CN109244441A - Non-newtonian flow posture Na-K alloy electrode and its preparation method and application - Google Patents
Non-newtonian flow posture Na-K alloy electrode and its preparation method and application Download PDFInfo
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- CN109244441A CN109244441A CN201810993691.8A CN201810993691A CN109244441A CN 109244441 A CN109244441 A CN 109244441A CN 201810993691 A CN201810993691 A CN 201810993691A CN 109244441 A CN109244441 A CN 109244441A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/40—Alloys based on alkali metals
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of non-newtonian flow posture Na-K alloy electrode and preparation method thereof and as the application of alkali metal secondary battery negative electrode material; this method comprises: under inert gas protection; karat gold is belonged to and Na metal physics stack; karat gold occurs to belong to and the metallic alloying reaction of Na, acquisition Na-K liquid alloy;Under inert gas protection, liquid Na-K alloy and powder granule are mixed, form non-newtonian fluid Na-K alloy composite materials, then the material is coated on carrier, obtain non-newtonian fluid Na-K alloy electrode.The non-newtonian fluid Na-K alloy composite materials that the electrode includes carrier, is coated on carrier.Electrode of the present invention has the characteristics that high coulombic efficiency, without dendritic growth and stable structure, can be used as potassium metal negative electrode and sodium metal negative electrode simultaneously, when matching with the positive electrodes such as sulphur, Prussian blue, significantly improve the energy density and cyclical stability of full battery.
Description
Technical field
The present invention relates to alkali metal secondary battery negative electrode material technical fields, and in particular to a kind of non-newtonian flow posture Na-K
Alloy electrode and preparation method thereof and application as alkali metal secondary battery negative electrode material.
Background technique
With the development of science and technology and electronic product it is universal, traditional battery can no longer meet demand.Alkali metal
Battery has the characteristics that reserves are big, preparation cost is low, electrochemical window mouth width as a kind of new type of energy storage device, mobile communication,
The fields such as electric car and energy storage have broad application prospects.Alkali metal cathode is aoxidized relative to traditional carbon material, metal
Object etc. has higher specific capacity.But alkali metal cathode is also easy to produce dendrite, leads to battery short circuit, causes security risk, limits
Its large-scale application.The growth that dendrite can be completely inhibited using Na-K alloy as the liquid alloy of representative becomes emerging no branch
Brilliant electrode material research direction.In addition, Na-K liquid alloy has hypotoxicity, wide (even -12.6 DEG C at normal temperature of equilibrium temperature
All exist in liquid form) etc. characteristics.However liquid Na-K alloy surface tension is big, it is difficult to it is wet in collection liquid surface, seriously
Hinder its commercial applications.Therefore, application of the stable liquid metal electrode of research room temperature flowering structure to alkali metal secondary battery
Development is of great significance.
Studies have shown that high-temperature process (> 420 DEG C) can promote wettability of the liquid Na-K alloy on carbon paper, while more
Pore structure substrate can capture more liquid Na-K alloys, solve the problems, such as Na-K liquid alloy mobility.However in room temperature
Under, due to the recovery of liquid Na-K alloy surface tension, cause the liquid Na-K alloy of combination electrode surface exposure to fall off, especially
It is that inner alloy can be squeezed out under the action of by external force, forms exposed alloy.Therefore simple carbon carrier loads liquid
Na-K alloy cannot inherently solve interface stability this problem.
Therefore, the fluid properties for changing liquid Na-K alloy are that essence solution liquid Na-K alloy electrode structural stability is asked
The key of topic.However, at present both at home and abroad without for the fluidity Quality Research for changing liquid Na-K alloy.Therefore, from change
The fluid properties of liquid Na-K alloy, constructing stable electrode and electrolyte interface is liquid Na-K alloy anode large-scale application
Continue the critical problem solved.
Summary of the invention
For the problems in background technique, the purpose of the present invention is to provide a kind of non-newtonian flow posture Na-K alloy electrodes
And preparation method thereof and as alkali metal secondary battery negative electrode material application, this method can change Na-K liquid alloy and easily flow
Physical property, with prepare have compared with stiff stability without dendrite alkali metal battery cathode.
