CN109755476A - Lithium an- ode and preparation method thereof based on tin oxide cladding three-dimensional conductive skeleton - Google Patents
Lithium an- ode and preparation method thereof based on tin oxide cladding three-dimensional conductive skeleton Download PDFInfo
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- CN109755476A CN109755476A CN201910198171.2A CN201910198171A CN109755476A CN 109755476 A CN109755476 A CN 109755476A CN 201910198171 A CN201910198171 A CN 201910198171A CN 109755476 A CN109755476 A CN 109755476A
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Abstract
The invention discloses a kind of lithium an- ode based on tin oxide cladding three-dimensional conductive skeleton, entire electrode includes the three-dimensional conductive metallic framework and lithium metal of tin oxide cladding；The tin oxide particles for uniformly coating one layer of nano-scale on three-dimensional conductive metallic framework especially by immersion method can make the lithium metal of molten condition equably be adsorbed on the surface of conducting matrix grain since tin oxide is to the compatibility of lithium metal.By adjusting the amount of molten lithium metal, to control the thickness of nickel foam skeleton surface lithium metal layer.The lithium an- ode of three-dimensional conductive skeleton preparation of the present invention, has bigger specific surface area, can not only increase the contact area of metal negative electrode and electrolyte, improve the transmittability of lithium, inhibit the generation of Li dendrite；Lithium can even more be slowed down in the variation of deposition and metal electrode volume during abjection.Preparation process of the present invention is simple, can be mass-produced, and the electrode has fabulous flexibility.
Description
Technical field
The invention belongs to materials and technical field of lithium batteries, more particularly to a kind of tin oxide that is based on to coat three-dimensional conductive skeleton
Lithium an- ode and preparation method thereof.
Background technique
Lithium an- ode has the energy density for outclassing lithium ion battery, and the up to energy density of 3862mAh/g is also
A possibility that lithium-sulfur cell and lithium-air battery of a new generation provide further development.With the play of global energy requirements amount
Increase, and fossil energy is petered out, this all makes energy of development a new generation become a kind of urgent and necessary demand.
Metal lithium electrode results in it and easily reacts simultaneously with electrolyte since it has extremely active chemical property
A kind of unstable solid film is generated, and in metal negative electrode in charge and discharge process repeatedly, this unstable SEI film
It is uneven with abjection to will lead to depositing for lithium, so as to cause the generation of Li dendrite, battery life is caused to decline.In addition, lithium
Dendrite during growth, easily punctures diaphragm paper, and positive and negative anodes is caused directly to contact, and causes battery short circuit, and initiation can not be pre-
The dangerous consequences estimated.These problems whether in secure context or the aspect of performance of battery entirety, all limit electricity of new generation
The development and application of pond device.So, prepare it is a kind of can stable and uniform abjection/deposition lithium an- ode will very great Cheng
Improve the above problem on degree, and the development of new device provides a possibility that bigger.
Currently, existing the relevant technologies trial solves the problem above-mentioned, such as application No. is 201710177007.4 patent public affairs
" a kind of surface treatment method of lithium metal battery cathode " is opened, by constructing one layer of artificial SEI on metal lithium electrode surface
Film with realize lithium uniformly deviate from insertion, reduce the generation of Li dendrite.For another example application No. is 201810292695.3 it is special
Benefit discloses " the modified carbon cloth base lithium of tin oxide and sodium metal negative electrode and preparation method ", has it by strong acid treatment carbon cloth
Hydrophily, then in this, as a conducting matrix grain, to improve metal caused overall structure avalanche during abjection.But
The improvement of artificial SEI film can not be solved these problems perfectly, can only play inhibiting effect, and the effect of carbon cloth skeleton
Though good, cost is excessively high, and acidization reaction is acutely, is not particularly suited for other metallic frameworks.
