CN109638271A - A kind of preparation method and lithium battery of lithium battery - Google Patents
A kind of preparation method and lithium battery of lithium battery Download PDFInfo
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- CN109638271A CN109638271A CN201811306676.8A CN201811306676A CN109638271A CN 109638271 A CN109638271 A CN 109638271A CN 201811306676 A CN201811306676 A CN 201811306676A CN 109638271 A CN109638271 A CN 109638271A
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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
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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
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
- H01M10/058—Construction or manufacture
-
- 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
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The present invention provides a kind of preparation method of lithium battery and lithium batteries, preparation method includes the steps that adding black phosphorus to the cathode of lithium battery, wherein, the step of adding black phosphorus to the cathode of lithium battery includes: step 1, the black phosphorus powder of predetermined weight is put into container, and dispersing agent is added thereto, obtain black phosphorus mixed liquor, then black phosphorus mixed liquor is poured into ultrasonic agitation machine, carry out the stirring operation of the first scheduled duration to black phosphorus mixed liquor according to the first mixing parametric using ultrasonic agitation machine, obtain black phosphorus solution, to effectively improve the chemical property of lithium ion battery, under equal conditions, black phosphorus is used to compare the negative electrode material for using graphite as lithium ion battery as the negative electrode material of lithium ion battery, more lithium ions can be embedded in battery, effectively improve the energy density of battery and the stability of electrolyte, it improves The cycle performance of battery is suitble to large-scale promotion to use.
Description
Technical field
The present invention relates to battery technology fields, and in particular to a kind of preparation method and lithium battery of lithium battery.
Background technique
Lithium ion battery has many advantages, such as that energy density is high, has extended cycle life, is environmentally friendly, therefore, not only in 3C
Digital domain is applied widely, and is also developed rapidly in electric automobiles in recent years.
Lithium ion battery generally comprises the major parts such as positive plate, negative electrode tab, diaphragm, electrolyte.Currently, graphite is extensive
Cathode material as lithium ion battery, but actively seek the alternative solution of higher capacity.Have in the prior art
Some cathode materials that can substitute graphite as lithium ion battery, for example, having many oxide, Si bases of the research based on Sn
The materials such as composite material, transition metal oxide, metal nitride and metal phosphide, research find above-mentioned material can with it is every
Reversible reaction occurs for a a large amount of Li of formula unit, is supplied to cathode materials for lithium battery as a result, and more selects.
But there are some problems in above-mentioned material, for example, although the system based on alloy is with higher during the test
Energy density, but due to during charge or discharge above-mentioned material biggish volume change can occur, use above-mentioned material
The holding capacity of the capacity of battery when using as cathode is poor, is unable to satisfy actual use demand.
In these above-mentioned material systems, commercially available phosphorus and transition metal are used to synthesis metal phosphide, but due to
The transition metal that weight has been used in above-mentioned material, causes the energy density of material to reduce.
Summary of the invention
In view of this, one of the objects of the present invention is to provide a kind of preparation method of lithium battery and lithium battery, to solve
Lithium battery existing in the prior art uses negative electrode material of the graphite as lithium battery, and it is bad that there are stable electrochemical properties,
The capacity of battery constantly declines in battery use process, until the problem of performance completely loses is recycled.
In order to achieve the above objectives, on the one hand, the invention adopts the following technical scheme:
A kind of preparation method of lithium battery, the preparation method include the step to the cathode of lithium battery addition black phosphorus
Suddenly, wherein the cathode of Xiang Suoshu lithium battery adds the step of black phosphorus and includes:
Step 1: the black phosphorus powder of predetermined weight is put into container, and dispersing agent is added thereto, obtains black phosphorus mixing
Liquid then pours into the black phosphorus mixed liquor in ultrasonic agitation machine, using the ultrasonic agitation machine according to the first mixing parametric pair
The black phosphorus mixed liquor carries out the stirring operation of the first scheduled duration, obtains black phosphorus solution.