A kind of preparation method of non-newtonian flow posture Na-K alloy electrode, comprising the following steps:
1) under inert gas protection, karat gold is belonged to and Na metal physics stack, karat gold category occurs and Na is metallic alloying anti-
It answers, obtains Na-K liquid alloy;
2) under inert gas protection, the liquid Na-K alloy of step 1) preparation and powder granule are mixed, formed
Non-newtonian fluid Na-K alloy composite materials, then the material is coated on carrier, non-newtonian flow posture Na-K alloy coat is formed,
Obtain non-newtonian fluid Na-K alloy electrode.
In step 1), the amount of the K and Na according to a certain percentage, the quality of quality and Na metal that the karat gold belongs to
The ratio between be 70~86:14~30, preferably 75~81:19~25 are still more preferably 77~79:21~23.
The karat gold belongs to and Na metal is pure K and pure Na.
The karat gold belongs to and Na metal is using preceding needing to cut removal oxide on surface.
In step 2), the powder granule is nano carbon microsphere, cupric oxide nano powder or silicon nano power.
The preparation of the nano carbon microsphere includes: by glucose and the aqueous solution for containing sodium alkyl benzene sulfonate (surfactant)
It is uniformly mixed, then pours into hydro-thermal tank, (hydro-thermal 12 was small at preferably 180 DEG C in 10~14 hours for hydro-thermal at 170 DEG C~190 DEG C
When), it cleans and obtains nano carbon microsphere.The ratio between the glucose and the dosage of aqueous solution containing sodium alkyl benzene sulfonate for 0.5g~
2.5g:400mL~600mL (preferably 1g:500mL), sodium alkyl benzene sulfonate in the aqueous solution containing sodium alkyl benzene sulfonate
Mass percent be 0.5~2% (preferably 1%).
The preparation of the cupric oxide nano powder includes: that two hydration dichloride copper (are lived on surface with containing sodium alkyl benzene sulfonate
Property agent) aqueous solution be uniformly mixed, then pour into hydro-thermal tank, (preferably 160 DEG C of hydro-thermal 9~13 hours at 150 DEG C~170 DEG C
Lower hydro-thermal 11 hours), it cleans and obtains cupric oxide nano powder.
The two hydration dichloride copper are 1.5g~3.5g with the ratio between the dosage of aqueous solution containing sodium alkyl benzene sulfonate:
800mL~1200mL (preferably 2.5g:1000mL), sodium alkyl benzene sulfonate in the aqueous solution containing sodium alkyl benzene sulfonate
Mass percent is 0.5~2% (preferably 1%).
The preparation of the silicon nano power includes: by silicon oxide powder and the water for containing sodium alkyl benzene sulfonate (surfactant)
Solution is uniformly mixed, then is poured into hydro-thermal tank, (the hydro-thermal 12 at preferably 180 DEG C of hydro-thermal 10~14 hours at 170 DEG C~190 DEG C
Hour), it cleans and obtains silicon nano power.
The ratio between the silicon oxide powder and the dosage of aqueous solution containing sodium alkyl benzene sulfonate for 1g~2.8g:800mL~
1200mL (preferably 1.8g:1000mL), the quality hundred of sodium alkyl benzene sulfonate in the aqueous solution containing sodium alkyl benzene sulfonate
Score is 0.5~2% (preferably 1%).
The non-newtonian fluid Na-K alloy composite materials are similar paint shape alloy, can be smeared with tools such as brushes
To carrier.
The amount of the liquid Na-K alloy and powder granule according to a certain percentage, the liquid Na-K alloy and powder
The mass ratio of body particle be 0.1~5:1, further preferably 0.1~3:1, be still more preferably 0.256~1.28:1.
The carrier can be any solid carrier.Conductive carrier, non-conducting carrier can be divided by electric conductivity, by dimension
Degree can be divided into one-dimensional carrier, two-dimensional carrier, three-dimensional carrier, can be divided into metallic carrier, organic carrier, without airborne by material
Body.Preferably certain thickness two-dimensional film conductive carrier, most preferably the two-dimensional film carbon material of certain thickness and area.It is non-
Newtonian fluid Na-K alloy itself has fine electric conductivity, therefore does not limit carrier characteristics.
