CN101399329B - Manufacturing method of positive pole plate of lithium-sulfur cell - Google Patents
Manufacturing method of positive pole plate of lithium-sulfur cell Download PDFInfo
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- CN101399329B CN101399329B CN2007101224442A CN200710122444A CN101399329B CN 101399329 B CN101399329 B CN 101399329B CN 2007101224442 A CN2007101224442 A CN 2007101224442A CN 200710122444 A CN200710122444 A CN 200710122444A CN 101399329 B CN101399329 B CN 101399329B
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Abstract
The invention relates to a pole piece of a positive electrode of a lithium-sulfur battery and a preparation method thereof. The pole piece takes gelatin as a binding agent to coat a positive electrode active material and a conductive additive on a current collector, thereby improving the adhesion and the dispersion of the electrode. Meanwhile, the pole piece of the positive electrode of the lithium-sulfur battery prepared by freeze-drying comprises a micro-porous structure, thereby reducing the infiltration resistance of electrolyte on the pole piece and improving the electrochemical reversibility and the cycle stability of the battery.
Description
Technical field:
The present invention relates to the preparation method of gelatin as a kind of positive pole plate of lithium-sulfur cell of adhesive.
Background technology:
Littler, the lighter and more fast development of high performance electronic communication apparatus requires exploitation high-performance and jumbo battery to adapt with it.Lithium-sulfur cell has high theoretical energy density (2800Whkg), and enrich in the source of while sulphur, environmental sound, becomes the focus of research.
The anodal preparation process of general lithium-sulfur cell is: in solvent positive active material, conductive agent and adhesive are mixed, make slurries, then slurries are coated on the collector, remove wherein remaining solvent by vacuumize, promptly obtain anode pole piece.Wherein adhesive is the key factor that influences battery performance, the condition that it should possess is: first should have good adhesiveness, avoid active material the serious phenomenon of peeling off to take place, thereby guarantee the mechanical integrity of anode pole piece, improve the cycle performance of battery in course of reaction; Second should have chemical anti-polysulfide, guarantee under the battery operated temperature stability and to the solubility of the organic solvent that uses in the slurries.
The lithium-sulfur cell adhesive of Shi Yonging in the past, majority is poly(ethylene oxide) (PEO), butadiene-styrene rubber or Kynoar (PVDF) etc., the former two's adhesiveness is relatively poor, need in positive pole, add more content (＞10%) to guarantee not peeling off phenomenon (Sang-Eun Cheon, Ki-Seok Ko, Ji-Hoon Cho et al of active matter and conductive agent, J.Electrochem.Soc., 2002,149 (11), A1437-A1441; Sang-Eun Cheon, Ki-Seok Ko, Ji-Hoon Cho et al, J.Electrochem.Soc., 2003,150 (6), A800-A805); Latter's adhesiveness is better, but high boiling solvents such as need employing N-methyl pyrrolidone disperse, simultaneously also need be under higher temperature dry pole piece (under the vacuum 80 ℃), thereby cause the loss of positive electrode active material elemental sulfur or polysulfide easily to a certain extent.
Gelatin is the collagen in mammal (pig, the ox etc.) connective tissue (bone, skin, tendon), the macro-molecular protein that obtains through appropriate hydrolysis and thermal denaturation.Can be divided into according to its source difference: skin gelatin and bone gelatin (" manufacturing of gelatin Processes and apparatus " writes group, manufacturing of gelatin Processes and apparatus [M], and Beijing, light industry publishing house, 1996:4-5).Gelatin has excellent physicochemical property as a kind of natural polymer product.It has good adhesiveness, in industries such as field of medicaments, furniture industry, leather and fur products, adhesive tape, carton, emery cloth, sand paper, match, be widely used, common have (Ye Chuping such as operation adhesive, medical solid adhesive, building construction adhesive, the Li Ling orchid, Wang Niangui writes, natural adhesive [M], Beijing, Chemical Industry Press, 2004:501-502).In addition, gelatin has good dispersiveness, successfully is applied to numerous areas such as sensitization; Gelatin has nontoxic and biodegradable, makes its be applied at aspects such as organizational projects (Yao Kangde, Yin Yuji, organizational project associated biomolecule material [M], Beijing, Chemical Industry Press, 2003.).
Be with the advantage of gelatin as electrode adhesive: (1) bonding force is strong, helps keeping the stable of positive electrode structure; (2) good dispersion, evenly dispersed electro-conductive agent and active material; (3) can water be solvent, environmental protection, safety; (4) can adopt freeze drying, prepare the loose structure pole piece, help the infiltration of electrolyte, avoid the pole piece high temperature drying to cause the elemental sulfur distillation simultaneously by the ice crystal drilling.Therefore, gelatin is used for positive pole plate of lithium-sulfur cell preparation as adhesive and has good prospect.