Summary of the invention
In view of this, the present invention provides one kind to coat three-dimensional conductive based on tin oxide to solve existing technical problem
Lithium an- ode of skeleton and preparation method thereof, this method are avoided strong acid acidization, are not only reduced based on metallic framework
The cost of consumptive material is more that of avoiding the danger of strong acid in experimentation, has good prospects for commercial application.It is with metallic framework
The tin dioxide nano-particle for wrapping up one layer of close lithium by the method for water-bath on it at all constructs a kind of lithium gold of metallic framework
Belong to cathode.This kind of cathode can not only improve metal caused overall structure avalanche during abjection, more can be by artificially controlling
The content of lithium on skeleton obtains the cathode of lithium that capacity can be big.
First aspect present invention provides a kind of preparation of lithium an- ode based on tin oxide cladding three-dimensional conductive skeleton
Method, step include:
(a) it pre-processes: by the cleaning of three-dimensional conductive metallic framework, dry, hydrophilic treated；
(b) stannic acid sodium water solution is prepared；
(c) three-dimensional conductive metallic framework pretreated in (a) is completely soaked stannic acid sodium water solution prepared by (b)
In, carry out water-bath；
(d) the three-dimensional conductive metallic framework after reaction in (c) is washed and dried；
(e) by the desciccate in (d), the high temperature anneal, the three-dimensional that tin oxide cladding is obtained after cooling are led in air
Electric metal skeleton；
(f) under inert gas protection, lithium simple substance is heated to molten condition, and is contacted with products therefrom in (e), make to melt
Melt lithium and be uniformly wrapped on gained three-dimensional conductive metallic framework surface in (e), obtains the three-dimensional coated with tin oxide after cooling completely
Conductive metal is the lithium an- ode of skeleton.
Preferably, in step (a), the 3-dimensional metal conducting matrix grain includes: nickel foam or foam copper.
More preferred, in step (a), the cleaning includes: to carry out ultrasonic cleaning 10-100 respectively with acetone and ethyl alcohol
Minute；The drying includes: to be dried in vacuo 2-12 hours at 50-70 DEG C；The hydrophilic treated includes: with UV ozone or table
Surface plasma cleaning treatment 5-60 minutes.
Preferably, in step (b), the stannic acid sodium water solution is the four hydrated stannic acid sodium water that concentration is 0-5 moles every liter
Solution.The thickness of stannic oxide of concentration and subsequent growth of the sodium stannate is directly related.
More preferred, in step (b), the preparation steps of stannic acid sodium water solution include: by four hydrated stannic acid sodium in 45-60
It stirs 10-30 minutes and is dissolved in the water at DEG C.
Preferably, in step (c), the bath temperature of the water-bath is 60-100 DEG C, and when reaction is 30-150 points a length of
Clock.The hydro-thermal time directly affects the thickness and content of tin oxide.
Specifically, the chemical reaction that water-bath described in step (c) carries out are as follows: Na2Sn(OH)6—2NaOH+Sn
(OH)4。
Preferably, in step (d), the cleaning includes: to be rinsed with deionized water and ethyl alcohol to skeleton obtained by step (c)
It washes.
Preferably, in step (e), the temperature of the high temperature anneal is 372-550 DEG C, and annealing time is 30-200 points
Clock.
Specifically, the chemical reaction carried out under step (e) high temperature are as follows: Sn (OH)4—SnO2+2H2O, gained SnO2To receive
Rice corpuscles.
Preferably, in step (f), the load capacity of lithium metal is 10-100mg/cm2, when load capacity is smaller, formation is
Lithium shell structurre then forms the solid construction of complete wetting when load capacity is larger.The lithium metal and (e) middle gained are three-dimensional
The mass ratio of conductive metal skeleton is 0.02-0.15:0.047.This method is by adjusting three-dimensional conductive metallic framework and lithium metal
Mass ratio realize being precisely controlled for lithium content on skeleton.
More preferred, in step (f), the lithium simple substance is heated to 300-500 DEG C of melting.
More preferred, in step (f), the inert gas is the gas that argon gas etc. is not reacted with lithium.
