CN102354759A - Lithium negative pole, preparation method thereof and battery comprising lithium negative pole - Google Patents
Lithium negative pole, preparation method thereof and battery comprising lithium negative pole Download PDFInfo
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- CN102354759A CN102354759A CN2011103452346A CN201110345234A CN102354759A CN 102354759 A CN102354759 A CN 102354759A CN 2011103452346 A CN2011103452346 A CN 2011103452346A CN 201110345234 A CN201110345234 A CN 201110345234A CN 102354759 A CN102354759 A CN 102354759A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a lithium negative pole, a preparation method thereof and a battery comprising the lithium negative pole. The preparation method of the lithium negative pole comprises the following specific steps: step 1, lithium embedding: coating a carbon material on an affluxion body Cu foil and drying, thereby obtaining a carbon material pole piece; packing a battery by taking a lithium metal piece as a negative pole and the carbon material pole piece as a counter electrode, carrying out charge-discharge circulation so as to finish the step of lithium embedding; and step2,deposition of a metal lithium layer through overdischarge: carrying out overdischarge on the finished embedding lithium step battery at current density of 10-100 m A/g through constant current discharging for 2-20 hours, thus the lithium negative pole is obtained on a carbon material pole piece surface electrochemical deposition lithium metal layer. The lithium negative pole provided by the invention has the advantages of taking a carbon electrode as a carrier; compared with a general lithium metal negative pole, the safety feature and the cycle performance are effectively improved, the negative pole capacity can be designed by self according to the requirements of the positive pole capacity, therefore the adjustable range is large.
Description
Technical field
The invention belongs to field of electrochemical batteries, relate to a kind of lithium secondary battery, be specifically related to a kind of cathode of lithium, its preparation method and comprise the battery of this cathode of lithium.
Background technology
Lithium metal relative standard hydrogen electrode electromotive force is-3.045 V, and specific capacity is 3861 mAh/g 10 times near conventional carbon negative pole specific capacity (graphite is 372 mAh/g), and good development prospect is arranged.But cathode of lithium constantly dissolves in charge and discharge process, deposits, and be prone to produce dendrite, causes cycle performance to descend, and dendrite can diaphragm contacts with positive pole and cause internal short-circuit when serious, even takes place on fire or security incident such as blast.
For cycle performance and the security performance of improving lithium anode; Major measure has: in electrolyte, add additive for improving cathode of lithium surface SEI film (solid electrolyte interface film; Solid electrolyte interface is called for short the SEI film) composition, in advance cathode of lithium surface deposition one deck passivation layer as the SEI film, use novel lithium electrode.And novel lithium electrode mainly contains alloy electrode, lithium powder electrode etc.
K. Chung etc. adopt the RF magnetron sputtering at the cathode of lithium surface deposition one deck LiPON film as the SEI film.Also have C
60Be deposited on and improve inhibition dendritic growth in cathode of lithium surface on the lithium surface.But these method costs are high, troublesome poeration.
The patent of FMC Corp. is mentioned and is used the lithium powder as electrode, and the lithium powder is depressed to pole piece at certain pressure, because the lithium powder particles is little, specific area is big, can suppress dendritic growth.But when discharge electricity amount is big, lithium powder electrode surface morphology change is very big, and promptly cycle performance can descend.
Therefore, it is low to need a kind of cost of exploitation badly, and the preparation method of cathode of lithium easy and simple to handle is with cycle performance and the security performance of improving cathode of lithium.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of secondary lithium batteries cathode of lithium; Through using carbon electrode to be carrier, behind its complete embedding lithium, again at its surface electrochemistry lithium deposition layer; Use these lithium sources, thereby avoid the use of the safety issue that the excess metal lithium brings.
For realizing above purpose, the invention provides a kind of preparation method of cathode of lithium, this method comprises following concrete steps:
Step 1, the embedding lithium: material with carbon element is coated on the collector Cu paper tinsel, and oven dry obtains the material with carbon element pole piece; With the metal lithium sheet is negative pole, and described material with carbon element pole piece is to electrode, and charge and discharge cycles is carried out in assembled battery, makes lithium ion evenly be embedded in the material with carbon element, accomplishes embedding lithium step;
Step 2, overdischarge plated metal lithium layer: with the battery of above-mentioned completion embedding lithium step, under 10-100 mA/g current density, constant-current discharge 2-20 h carries out overdischarge, at material with carbon element pole piece surface electrochemistry plated metal lithium layer, obtains cathode of lithium.
The preparation method of above-mentioned cathode of lithium, wherein, described material with carbon element comprises: more than any one in MCMB, hard carbon, graphite, the Graphene.