Preferably, the dispersing agent includes N-Methyl pyrrolidone；And/or
First predetermined weight is 1 to 20g；And/or
First mixing parametric is 500 to 20000r/min；And/or
First scheduled duration is 1 to 10h.
Preferably, the preparation method further include:
Step 2: being put into the black phosphorus solution into vacuum oven, it is predetermined that second is carried out under the first predetermined temperature
The drying process of duration removes the dispersing agent in the black phosphorus solution, obtains dried powder.
Preferably, first predetermined temperature is 40 to 120 DEG C；And/or
Second scheduled duration is 3 to 10 hours.
Preferably, the preparation method further include:
Step 3: taking the dried powder obtained in the step 2 and conductive agent and adhesive with the first predetermined ratio
It is matched, and it is mixed with the solvent of the first predetermined volume of the first predetermined concentration, protected in magnetic stirring apparatus
The stirring that the second predetermined temperature carries out third scheduled duration is held, to obtain the uniform sizing material without precipitating.
Preferably, first predetermined ratio is weight ratio 69:20:10, alternatively, first predetermined ratio is weight ratio
79:10:10；And/or
First predetermined concentration is 1% to 2%；And/or
First predetermined volume is 2 to 10ml；And/or
Second predetermined temperature is 30 to 65 DEG C；And/or
The third scheduled duration is 30 to 100 minutes.
Preferably, the preparation method further include Step 4:
Slurry obtained in the step 3 is uniformly applied on the copper foil used as electrode film, the density of coating is
1 to 5mg/cm2。
Preferably, the preparation method further include:
Kept for 80 to 250 DEG C Step 5: the electrode film for being coated with the slurry in the step 4 is put into drying box
At a temperature of dry 1 to 20h, then 50 to 150 DEG C at a temperature of dry 1 to 20h, then apply 1 on the electrode film
To the pressure of 10MPa.
Preferably, the preparation method further include:
Step 6: using lithium metal as anode, uses the above-mentioned electrode film coated with the slurry as cathode, use
Ethylene carbonate, dimethyl carbonate, diethyl carbonate, propene carbonate carry out mixing as electricity according to the volume ratio of 1:1:1:1
Liquid is solved, fits together to form battery in environment under argon gas state.
In order to achieve the above object, on the other hand, the invention adopts the following technical scheme:
A kind of lithium battery, the battery are made of the preparation method of lithium battery as described above.
Lithium battery in the application uses black phosphorus to replace negative electrode material of the graphite as lithium ion battery, can effectively avoid
Destruction of the propene carbonate to cathode graphite in electrolyte, so that the chemical property of lithium ion battery is effectively improved, same
Deng under the conditions of, black phosphorus is used to compare the cathode material for using graphite as lithium ion battery as the negative electrode material of lithium ion battery
Expect, more lithium ions can be embedded in battery, the energy density of battery and the stability of electrolyte is effectively improved, improve electricity
The cycle performance in pond is suitble to large-scale promotion to use.
Detailed description of the invention
By referring to the drawings to the description of the embodiment of the present invention, the above and other purposes of the present invention, feature and
Advantage will be apparent from, in the accompanying drawings:
Fig. 1 shows the flow chart of the preparation method of the lithium battery of specific embodiment of the invention offer；
After the black phosphorus solution obtained in the step of Fig. 2 shows specific embodiment of the invention offers one is ultrasonically treated
Figure under scanning electron microscope；
Fig. 3 shows the black phosphorus solution obtained in the step of specific embodiment of the invention provides one by projection Electronic Speculum point
The image obtained after analysis.
Specific embodiment
Below based on embodiment, present invention is described, it should be understood by one skilled in the art that provided herein
Attached drawing is provided to the purpose of explanation, and attached drawing is not necessarily drawn to scale.
Unless the context clearly requires otherwise, "include", "comprise" otherwise throughout the specification and claims etc. are similar
Word should be construed as the meaning for including rather than exclusive or exhaustive meaning；That is, be " including but not limited to " contains
Justice.