The carrier with a thickness of 0.1mm~10mm, further preferably 0.5mm~5mm, most preferably 1mm~
2mm。
The area of the carrier is 0.1cm2~10cm2, further preferably 0.2cm2~2cm2, most preferably 0.5cm2
~1.5cm2, wherein length and width shape is unlimited, is preferably square or round.
In step 2), the non-newtonian flow posture Na-K alloy electrode is calculated as 0.001gcm according to electrode area-2~
10gcm-2, further preferably 0.01gcm-2~5gcm-2, most preferably 0.05gcm-2~0.2gcm-2。
Step 1) and 2) described in inert gas be argon gas, preferably high-purity argon gas.Full of in inert gas environment, water
Content is lower than 0.1ppm.
It obtains Na-K alloy under non-newtonian flow posture Na-K alloy at normal temperature and remains liquid, dendritic growth situation is not present,
It can be used as K ion battery cathode material and Na ion battery cathode material simultaneously.
The non-newtonian flow posture Na-K alloy electrode includes carrier and the non-newtonian flow posture Na- in supported on carriers
K alloy.The non-newtonian flow posture Na-K alloy/nm carbon composite is paint shape, has paintable characteristic, not loaded
Bulk area limitation, can prepare larger size electrode.
The non-newtonian fluid Na-K alloy composite materials have the abilities such as very strong stretch-proof, bending, can be used as
Flexible battery cathode uses.
Application of the non-newtonian flow posture Na-K alloy electrode as alkali metal secondary battery negative electrode material.
The present invention compared with the prior art, has the following advantages that and protrudes effect:
The present invention is for preparation with rock-steady structure without dendrite liquid alloy negative electrode.The present invention has following two
Feature: 1) the liquid Na-K alloy of conventional liquid property is easy to fall off from electrode surface, lead because having stronger surface tension
Send a telegraph pole structural instability.The present invention proposes building non-newtonian flow posture Na-K alloy, inherently solves conventional liquid Na-K
The problem of alloy and electrode binding force, various shape carrier surface can be applied directly to.2) conventional liquid Na-K alloy is liquid
Body needs to be adsorbed on carrier inside, and during carrier is bent and is stretched, liquid Na-K alloy itself is difficult with carrier change
Shape is easy to fall off from carrier.Non-newtonian flow posture Na-K alloy proposed by the present invention changes the property of easily flowing liquid, becomes
At coating, inherently there are the abilities such as stretch-proof, bending, can be applied to flexible battery.In addition, because its non-newtonian fluid
The characteristic of state can be applied on large area carrier, be suitable for enterprise and be mass produced.
Non-newtonian flow posture Na-K alloy electrode of the present invention has high coulombic efficiency, special without dendritic growth and stable structure etc.
Point can be used as potassium metal negative electrode and sodium metal negative electrode simultaneously, when matching with the positive electrodes such as sulphur, Prussian blue, significantly improve complete
The energy density and cyclical stability of battery.
Detailed description of the invention
Fig. 1 is that non-newtonian flow posture Na-K alloy large area prepared by embodiment 1 coats schematic diagram;
Fig. 2 is non-newtonian flow posture Na-K alloy tensile performance test schematic diagram prepared by embodiment 1, (a) in Fig. 2,
(b), (c) shows different tensional states, and wherein the arrow meaning in Fig. 2 in (a) is non-newtonian flow posture Na-K alloy coat;
Fig. 3 is non-newtonian flow posture Na-K alloy electrode dress obtained in common Na-K alloy electrode curve and embodiment 1
At the cyclic curve figure after symmetry electrode.
Specific embodiment
Below with reference to embodiment, the present invention will be described in detail, but the present invention is not limited to this.