What second aspect of the present invention provided that above-mentioned preparation method is prepared coats three-dimensional conductive skeleton based on tin oxide
Lithium an- ode, load has lithium metal that lithium metal is made to be uniformly wrapped on the skeleton surface on the stannic oxide.It is specific and
Speech, this programme is different with the structure of lithium load capacity being differently formed, when stannic oxide loads a small amount of lithium, lithium metal
It is uniformly wrapped on the skeleton surface and forms lithium shell, as the content of lithium increases, may eventually form the reality of a complete wetting
Core structure.In 10-100mg/cm2Lithium metal load capacity under obtained lithium shell and solid construction be provided with good effect.
Compared with the prior art, the beneficial effects of the present invention are:
(1) three-dimensional conductive skeleton can improve metal caused overall structure avalanche during abjection；(2) porous knot
Structure can also increase the response area of electrode, and the amount of controllable lithium absorption；(3) metallic framework and traditional carbon cloth skeleton phase
The more cheap cost than having, and in reaction process, directly avoid strong acid reaction；(4) compared with pour lithium slice cathode, the electricity
There is more preferably battery performance in pole, more stably voltage distribution curves；(5) generation of Li dendrite can be inhibited and limit electricity
Volume change of the pole in charge and discharge process.
Detailed description of the invention
Fig. 1 is the surface topography map of the nickel foam metallic framework of tin oxide cladding；
Fig. 2 is that the nickel foam metallic framework of tin oxide cladding adsorbs the surface topography of 20 milligrams of lithium metals every square centimeter
Figure；
Fig. 3 is that the nickel foam metallic framework of tin oxide cladding adsorbs the surface topography of 80 milligrams of lithium metals every square centimeter
Figure；
Fig. 4 is that the nickel foam metallic framework of tin oxide cladding adsorbs 20 milligrams of lithium metals every square centimeter in 1mAh/cm2
Under capacity, 5mAh/g cm2The cycle performance figure of Symmetrical cells under electric current；
Fig. 5 is that the nickel foam metallic framework of tin oxide cladding adsorbs 80 milligrams of lithium metals every square centimeter in 1mAh/cm2
Under capacity, 5mAh/g cm2The cycle performance figure of Symmetrical cells under electric current.
Specific embodiment
To facilitate the understanding of the present invention, present invention work more comprehensively, is meticulously described below in conjunction with embodiment, but this hair
Bright protection scope is not limited to embodiment in detail below.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention, can pass through
Market is commercially available or can be prepared by existing method.
Embodiment 1
This implementation provides a kind of preparation method of lithium an- ode based on tin oxide cladding three-dimensional conductive skeleton, described
Three-dimensional conductive skeleton is nickel foam.
Above-mentioned preparation method includes the following steps: for nickel foam ethyl alcohol acetone to be cleaned by ultrasonic respectively 50 minutes, and 60 is Celsius
It degree lower vacuum drying 12 hours, is handled 30 minutes with UV ozone.Four hydrated stannic acid sodium water solutions of 0.5 gram every milliliter of configuration,
And at 60 c stirring in water bath 15 minutes until being completely dissolved.Nickel foam after hydrophilic treated is completely immersed in four hydration tin
In acid sodium aqueous solution, and 75 degrees Celsius lower stirring in water bath 90 minutes, after reacting completely, take out reaction after nickel foam and
Distribution rinses 3 times in deionized water and ethyl alcohol, is subsequently placed at drying 8 hours under 80 degrees Celsius, and the product after drying uses Muffle
It anneals 150 minutes in 450 degrees Celsius of air of furnace, obtains the foam nickel skeleton of tin oxide cladding, then being prepared diameter is
14 millimeters of circle, with a thickness of 1.6 millimeters.A certain amount of lithium metal is dissolved in argon gas glove box, and is coated using tin oxide
Foam nickel skeleton disk be in contact with it, obtain lithium metal load capacity be 20 milligrams of lithium an- odes every square centimeter.To complete
The three-dimensional conductive metal for obtaining coating using tin oxide after full cooling is the lithium an- ode of skeleton.
Embodiment 2
This implementation provides a kind of preparation method of lithium an- ode based on tin oxide cladding three-dimensional conductive skeleton, described
Three-dimensional conductive skeleton is nickel foam.