Summary of the invention:
The preparation method who the purpose of this invention is to provide a kind of positive pole plate of lithium-sulfur cell is coated in positive active material, conductive agent on the collector as adhesive with gelatin, improves the cementability and the dispersiveness of electrode.Adopt the positive pole plate of lithium-sulfur cell of freeze drying preparation to have the microcosmic loose structure simultaneously, reduced the infiltration resistance of electrolyte, improve the electrochemical reversibility and the cyclical stability of battery pole piece.
Positive pole plate of lithium-sulfur cell of the present invention is made up of the collector of conduction current and positive active material, conductive agent and the adhesive that is coated on the collector, and it is characterized in that: the pole piece surface presents the microcosmic loose structure; Said adhesive is a gelatin, and wherein, the mass percent of positive active material, conductive agent and gelatin is 50～80%, 15～30% and 5～20%.
Described positive active material is S
8, Li
2S
n(1≤n≤8) or organosulfur compound, the preferred carbon sulphur of organosulfur compound polymer (C
2S
x)
m(x is 2.5～50, and m 〉=2).
Described conductive agent is a carbon-based conductive agent, as conductive carbon black, acetylene black or graphite powder etc.
Said collector is aluminium foil or aluminium net.
Described gelatin can be that the whole bag of tricks makes, and both can be that skin gelatin also can be a bone gelatin according to its source difference.
Positive pole plate of lithium-sulfur cell of the present invention is according to following method preparation, gelatin is dissolved in the water, make mass concentration and be 1～6% gelatin solution, positive active material, conductive agent, gelatin are mixed, wherein, the mass percent of positive active material, conductive agent and adhesive is respectively 50～80%, 15～30% and 5～20%.The method of mixing comprises: mechanical ball milling method, physical grinding method or mechanical mixing method etc.The positive electrode material slurry of making is coated on the collector, and drying is made the anode pole piece of lithium-sulfur cell.
The dry run of above-mentioned positive electrode material slurry can adopt conventional vacuum seasoning or other seasoning, as the solvent dehydration seasoning.Simultaneously for making pole piece surface obtain the microcosmic loose structure, also can be before drying, will be coated in positive electrode material slurry on the collector earlier and in-30～-60 ℃ temperature range, be refrigerated to and form the ice crystal structure, carry out drying again.
What the present invention was prepared is the lithium-sulphur cell positive electrode of adhesive with the gelatin, and the positive pole prepared with adopting existing adhesive compared, characteristics such as have that cementability is strong, good dispersion, technology environmental protection, specific capacity height, cyclicity are good.Simultaneously, positive pole plate of lithium-sulfur cell by the freeze drying preparation, the microcosmic loose structure that it possessed soaks into for the deep layer of electrolyte provides good passage, has reduced the infiltration resistance of electrolyte to pole piece, has improved the electrochemical reversibility and the cyclical stability of battery.
Be assembled into CR2025 type button cell with anode pole piece cooperation of the present invention, negative material is alloys such as the alloy of lithium or lithium and other alkali metal or alkaline-earth metal and Li/Al, Li/Si, Li/Pb, Li/Sn, Li/Sb, Li/Bi, Li/Zn, Li/Cd, Li/C, electrolytical range of choice is liquid state, gel, solid-state electrolyte system, liquid electrolyte can be selected a kind of organic solvent among DME (glycol dimethyl ether), DOL (1,3 dioxolane) and the THF (oxolane) or the mixture of several organic solvents for use.Supporting electrolyte can be lithium perchlorate, trifluoromethyl sulfonic acid lithium, lithium hexafluoro phosphate etc.Under the room temperature environment, be 1.5V to 2.8V at deboost, charging and discharging currents density is respectively 1mAh/cm
2And 0.4mAh/cm
2Condition under carry out the constant current charge-discharge performance test.
At first, be negative pole with the lithium, the pole piece (embodiment 1) of boulton process preparation of the present invention is anodal, the LiClO of 1mol/L
4(V/V=1: 1) for electrolyte is assembled into battery, carry out the charge-discharge performance test, the result shows that its first discharge capacity reaches 1056mAh/g to/DME+THF.
Secondly, with the lithium be the LiClO of the pole piece (embodiment 2) of negative pole, boulton process of the present invention preparation for positive pole, 1mol/L
4(V/V=1: 1) for electrolyte is assembled into battery, carry out the charge-discharge performance test, the result shows that its first discharge capacity reaches 1132mAh/g to/DME+DOL, after 20 circulations, leaves the specific capacity of 485mAh/g.