The preparation method of cathode of lithium of the present invention be with material with carbon element as carrier, behind the embedding lithium, carry out overdischarge again, obtain at its surface electrochemistry plated metal lithium layer.The amount of electrochemical deposition lithium can design (negative pole design capacity excessive about 100%) voluntarily according to anodal demand.This type of cathode of lithium can be formed battery with poor lithium anode material.
The material with carbon element electrode is porous state, is carrier with it, and is bigger in the specific area of its surface electrochemistry precipitated lithium metal layer, under identical electric current, can reduce the current density (mA/cm of electrode
2), reduce the probability that dendrite forms; And the lithium electrode that the present invention prepares is in charge and discharge process, and the dissolving of the deposition of lithium can be carried out in porous carbon electrodes, reduces the probability that dendrite forms, thereby improves the security performance and the cycle performance of battery.
The cathode of lithium that the present invention also provides said method to make, this cathode of lithium be with the Cu paper tinsel as collector, material with carbon element is coated on the collector Cu paper tinsel as carrier, embeds lithium ion in carrier inside, forms at the surface deposition lithium metal layer of carrier; This cathode of lithium has higher specific capacity.
The present invention also provides a kind of battery that comprises the cathode of lithium that said method makes, and this battery comprises above-mentioned cathode of lithium and poor lithium anode material, and this cycle performance of battery is good, and fail safe is good.
Above-mentioned battery, wherein, more than any one in described poor lithium anode material selection lithium titanate, elemental sulfur, elemental sulfur/carbon material compound, the sulfur-based compound.
Cathode of lithium proposed by the invention is to use carbon electrode to be carrier, with the common metal cathode of lithium relatively, security performance and cycle performance be effectively improvement all, and capacity of negative plates can design according to the positive electrode capacity demand voluntarily, adjustable extent is big.
Description of drawings
Fig. 1 prepares the process sketch map for cathode of lithium of the present invention, and step 1 is a material with carbon element embedding lithium process, when the embedding lithium is accomplished, carry out step 2, i.e. overdischarge plated metal lithium layer.
Fig. 2 takes off the lithium curve for cathode of lithium of the present invention, is to electrode with the lithium electrode of preparing, and the nickel sheet is anodal, charges to 3 V, and the capacity that obtains is the capacity of lithium electrode.
Fig. 3 is lithium in the embodiment of the invention 5/lithium titanate system first charge-discharge curve.
Fig. 4 is the cycle performance figure of lithium in the embodiment of the invention 5/lithium titanate system.
Embodiment
Do explanation further below in conjunction with embodiment and accompanying drawing specific embodiments of the invention.
As shown in Figure 1, the preparation method of cathode of lithium provided by the invention comprises:
Step 1, the embedding lithium: material with carbon element 2 is uniformly coated on the collector 1, and oven dry obtains the material with carbon element pole piece; With the metal lithium sheet is negative pole, and described material with carbon element pole piece is to electrode, and charge and discharge cycles is carried out in assembled battery, makes lithium ion 3 evenly be embedded in the material with carbon element 2, accomplishes embedding lithium step;
Step 2, overdischarge plated metal lithium layer 4: with the battery of above-mentioned completion embedding lithium step, under 10-100 mA/g current density, constant-current discharge 2-20 h carries out overdischarge, at material with carbon element pole piece surface electrochemistry plated metal lithium layer 4, obtains cathode of lithium.
Embodiment 1
With carbonaceous mesophase spherules (MCMB) is the lithium carrier; Mix by mass ratio 91:3:6 with conductive agent carbon black (SP), binding agent Kynoar (PVDF); With N-N-methyl-2-2-pyrrolidone N-(NMP) is solvent; With being uniformly coated on behind the high-speed emulsifying machine mixing pulping on the collector Cu paper tinsel; Oven dry 24 h in 60 ℃ vacuum drying chamber are subsequent use then.With the metal lithium sheet is negative pole, and MCMB is to electrode, and Celgrad 2325 is a barrier film, 1.2 mol/L lithium hexafluoro phosphate (LiPF
6The basic carbonic ester of)/ethylene carbonate (EC)+first and second (EMC) (volume ratio is 3:7) is assembled into battery for electrolyte.
Battery at first carries out charge and discharge cycles with the current density of 40 mA/g, and voltage range is 0-3 V.Behind circulation 10 circles, be discharged to 0 V again, and then with current density constant-current discharge 9 h of 40 mA/g, at MCMB pole piece surface electrochemistry plated metal lithium layer, the cathode of lithium capacity that obtains is 5.36 mAh, capacity is very little, and is seldom excessive, i.e. fail safe is good.