Above-mentioned preparation method includes the following steps: for nickel foam ethyl alcohol acetone to be cleaned by ultrasonic respectively 50 minutes, and 60 is Celsius
It degree lower vacuum drying 12 hours, is handled 30 minutes with UV ozone.Four hydrated stannic acid sodium water solutions of 0.75 gram every milliliter of configuration,
And at 60 c stirring in water bath 15 minutes until being completely dissolved.Nickel foam after hydrophilic treated is completely immersed in four hydration tin
In acid sodium aqueous solution, and 70 degrees Celsius lower stirring in water bath 60 minutes, after reacting completely, take out reaction after nickel foam and
Distribution rinses 3 times in deionized water and ethyl alcohol, is subsequently placed at drying 8 hours under 80 degrees Celsius, and the product after drying uses Muffle
It anneals 120 minutes in 450 degrees Celsius of air of furnace, obtains the foam nickel skeleton of tin oxide cladding, then being prepared diameter is
14 millimeters of circle, with a thickness of 1.6 millimeters.A certain amount of lithium metal is dissolved in argon gas glove box, and coated using tin oxide
Foam nickel skeleton disk is in contact with it, and obtaining lithium metal load capacity is 80 milligrams of lithium an- odes every square centimeter.To complete
The three-dimensional conductive metal for obtaining coating using tin oxide after cooling is the lithium an- ode of skeleton.
Embodiment 3
This implementation provides a kind of preparation method of lithium an- ode based on tin oxide cladding three-dimensional conductive skeleton, described
Three-dimensional conductive skeleton is nickel foam.
Above-mentioned preparation method includes the following steps: for foam copper ethyl alcohol acetone to be cleaned by ultrasonic respectively 50 minutes, and 60 is Celsius
It degree lower vacuum drying 12 hours, is handled 30 minutes with UV ozone.Four hydrated stannic acid sodium water solutions of 0.5 gram every milliliter of configuration,
And at 60 c stirring in water bath 15 minutes until being completely dissolved.Foam copper after hydrophilic treated is completely immersed in four hydration tin
In acid sodium aqueous solution, and 75 degrees Celsius lower stirring in water bath 90 minutes, after reacting completely, take out reaction after nickel foam and
Distribution rinses 3 times in deionized water and ethyl alcohol, is subsequently placed at drying 8 hours under 80 degrees Celsius, and the product after drying uses Muffle
It anneals 150 minutes in 450 degrees Celsius of air of furnace, obtains the foam copper skeleton of tin oxide cladding, then being prepared diameter is
14 millimeters of circle, with a thickness of 1.6 millimeters.A certain amount of lithium metal is dissolved in argon gas glove box, and coated using tin oxide
Foam copper skeleton disk is in contact with it, and obtaining lithium metal load capacity is 80 milligrams of lithium an- odes every square centimeter.To complete
The three-dimensional conductive metal for obtaining coating using tin oxide after cooling is the lithium an- ode of skeleton.
Embodiment 4
This implementation provides a kind of preparation method of lithium an- ode based on tin oxide cladding three-dimensional conductive skeleton, described
Three-dimensional conductive skeleton is nickel foam.
Above-mentioned preparation method includes the following steps: for nickel foam ethyl alcohol acetone to be cleaned by ultrasonic respectively 50 minutes, and 60 is Celsius
It degree lower vacuum drying 12 hours, is handled 30 minutes with UV ozone.Four hydrated stannic acid sodium water solutions of 0.5 gram every milliliter of configuration,
And at 60 c stirring in water bath 15 minutes until being completely dissolved.Nickel foam after hydrophilic treated is completely immersed in four hydration tin
In acid sodium aqueous solution, and 75 degrees Celsius lower stirring in water bath 90 minutes, after reacting completely, take out reaction after nickel foam and
Distribution rinses 3 times in deionized water and ethyl alcohol, is subsequently placed at drying 8 hours under 80 degrees Celsius, and the product after drying uses Muffle
It anneals 150 minutes in 450 degrees Celsius of air of furnace, obtains the foam nickel skeleton of tin oxide cladding, surface topography such as 1 institute of attached drawing
Show.The circle that diameter is 14 millimeters is prepared, then with a thickness of 1.6 millimeters.