Present applicant proposes a kind of preparation methods of lithium ion battery, and black phosphorus is used to replace existing graphite as lithium ion
The negative electrode material of battery, to improve the chemical property and energy density of lithium ion battery, when extending the use of lithium ion battery
It is long.
As shown in Figure 1, preparation method includes the cathode to lithium battery this application provides a kind of preparation method of lithium battery
The step of adding black phosphorus.Specifically, to the cathode of lithium battery add black phosphorus the step of the following steps are included:
Step 1: the black phosphorus powder of predetermined weight is put into container, and dispersing agent is added thereto, obtains black phosphorus mixing
Liquid then pours into black phosphorus mixed liquor in ultrasonic agitation machine, is mixed according to the first mixing parametric to black phosphorus using ultrasonic agitation machine
Liquid carries out the stirring operation of the first scheduled duration, obtains black phosphorus solution.Container is according to the weight of black phosphorus powder, and the lithium of preparation
The volume of ion battery is determined, and when preparing lithium ion button shape cell, selects beaker, the volume of beaker can be
100ml, 200ml, 300ml or 500ml.Wherein, dispersing agent includes N-Methyl pyrrolidone, the first predetermined weight be 1 to
20g, the first mixing parametric are 500 to 20000r/min, and the first scheduled duration is 1 to 10h.Preferably, the type of machine is stirred by ultrasonic
Number be JY-Y202G, to guarantee mixing effect.
It in order to which the chemistry to black phosphorus solution newly can be carried out analysis, needs to observe its form after handling it, take a small amount of
The black phosphorus solution obtained in step 1 is put it into 5 into 20ml volumetric flask, using FS-1500T processor for ultrasonic wave to it
1 to 100 minute ultrasonication is carried out, it is to be processed to complete or solution is analyzed using scanning electron microscope, as shown in Fig. 2,
Be one the step of being observed under scanning electron microscope in black phosphorus solution be ultrasonically treated device treated image.In addition, also
It to be analyzed it using transmission electron microscope, as shown in figure 3, being that black phosphorus solution of the step in is ultrasonically treated device processing
The image observed afterwards in the case where projecting Electronic Speculum.Wherein, the running parameter of processor for ultrasonic wave is, device working efficiency be 50 to
1200W, working frequency are 5 to 20KHz, and regulation rate is 10% to 80%, the progressive speed of the regulation rate during ultrasonication
Rate is 1%.During ultrasonication, the temperature inside processor for ultrasonic wave is -30 to -300 DEG C, warm during processing
Degree constantly variation, change rate are 1 DEG C of variation every time.Processor for ultrasonic wave includes random probe, and the head diameter popped one's head at random is
20mm, the treating capacity of processor for ultrasonic wave are 50 to 2000ml, and the total length of processor for ultrasonic wave inner space is 139mm, whole
Body weight is 450g.
Further, preparation method further include:
Step 2: being put into black phosphorus solution into vacuum oven, the second scheduled duration is carried out under the first predetermined temperature
Drying process, by black phosphorus solution dispersing agent remove, obtain dried powder.Wherein, the first predetermined temperature is 40 to 120
DEG C, the second scheduled duration is 3 to 10 hours.
In order to need to be made by black phosphorus to using electrochemistry of the black phosphorus as the lithium ion battery of cathode to can be carried out test
It is fabricated to complete battery for the lithium ion battery of cathode, then chemical property is measured, preparation method further include:
Step 3: taking the dried powder obtained in step 2 and conductive agent and adhesive with the progress of the first predetermined ratio
Proportion, and it is mixed with the solvent of the first predetermined volume of the first predetermined concentration, and the is kept in magnetic stirring apparatus
Two predetermined temperatures carry out the stirring of third scheduled duration, to obtain the uniform sizing material without precipitating.