Embodiment 2
With graphite (MCP-1) is the lithium carrier; Mix by mass ratio 91:3:6 with conductive agent carbon black (SP), binding agent Kynoar (PVDF); With N-N-methyl-2-2-pyrrolidone N-(NMP) is solvent; With being uniformly coated on behind the high-speed emulsifying machine mixing pulping on the collector Cu paper tinsel; Oven dry 24 h in 60 ℃ vacuum drying chamber are subsequent use then.With the metal lithium sheet is negative pole, and graphite is to electrode, and Celgrad 2325 is a barrier film, 1.2 mol/L lithium hexafluoro phosphate (LiPF
6(volume ratio is 3:7)+(FEC 5wt%) is assembled into battery for electrolyte to fluorinated ethylene carbonate to the basic carbonic ester of)/ethylene carbonate (EC)+first and second (EMC).
Battery at first carries out charge and discharge cycles with the current density of 31 mA/g, and voltage range is 0-2 V.Behind circulation 10 circles, be discharged to 0V again, and then with current density constant-current discharge 5 h of 31 mA/g, at graphite pole piece surface electrochemistry plated metal lithium layer, the cathode of lithium capacity that obtains is 2.25 mAh, capacity is very little, and is seldom excessive, i.e. fail safe is good.
Embodiment 3
With hard carbon (HC) is the lithium carrier; Mix by mass ratio 92:2:1:5 with conductive agent carbon black (SP), conductive agent gas-phase growth of carbon fibre (VGCF), binding agent Kynoar (PVDF); With N-N-methyl-2-2-pyrrolidone N-(NMP) is solvent; With being uniformly coated on behind the high-speed emulsifying machine mixing pulping on the collector Cu paper tinsel; Oven dry 24 h in 60 ℃ vacuum drying chamber are subsequent use then.With the metal lithium sheet is negative pole, and hard carbon is to electrode, and Celgrad 2325 is a barrier film, 1.2 mol/L lithium hexafluoro phosphate (LiPF
6The basic carbonic ester of)/ethylene carbonate (EC)+first and second (EMC) (volume ratio is 3:7) is assembled into battery for electrolyte.
Battery at first carries out charge and discharge cycles with the current density of 40 mA/g, and voltage range is 0-3 V.Behind circulation 10 circles, be discharged to 0 V again, and then with current density constant-current discharge 4 h of 40 mA/g, at hard carbon pole piece surface electrochemistry plated metal lithium layer, the cathode of lithium capacity that obtains is 1.40 mAh, capacity is very little, and is seldom excessive, i.e. fail safe is good.For to electrode, the nickel sheet be a positive pole, charges to 3 V with the lithium electrode prepared, and the capacity that obtains is the capacity of lithium electrode, this cathode of lithium take off the lithium curve as shown in Figure 2.
Embodiment 4
The preparation method of carbon carrier and battery is with embodiment 3, and battery at first carries out charge and discharge cycles with the current density of 40 mA/g, and voltage range is 0-3 V.Behind circulation 10 circles, be discharged to 0 V again, and then with current density constant-current discharge 8 h of 40 mA/g, at hard carbon pole piece surface electrochemistry plated metal lithium layer, the cathode of lithium capacity that obtains is 2.57 mAh, capacity is very little, and is seldom excessive, i.e. fail safe is good.
Embodiment 5
With lithium titanate (Li
4Ti
5O
12) be anodal; Mix by mass ratio 90:5:5 with conductive agent carbon black (SP), binding agent Kynoar (PVDF); With N-N-methyl-2-2-pyrrolidone N-(NMP) is solvent; With being uniformly coated on behind the high-speed emulsifying machine mixing pulping on the collector Al paper tinsel, oven dry 24 h obtain lithium titanate (Li in 60 ℃ vacuum drying chamber then
4Ti
5O
12) pole piece, subsequent use.Use the cathode of lithium that makes among the embodiment 1, lithium titanate (Li
4Ti
5O
12) pole piece is anodal, Celgrad 2325 is a barrier film, 1.2 mol/L lithium hexafluoro phosphate (LiPF
6The basic carbonic ester of)/ethylene carbonate (EC)+first and second (EMC) (volume ratio is 3:7) is assembled into battery for electrolyte.
Battery at first with 0.05C charge and discharge cycles 2 times, charges and discharge circulation with 0.2C again.The first charge-discharge curve of this lithium/lithium titanate system battery has the characteristic platform of lithium carbonate as shown in Figure 3.Battery first circle capacity is 1.3601mAh, and after 100 circulations, capability retention is 83.48%, as shown in Figure 4.