A certain amount of lithium metal is dissolved in argon gas glove box, and uses the foam nickel skeleton disk of tin oxide cladding and its
Contact, obtaining lithium metal load capacity is 20 milligrams of lithium an- odes every square centimeter.It obtains after cooling down completely with tin oxide
The three-dimensional conductive metal of cladding is the lithium an- ode of skeleton, and surface topography is as shown in Fig. 2.
As a comparison, 0.1 gram of lithium metal, and the foam nickel skeleton coated using tin oxide are dissolved in argon gas glove box
Disk is in contact with it, and obtaining lithium metal load capacity is 80 milligrams of lithium an- odes every square centimeter.It is obtained after cooling down completely
Using the three-dimensional conductive metal of tin oxide cladding as the lithium an- ode of skeleton, surface topography is as shown in Fig. 3.
It is 20mg/cm to lithium metal adsorbance2、80mg/cm2Tin oxide cladding nickel foam metallic framework lithium metal
Cathode carries out electric performance test respectively, and test result difference is as shown in figures 4 and 5.
Although preferred embodiments of the present invention have been described, it is created once a person skilled in the art knows basic
Property concept, then additional changes and modifications may be made to these embodiments.So it includes excellent that the following claims are intended to be interpreted as
It selects embodiment and falls into all change and modification of the scope of the invention.Obviously, those skilled in the art can be to the present invention
Carry out various modification and variations without departing from the spirit and scope of the present invention.If in this way, these modifications and changes of the present invention
Within the scope of the claims of the present invention and its equivalent technology, then the present invention is also intended to encompass these modification and variations and exists
It is interior.
Claims (10)
1. a kind of preparation method of the lithium an- ode based on tin oxide cladding three-dimensional conductive skeleton, step include:
(a) it pre-processes: by the cleaning of three-dimensional conductive metallic framework, dry, hydrophilic treated；
(b) stannic acid sodium water solution is prepared；
(c) three-dimensional conductive metallic framework pretreated in (a) is completely soaked in stannic acid sodium water solution prepared by (b),
Carry out water-bath；
(d) the three-dimensional conductive metallic framework after reaction in (c) is washed and dried；
(e) by the desciccate in (d), the high temperature anneal, the three-dimensional conductive that tin oxide cladding is obtained after cooling are golden in air
Belong to skeleton；
(f) under inert gas protection, lithium simple substance is heated to molten condition, and is contacted with products therefrom in (e), make molten lithium
It is uniformly wrapped on gained three-dimensional conductive metallic framework surface in (e), obtains the three-dimensional conductive coated with tin oxide after cooling completely
Metal is the lithium an- ode of skeleton.
2. the preparation method of the lithium an- ode according to claim 1 based on tin oxide cladding three-dimensional conductive skeleton,
Be characterized in that: in step (a), the 3-dimensional metal conducting matrix grain includes: nickel foam or foam copper.
3. the preparation method of the lithium an- ode according to claim 1 or 2 based on tin oxide cladding three-dimensional conductive skeleton,
It is characterized by: the cleaning includes: to carry out ultrasonic cleaning 10-100 minutes respectively with acetone and ethyl alcohol in step (a)；It is described
Drying includes: to be dried in vacuo 2-12 hours at 50-70 DEG C；The hydrophilic treated includes: with UV ozone or surface plasma
Body cleaning treatment 5-60 minutes.
4. the preparation method of the lithium an- ode according to claim 1 based on tin oxide cladding three-dimensional conductive skeleton,
Be characterized in that: in step (b), the stannic acid sodium water solution is the four hydrated stannic acid sodium water solutions that concentration is 0-5 moles every liter.