Embodiment 1
Under inert gas argon gas shielded, karat gold belongs to and Na metal is using preceding needing to cut removal oxide on surface, by 0.1g
Karat gold belongs to and 0.028g Na metal stacks in glove box, after a period of time reacts, that is, forms liquid Na-K alloy.By 1g grape
Sugar is uniformly mixed with the aqueous solution of 500mL 1% surfactant containing mass percent (sodium alkyl benzene sulfonate), then pours into hydro-thermal tank
In, hydro-thermal 12 hours at 180 DEG C are cleaned and obtain nano carbon microsphere.0.128g liquid Na-K alloy is mixed with 0.5g nano carbon microsphere,
It continues stirring until to form mixture of viscous form, forming non-newtonian flow posture Na-K alloy, (i.e. non-newtonian fluid Na-K alloy is compound
Material), re-coating forms non-newtonian flow posture Na-K alloy coat on copper sheet surface, and non-newtonian flow posture Na-K alloy is made
Electrode.
Non-newtonian flow posture Na-K alloy prepared by embodiment 1 is more sticky, can coat.Fig. 1 is non-ox prepared by embodiment 1
Fluid state Na-K alloy large area of pausing coats schematic diagram, indicates that the alloy can be coated in carrier surface with large area.Fig. 2 is to implement
Non-newtonian flow posture Na-K alloy tensile performance test schematic diagram prepared by example 1 indicates that the alloy has extremely strong stretch-resistance
Energy.
Embodiment 2
Under inert gas argon gas shielded, karat gold belongs to and Na metal is using preceding needing to cut removal oxide on surface, by 0.2g
Karat gold belongs to and 0.056g Na metal stacks in glove box, after a period of time reacts, that is, forms liquid Na-K alloy.By 2.5g bis-
Hydration dichloride copper is uniformly mixed with the aqueous solution of 1000mL 1% surfactant containing mass percent (sodium alkyl benzene sulfonate),
It is poured into hydro-thermal tank again, hydro-thermal 11 hours at 160 DEG C, cleans and obtain cupric oxide nano powder.By 0.256g liquid Na-K alloy with
The mixing of 0.2g cupric oxide nano powder, continues stirring until to form mixture of viscous form, that is, forms non-newtonian flow posture Na-K alloy, then
Coated in carbon cloth surfaces, non-newtonian flow posture Na-K alloy electrode is made.
The performance for obtaining electrode is similar to Example 1.
Embodiment 3
Under inert gas argon gas shielded, karat gold belongs to and Na metal is using preceding needing to cut removal oxide on surface, by 0.2g
Karat gold belongs to and 0.056g Na metal stacks in glove box, after a period of time reacts, that is, forms liquid Na-K alloy.By 1.8g oxygen
SiClx powder is uniformly mixed with the aqueous solution of 1000mL 1% surfactant containing mass percent (sodium alkyl benzene sulfonate), then is fallen
Enter in hydro-thermal tank, hydro-thermal 12 hours at 180 DEG C, cleans and obtain silicon nano power.0.256g liquid Na-K alloy is received with 0.4g silicon
Rice flour mixing, continues stirring until to form mixture of viscous form, that is, forms non-newtonian flow posture Na-K alloy, is coated in plastic foil
Non-newtonian flow posture Na-K alloy electrode is made in surface.
The performance for obtaining electrode is similar to Example 1.
Performance test
By 400 degree of absorption liquid Na-K of non-newtonian flow posture Na-K alloy electrode made of above-described embodiment 1~3 and carbon cloth
For alloy electrode respectively as button cell to electrode and working electrode, electrolyte is 1M KPF6(or 1M NaPF6) electrolyte
In, current density is 1mA cm-2, circulation electricity is 1mAh cm-2, K in symmetry electrode system is measured in 25 ± 1 DEG C of environment
The overpotential of (or Na) metal negative electrode.
The performance test results are as follows:
The Na-K alloy combination electrode of embodiment 1, embodiment 2 and embodiment 3 is in 1mAcm-2360 are recycled under current density
Secondary, overvoltage can be stablized within 15mV, 13mV and 19mV respectively, and voltage platform is stablized, and fluctuate without obvious, and carbon cloth 400
Degree absorption liquid Na-K electrode potential of alloy fluctuation is violent.In addition, the coulombic efficiency that electrode cycle 100 encloses can be respectively maintained at
99.2%, 98.6% and 99.4% or more.As it can be seen that the overvoltage of non-newtonian flow posture Na-K alloy combination electrode obtained above
It is low, good cycling stability, coulombic efficiency height.Non-newtonian flow posture Na-K alloy combination electrode obtained is assembled into embodiment 1
The curve graph under different multiplying after symmetry electrode is as shown in figure 3, common Na-K alloy electrode curve is also as shown in Figure 3.
