkali metal base composite negative pole according to claim 1, which is characterized in that the fluorinated carbon material and alkali metal
Weight ratio is 1~20:100.
5. alkali metal base composite negative pole described in any claim according to claim 1~4, which is characterized in that the fluorination
Carbon material is selected from fluorinated nano carbon pipe, fluorinated carbon fiber or fluorinated graphene.
6. alkali metal base composite negative pole according to claim 5, which is characterized in that the fluorinated carbon material and alkali metal
Weight ratio is 2.5~10:100.
7. alkali metal base composite negative pole according to claim 1, which is characterized in that the step of the infiltrated with molten metal method such as
Under:
1) under inert atmosphere protection, by alkali metal heating and melting；
2) carbon fluoride powder is added in the alkali metal melted, does not stop to be stirred until homogeneous, alkali metal base is obtained after cooled and solidified
Composite negative pole.
8. alkali metal base composite negative pole according to claim 7, which is characterized in that the inert atmosphere is selected from argon gas, nitrogen
Gas or helium.
9. alkali metal base composite negative pole described in a kind of any claim according to claim 1~6 is in alkali metal battery, alkali gold
Application in category-sulphur battery, alkali metal-air cell.
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| CN111564591A (en) * | 2020-04-30 | 2020-08-21 | 北京航空航天大学 | Lithium metal battery diaphragm modified slurry and application thereof |
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| CN109713223A (en) * | 2018-12-28 | 2019-05-03 | 蜂巢能源科技有限公司 | Lithium an- ode and preparation method thereof, lithium ion battery |
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| CN109037627B (en) | 2020-08-25 |
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