Embodiment 6
Lithium titanate (Li
4Ti
5O
12) the pole piece preparation method is with embodiment 5, uses the cathode of lithium among the embodiment 2, lithium titanate (Li
4Ti
5O
12) pole piece is anodal, Celgrad 2325 is a barrier film, 1.2 mol/L lithium hexafluoro phosphate (LiPF
6(volume ratio is 3:7)+(FEC 5wt%) is assembled into battery for electrolyte to fluorinated ethylene carbonate to the basic carbonic ester of)/ethylene carbonate (EC)+first and second (EMC).
Battery at first with 0.05C charge and discharge cycles 2 times, charges and discharge circulation with 0.2C again.Battery first circle capacity is 0.7990 mAh, and after 45 circulations, capability retention is 77.40%.
Embodiment 7
Lithium titanate (Li
4Ti
5O
12) the pole piece preparation method is with embodiment 5, uses the cathode of lithium among the embodiment 3, lithium titanate (Li
4Ti
5O
12) pole piece is anodal, Celgrad 2325 is a barrier film, 1 mol/L lithium hexafluoro phosphate (LiPF
6The basic carbonic ester of)/ethylene carbonate (EC)+first and second (EMC) (volume ratio is 3:7) is assembled into battery for electrolyte.
Battery at first with 0.05C charge and discharge cycles 2 times, charges and discharge circulation with 0.2C again.Battery discharge capacity first is 0.6702 mAh, and after 75 circulations, capability retention is 89.33%.
Embodiment 8
With polymer sulphur is positive pole; Is that 70:20:10 mixes with conductive agent carbon black (ketjenblack), binding agent Kynoar (PVDF) by mass ratio; With N-N-methyl-2-2-pyrrolidone N-(NMP) is solvent; With being uniformly coated on behind the high-speed emulsifying machine mixing pulping on the collector Al paper tinsel; Oven dry 24 h obtain polymer sulphur pole piece in 50 ℃ vacuum drying chamber then, and are subsequent use.Use cathode of lithium among the embodiment 4, polymer sulphur is anodal, and Celgrad 2325 is a barrier film, 1.2 mol/L lithium hexafluoro phosphate (LiPF
6The basic carbonic ester of)/ethylene carbonate (EC)+first and second (EMC) (volume ratio is 3:7) is assembled into battery for electrolyte.
Battery discharges and recharges with 50 mA/g, and battery discharge capacity first is 0.8558 mAh, and the battery specific capacity is 653.78 mAh/g, and circulating, capability retention is 76.06% after 15 times.
Although content of the present invention has been done detailed introduction through above preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple modification of the present invention with to substitute all will be conspicuous.Therefore, protection scope of the present invention should be limited appended claim.
Claims (5)
1. the preparation method of a cathode of lithium is characterized in that, this method comprises following concrete steps:
Step 1, the embedding lithium: material with carbon element (2) is coated on the collector (1), and this collector (1) is selected the Cu paper tinsel, and oven dry obtains the material with carbon element pole piece; With the metal lithium sheet is negative pole, and described material with carbon element pole piece is to electrode, and charge and discharge cycles is carried out in assembled battery, makes lithium ion (3) evenly be embedded in the material with carbon element (2), accomplishes embedding lithium step;
Step 2, overdischarge plated metal lithium layer (4): with the battery of above-mentioned completion embedding lithium step, under 10-100 mA/g current density, constant-current discharge 2-20 h carries out overdischarge, at material with carbon element pole piece surface electrochemistry plated metal lithium layer (4), obtains cathode of lithium.
2. the preparation method of cathode of lithium as claimed in claim 1 is characterized in that, described material with carbon element (2) comprises: more than any one in MCMB, hard carbon, graphite, the Graphene.
3. cathode of lithium that method according to claim 1 and 2 makes; It is characterized in that; This cathode of lithium is as collector (1) with the Cu paper tinsel; Material with carbon element (2) is coated on the collector (1) as carrier; Embed lithium ion (3) in carrier inside, at the surface deposition lithium metal layer (4) of carrier.
4. a battery that comprises the cathode of lithium that claim 1 or 2 described methods make is characterized in that this battery comprises described cathode of lithium and poor lithium anode material.
5. battery as claimed in claim 4 is characterized in that, more than any one in described poor lithium anode material selection lithium titanate, elemental sulfur, elemental sulfur/carbon material compound, the sulfur-based compound.
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