This is because non-newtonian flow posture Na-K alloy has better rock-steady structure relative to ordinary liquid Na-K alloy,
Maintain liquid without dendrite characteristic while, change the runny property of liquid Na-K alloy, ensure that electrode structure
Stability.
Therefore, non-newtonian flow posture Na-K alloy electrode of the present invention have high coulombic efficiency, significantly inhibit dendritic growth and
The features such as interfacial structure is stablized is of great significance on the metal negative electrode of alkali metal secondary battery is modified, and this method facilitates
Large-scale application without dendrite alkali metal cathode.
Claims (10)
1. a kind of preparation method of non-newtonian flow posture Na-K alloy electrode, which comprises the following steps:
1) under inert gas protection, karat gold is belonged to and Na metal physics stack, karat gold category and the metallic alloying reaction of Na occurs, obtains
Obtain Na-K liquid alloy;
2) under inert gas protection, the liquid Na-K alloy of step 1) preparation and powder granule are mixed, form non-ox
Pause fluid Na-K alloy composite materials, then the material is coated on carrier, forms non-newtonian flow posture Na-K alloy coat, obtains
Non-newtonian fluid Na-K alloy electrode.
2. the preparation method of non-newtonian flow posture Na-K alloy electrode according to claim 1, which is characterized in that step 1)
In, the mass ratio of quality and Na metal that the karat gold belongs to is 70~86:14~30.
3. the preparation method of non-newtonian flow posture Na-K alloy electrode according to claim 2, which is characterized in that step 1)
In, the mass ratio of quality and Na metal that the karat gold belongs to is 75~81:19~25.
4. the preparation method of non-newtonian flow posture Na-K alloy electrode according to claim 3, which is characterized in that step 1)
In, the mass ratio of quality and Na metal that the karat gold belongs to is 77~79:21~23.
5. the preparation method of non-newtonian flow posture Na-K alloy electrode according to claim 1, which is characterized in that step 1)
In, the karat gold belongs to and Na metal is using preceding needing to cut removal oxide on surface.
6. the preparation method of non-newtonian flow posture Na-K alloy electrode according to claim 1, which is characterized in that step 2)
In, the powder granule is nano carbon microsphere, cupric oxide nano powder or silicon nano power.
7. the preparation method of non-newtonian flow posture Na-K alloy electrode according to claim 6, which is characterized in that step 2)
In, the preparation of the nano carbon microsphere includes: to be uniformly mixed glucose with the aqueous solution containing sodium alkyl benzene sulfonate, then pour into water
In hot tank, hydro-thermal 10~14 hours at 170 DEG C~190 DEG C is cleaned and obtains nano carbon microsphere;
The preparation of the cupric oxide nano powder includes: to mix two hydration dichloride copper with the aqueous solution containing sodium alkyl benzene sulfonate
Uniformly, it then pours into hydro-thermal tank, hydro-thermal 9~13 hours at 150 DEG C~170 DEG C, cleans and obtain cupric oxide nano powder;
The preparation of the silicon nano power include: silicon oxide powder is uniformly mixed with the aqueous solution containing sodium alkyl benzene sulfonate, then
It pours into hydro-thermal tank, hydro-thermal 10~14 hours at 170 DEG C~190 DEG C, cleans and obtain silicon nano power.
8. the preparation method of non-newtonian flow posture Na-K alloy electrode according to claim 1, which is characterized in that step 2)
In, the mass ratio of the liquid Na-K alloy and powder granule is 0.1~5:1.
9. the non-newtonian flow posture Na-K alloy electrode of described in any item preparation method preparations according to claim 1~8.
10. non-newtonian flow posture Na-K alloy electrode according to claim 9 is as alkali metal secondary battery negative electrode material
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