Wherein, while the dried powder obtained in adding step 2, it is also necessary to which addition is used as active material thereto
The BP used.Carbon black can be used in above-mentioned conductive agent, and polyvinylidene fluoride or PVDF can be used in adhesive.In use process
In, it is mixed between active material, conductive agent and binder according to weight ratio for the first predetermined ratio, the first predetermined ratio is
69:20:10, alternatively, the first predetermined ratio is that 79:10:10 makes when being designed to the first predetermined ratio according to different
It is adjusted correspondingly with situation, as long as can guarantee the chemical property of battery.In step 3, N- methyl pyrrole is used
Pyrrolidone is as solvent, and the concentration of solvent is that the first predetermined concentration mixes above-mentioned each substance, wherein the first predetermined concentration
It is 1% to 2%, the first predetermined volume is 2 to 10ml.Mixed solution is added to be stirred in magnetic stirring apparatus when,
Two predetermined temperatures are 30 to 65 DEG C, and third scheduled duration is 30 to 100 minutes.It is completed by above-mentioned magnetic stirrer
Afterwards, slurry is in uniformly without the state of precipitating, to guarantee in the next steps to the reliability in cell manufacturing process, the electricity of battery
Chemical property is more preferable.
Further, preparation method further include:
Step 4: being uniformly applied to slurry obtained in step 3 on the copper foil used as electrode film, coating it is close
Degree is 1 to 5mg/cm2.Wherein, the area of the copper foil used as electrode film is 0.75 to 2.5cm2, the area of the copper foil is root
It is determined according to the use environment of battery and the volume of battery, when the volume difference of battery, the area for the copper foil that device uses
Also different, to guarantee the reliability of electrode film in use, and further increase the chemical property of battery.
Further, preparation method further include:
It is kept at a temperature of 80 to 250 DEG C Step 5: the electrode film for being coated with slurry in step 4 is put into drying box
Dry 1 to 20h, then in 50 to 150 DEG C of at a temperature of drying 1 to 20h, then apply 1 to 10MPa pressure on electrode film
Power.By applying pressure on electrode film, slurry can be effectively avoided to fall off from motor film, the electrochemistry for influencing battery uses
Performance.
Further, preparation method further include:
Step 6: using lithium metal as anode, uses the above-mentioned electrode film coated with slurry as cathode, use carbonic acid
Ethyl, dimethyl carbonate, diethyl carbonate, propene carbonate carry out mixing according to the volume ratio of 1:1:1:1 and are used as electrolyte,
It fits together to form battery in environment under argon gas state.It in this step, is round by the battery made in this present embodiment
The button cell of shape, therefore use circular lithium metal as to motor, use Celgard 2400 as diaphragm, is full of argon gas
Environment in preferably full of argon gas glove box in above-mentioned circular motor is fitted into button cell, wherein button cell
Model CR2032.
The above-mentioned button cell made is carried out in test process using test macro, it is close in long circulating charge-discharge test
Degree is 500mAg-1, recycle under the test condition that 800 enclose, obtain following test result: discharge capacity is battery for the first time
2100mAhg-1, initial charge capacity is 1300mAhg-1, by above-mentioned numerical value it is found that using black phosphorus as the electricity of battery cathode
The stability in pond and the capability value of battery are all much better than the battery for using graphite as cathode.
PC (propene carbonate) in electrolyte is largely decomposed on graphite electrode, and is embedded in graphite together with lithium ion
Layer, causes graphite completely peeled off, so that the decline of graphite electrode reversible capacity or even cycle performance be caused to completely lose.And this Shen
Please in lithium ion battery preparation method, above-mentioned motor will not be occurred and exist by using black phosphorus to use as the cathode of lithium ion battery
The case where largely decomposing in point solution liquid appearance, therefore, lithium ion battery when doing cathode using black phosphorus has more stable follow
Ring stability.
Present invention also provides a kind of lithium battery, which uses the preparation method such as above-mentioned lithium battery to be made.
Lithium battery uses negative electrode material of the black phosphorus as lithium ion battery, black phosphorus and graphite laminate structure phase in the application
Seemingly, the black phosphorus performance of sheet is close to graphene, using the characteristic of black phosphorus mobility with higher, make it through it is compound with silicon,
The immigration load of silicon is reduced, further ternary lithium cell cathode material is formed with liquid metals such as gallium niobiums, can effectively inhibit
The volume expansion of silicon, under equal conditions, to be embedded in more lithium ion, improve the energy density of battery and to the steady of electrolyte
It is qualitative, improve the cycle performance of battery.