5. the preparation method of the lithium an- ode according to claim 4 based on tin oxide cladding three-dimensional conductive skeleton,
Be characterized in that: in step (b), the preparation steps of stannic acid sodium water solution include: to stir four hydrated stannic acid sodium at 45-60 DEG C
It is dissolved in the water within 10-30 minutes.
6. the preparation method of the lithium an- ode according to claim 1 based on tin oxide cladding three-dimensional conductive skeleton,
Be characterized in that: in step (c), the bath temperature of the water-bath is 60-100 DEG C, and when reaction is 30-150 minutes a length of.
7. the preparation method of the lithium an- ode according to claim 1 based on tin oxide cladding three-dimensional conductive skeleton,
Be characterized in that: in step (e), the temperature of the high temperature anneal is 372-550 DEG C, and annealing time is 30-200 minutes.
8. the preparation method of the lithium an- ode according to claim 1 based on tin oxide cladding three-dimensional conductive skeleton,
Be characterized in that: in step (f), the lithium metal load capacity is 10-100mg/cm2。
9. the preparation method of the lithium an- ode according to claim 8 based on tin oxide cladding three-dimensional conductive skeleton,
Be characterized in that: in step (f), the lithium simple substance is heated to 300-500 DEG C of melting.
10. the lithium an- ode based on tin oxide cladding three-dimensional conductive skeleton that preparation method described in claim 1 is prepared,
It is characterized by: the lithium an- ode is coated with the three-dimensional conductive metal of tin dioxide nano-particle as skeleton using surface, institute
Stating carried metal lithium on stannic oxide makes lithium metal be uniformly wrapped on the skeleton surface.
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Cited By (8)
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| CN110212200A (en) * | 2019-05-30 | 2019-09-06 | 江汉大学 | A kind of battery, compound cathode of lithium and preparation method thereof |
| CN110212199A (en) * | 2019-05-30 | 2019-09-06 | 江汉大学 | A kind of conducting matrix grain and preparation method thereof |
| CN111430660A (en) * | 2020-03-19 | 2020-07-17 | 浙江大学 | Ion-electron mixed conductive metal sodium cathode and preparation method thereof |
| CN111599983A (en) * | 2020-05-18 | 2020-08-28 | 中山大学 | Lithium metal composite negative electrode with hydrophilic-hydrophobic lithium gradient structure and preparation method thereof |
| CN112103472A (en) * | 2019-06-17 | 2020-12-18 | 上海汽车集团股份有限公司 | Metal lithium composite material and preparation method thereof |
| CN112447979A (en) * | 2019-08-30 | 2021-03-05 | 广州汽车集团股份有限公司 | Porous current collector and preparation method thereof, lithium negative electrode and lithium ion battery |
| CN112909229A (en) * | 2021-01-19 | 2021-06-04 | 南昌大学 | Silver coating method of three-dimensional lithium-philic metal foam framework and preparation method of application of silver coating method in lithium metal negative electrode |
| CN113036100A (en) * | 2021-02-25 | 2021-06-25 | 浙江大学 | Lithium metal composite negative electrode containing rigid particle framework and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112447979A (en) * | 2019-08-30 | 2021-03-05 | 广州汽车集团股份有限公司 | Porous current collector and preparation method thereof, lithium negative electrode and lithium ion battery |
| CN111430660A (en) * | 2020-03-19 | 2020-07-17 | 浙江大学 | Ion-electron mixed conductive metal sodium cathode and preparation method thereof |
| CN111599983A (en) * | 2020-05-18 | 2020-08-28 | 中山大学 | Lithium metal composite negative electrode with hydrophilic-hydrophobic lithium gradient structure and preparation method thereof |
| CN112909229A (en) * | 2021-01-19 | 2021-06-04 | 南昌大学 | Silver coating method of three-dimensional lithium-philic metal foam framework and preparation method of application of silver coating method in lithium metal negative electrode |
| CN113036100A (en) * | 2021-02-25 | 2021-06-25 | 浙江大学 | Lithium metal composite negative electrode containing rigid particle framework and preparation method thereof |
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Application publication date: 20190514 |
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