Once more, with the lithium be the LiClO of the pole piece with loose structure (embodiment 3) of negative pole, freeze-drying of the present invention preparation for positive pole, 1mol/L
4/ DME+THF (V/V=1: 1) for electrolyte is assembled into battery, carry out the charge-discharge performance test, find that first discharge capacity reaches 1108mAh/g.
At last, with the lithium be the LiClO of the pole piece with loose structure (embodiment 4) of negative pole, freeze-drying of the present invention preparation for positive pole, 1mol/L
4/ DME+DOL (V/V=1: 1) for electrolyte is assembled into battery, carry out the charge-discharge performance test, find first discharge capacity, after 20 circulations, still leave the specific capacity of 770mAh/g up to 1198mAh/g.
Description of drawings:
Fig. 1 amplifies 50,000 times SEM (electronic scanner microscope) photo for the embodiment of the invention 2 anode pole pieces;
Fig. 2 amplifies 50,000 times SEM photo for the loose structure lithium-sulphur cell positive electrode of the embodiment of the invention 4 preparations;
Fig. 3 is the loose structure lithium-sulphur cell positive electrode of the embodiment of the invention 4 preparations, after 50 charge and discharge cycles, amplifies 3.5 ten thousand times SEM photo;
Fig. 4 is for adopting the embodiment of the invention 1, the lithium-sulfur cell units activity material sulphur weight discharge characteristic curve figure of embodiment 2, embodiment 3 and embodiment 4 anode pole pieces;
Fig. 5 is for adopting the lithium-sulfur cell units activity material sulphur weight cycle performance figure of the embodiment of the invention 2 and embodiment 4 anode pole pieces;
Fig. 6 is for adopting the cyclic voltammogram of lithium-sulfur cell under different time of the embodiment of the invention 4 anode pole pieces.
Embodiment:
Below prepare the exemplary embodiments of high energy storage lithium-sulfur cell, the invention is not restricted to these embodiment but should understand for the present invention.
Embodiment 1
Under the room temperature,, in 60 ℃ water-bath, dissolve again, be mixed with mass percentage concentration and be 3% aqueous gelatin solution gelatin abundant swelling in water, standby.
The preparation of anode pole piece: with mass fraction is that sublimed sulfur and 2 parts of acetylene blacks of 7 parts are mixed in proportion, grind evenly, add the binder solution that contains 1 part of gelatin solid again, grinding makes binder solution with active material with acetylene black is full and uniform mixes, make the positive electrode material slurry, be coated on the aluminum foil current collector, vacuumize 10h obtains positive active material, conductive agent and gelatin adhesive quality percentage composition and is 70%, 20%, 10% anode pole piece.
Use the pole piece of above-mentioned preparation to be positive pole, Li is a negative pole, and barrier film is selected polypropylene screen for use, and electrolyte is the LiClO of 1mol/L
4Solution, solvent are that (V/V=1: 1), (humidity is less than 1%) is assembled into CR2025 type button cell to DME (glycol dimethyl ether)+THF (oxolane) in glove box, carries out electro-chemical test then.
Embodiment 2
Under the room temperature,, in 60 ℃ water-bath, dissolve again, be mixed with mass percentage concentration and be 2% aqueous gelatin solution gelatin abundant swelling in water, standby.
The preparation of anode pole piece: with mass fraction is that sublimed sulfur and 3 parts of acetylene blacks of 6 parts are mixed in proportion, grind evenly, add the binder solution that contains 1 part of gelatin solid again, grinding makes binder solution with active material with acetylene black is full and uniform mixes, make the positive electrode material slurry, be coated on the aluminum foil current collector, vacuumize 10h obtains positive active material, conductive agent and gelatin adhesive quality percentage composition and is 60%, 30%, 10% anode pole piece.
Because of the gelatin adhesive that is adopted has good dispersive property to conductive agent, thereby this pole piece component is uniformly dispersed, and do not have tangible agglomeration, as shown in Figure 1.Thereby improved the discharge performance of electrode.
Use the pole piece of above-mentioned preparation to be positive pole, Li is a negative pole, and barrier film is selected polypropylene screen for use, and electrolyte is the LiClO of 1mol/L
4Solution, solvent are that (V/V=1: 1), (humidity is less than 1%) is assembled into CR2025 type button cell to DME (glycol dimethyl ether)+DOL (1, the 3-dioxolane) in glove box, carries out electro-chemical test then.
Embodiment 3
Under the room temperature,, in 60 ℃ water-bath, dissolve again, be mixed with mass percentage concentration and be 4% aqueous gelatin solution gelatin abundant swelling in water, standby.