Those skilled in the art will readily recognize that above-mentioned each preferred embodiment can be free under the premise of not conflicting
Ground combination, superposition.
The above is only a preferred embodiment of the present invention, is not intended to restrict the invention, to those skilled in the art,
The invention can have various changes and changes.It is all within the spirit and principles of the present invention made by any modification, equivalent replacement,
Improve etc., it should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of lithium battery, which is characterized in that the preparation method includes adding to the cathode of the lithium battery
The step of black phosphorus, wherein the cathode of Xiang Suoshu lithium battery adds the step of black phosphorus and includes:
Step 1: the black phosphorus powder of predetermined weight is put into container, and dispersing agent is added thereto, obtains black phosphorus mixed liquor,
Then the black phosphorus mixed liquor is poured into ultrasonic agitation machine, using the ultrasonic agitation machine according to the first mixing parametric to described
Black phosphorus mixed liquor carries out the stirring operation of the first scheduled duration, obtains black phosphorus solution.
2. the preparation method of lithium battery according to claim 1, which is characterized in that the dispersing agent includes N- methylpyrrole
Alkanone；And/or
First predetermined weight is 1 to 20g；And/or
First mixing parametric is 500 to 20000r/min；And/or
First scheduled duration is 1 to 10h.
3. the preparation method of lithium battery according to claim 1, which is characterized in that the preparation method further include:
Step 2: being put into the black phosphorus solution into vacuum oven, the second scheduled duration is carried out under the first predetermined temperature
Drying process, by the black phosphorus solution the dispersing agent remove, obtain dried powder.
4. the preparation method of lithium battery according to claim 3, which is characterized in that first predetermined temperature be 40 to
120℃；And/or
Second scheduled duration is 3 to 10 hours.
5. the preparation method of lithium battery according to claim 3, which is characterized in that the preparation method further include:
Step 3: taking the dried powder obtained in the step 2 and conductive agent and adhesive with the progress of the first predetermined ratio
Proportion, and it is mixed with the solvent of the first predetermined volume of the first predetermined concentration, and the is kept in magnetic stirring apparatus
Two predetermined temperatures carry out the stirring of third scheduled duration, to obtain the uniform sizing material without precipitating.
6. the preparation method of lithium battery according to claim 5, which is characterized in that first predetermined ratio is weight ratio
69:20:10, alternatively, first predetermined ratio is weight ratio 79:10:10；And/or
First predetermined concentration is 1% to 2%；And/or
First predetermined volume is 2 to 10ml；And/or
Second predetermined temperature is 30 to 65 DEG C；And/or
The third scheduled duration is 30 to 100 minutes.
7. the preparation method of lithium battery according to claim 5, which is characterized in that the preparation method further includes step
Four,
Slurry obtained in the step 3 is uniformly applied on the copper foil used as electrode film, the density of coating be 1 to
5mg/cm2。
8. the preparation method of lithium battery according to claim 7, which is characterized in that the preparation method further include:
Step 5: the electrode film for being coated with the slurry in the step 4 to be put into the temperature of 80 to 250 DEG C of holding in drying box
Degree lower dry 1 to 20h, then 50 to 150 DEG C at a temperature of dry 1 to 20h, then apply on the electrode film 1 to
The pressure of 10MPa.
9. the preparation method of lithium battery according to claim 8, which is characterized in that the preparation method further include:
Step 6: using lithium metal as anode, uses the above-mentioned electrode film coated with the slurry as cathode, use carbonic acid
Ethyl, dimethyl carbonate, diethyl carbonate, propene carbonate carry out mixing according to the volume ratio of 1:1:1:1 and are used as electrolyte,
It fits together to form battery in environment under argon gas state.
10. a kind of lithium battery, which is characterized in that the battery uses the preparation of the lithium battery as described in one of claim 1 to 9
Method is made.
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