The preparation of positive electrode: with mass fraction is that sublimed sulfur and 2 parts of acetylene blacks of 7 parts are mixed in proportion, grind evenly, add the binder solution that contains 1 part of gelatin solid again, grinding is until forming homodisperse positive electrode material slurry, and it is coated on the aluminum foil current collector, freezing 4h is to form the ice crystal structure under-40 ℃, vacuumize dry 12h afterwards, obtain positive active material, conductive agent and gelatin adhesive quality percentage composition and be 70%, 20%, 10% anode pole piece with microcosmic loose structure.
Use the pole piece of above-mentioned preparation to be positive pole, Li is a negative pole, and barrier film is selected polypropylene screen for use, and electrolyte is the LiClO of 1mol/L
4Solution, solvent are that (V/V=1: 1), (humidity is less than 1%) is assembled into CR2025 type button cell to DME (glycol dimethyl ether)+THF (oxolane) in glove box, carries out electro-chemical test then.
Embodiment 4
Under the room temperature,, in 60 ℃ water-bath, dissolve again, be mixed with mass percentage concentration and be 2% aqueous gelatin solution gelatin abundant swelling in water, standby.
The preparation of positive electrode: with mass fraction is that sublimed sulfur and 3 parts of acetylene blacks of 6 parts are mixed in proportion, grind evenly, add the binder solution that contains 1 part of gelatin solid again, grinding is until forming homodisperse positive electrode material slurry, and it is coated on the aluminum foil current collector, form the ice crystal structures in-50 ℃ of down freezing 5h, vacuumize 16h afterwards obtains positive active material, conductive agent and gelatin adhesive quality percentage composition and is 60%, 30%, 10% anode pole piece.Pole piece has uniform microcosmic loose structure, as shown in Figure 2.
In addition, this loose structure has good stable to electrolyte, and along with the carrying out of charge and discharge cycles, no collapse phenomenon occurs, and still can keep stable after 50 circulations, as shown in Figure 3.
Use the pole piece of above-mentioned preparation to be positive pole, Li is a negative pole, and barrier film is selected polypropylene screen for use, and electrolyte is the LiClO of 1mol/L
4Solution, solvent are that (V/V=1: 1), (humidity is less than 1%) is assembled into CR2025 type button cell to DME (glycol dimethyl ether)+DOL (1, the 3-dioxolane) in glove box, and has carried out discharging and recharging with cyclic voltammetric and tested.
The battery of making in embodiment 1,2,3 and 4 is carried out the charge-discharge performance test at ambient temperature, and deboost is 2.8V to 1.5V, and charging and discharging currents density is respectively 1mAh/cm
2With 0.4 mAh/cm
2Battery has a discharge platform respectively between 2.3-2.4V and 2.0-2.1V as shown in Figure 4.Fig. 5 shows that the battery head among the embodiment 1 puts capacity and reach 1056mAh/g; Battery head among the embodiment 2 is put capacity and is reached 1132mAh/g, after 20 circulations, leaves the specific capacity of 485mAh/g; Battery head among the embodiment 3 is put capacity and is reached 1108mAh/g; And the battery among the embodiment 4 is put at head and all is significantly improved aspect capacity and the cycle performance, and its head is put capacity up to 1198mAh/g, after 20 circulations, still remains the specific capacity of 770mAh/g.In addition, by finding that to the contrast (Fig. 6) of the cyclic voltammetric data of loose structure electrode under the difference circulation lithium-sulphur cell positive electrode of this loose structure has good cyclical stability and electrochemical reversibility.
Claims (7)
1. the preparation method of a positive pole plate of lithium-sulfur cell, gelatin is dissolved in the water, make gelatin solution, positive active material, conductive agent, gelatin are respectively 50～80%, 15～30% and 5～20% with mass percent and mix, make the positive electrode material slurry and be coated on the collector, drying is made the anode pole piece of lithium-sulfur cell, it is characterized in that: before the drying, the positive electrode material slurry that will be coated in earlier on the collector is refrigerated to formation ice crystal structure in-30～-60 ℃ of temperature ranges.
2. preparation method according to claim 1 is characterized in that: the mass concentration of gelatin solution is 1～6%.
3. according to the preparation method of claim 1 or 2, it is characterized in that: positive active material is S
8, Li
2S
nOr organosulfur compound, wherein 1≤n≤8.
4. according to the preparation method of claim 3, it is characterized in that: described organosulfur compound is carbon sulphur polymer (C
2S
x)
m, wherein x is 2.5～50, and m 〉=2.
5. according to the preparation method of claim 1 or 2, it is characterized in that: said collector is aluminium foil or aluminium net.
6. according to the preparation method of claim 1 or 2, it is characterized in that: conductive agent is a carbon-based conductive agent.
7. according to the preparation method of claim 6, it is characterized in that: conductive agent is conductive carbon black, acetylene black or graphite powder.
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