CN1750296A - Lithium ion secondary battery negative pole and its preparing method and lithium secondary battery including said negative pole - Google Patents

Lithium ion secondary battery negative pole and its preparing method and lithium secondary battery including said negative pole Download PDF

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Publication number
CN1750296A
CN1750296A CNA2004100514938A CN200410051493A CN1750296A CN 1750296 A CN1750296 A CN 1750296A CN A2004100514938 A CNA2004100514938 A CN A2004100514938A CN 200410051493 A CN200410051493 A CN 200410051493A CN 1750296 A CN1750296 A CN 1750296A
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China
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lithium
negative pole
lithium ion
conduction material
ion conduction
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CNA2004100514938A
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陈冠宗
周俊杰
张翠萍
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Priority to CNA2004100514938A priority Critical patent/CN1750296A/en
Priority to PCT/CN2005/001267 priority patent/WO2006029561A1/en
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • 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

Abstract

This invention discloses the negative of a Li ionic secondary battery, its preparation method and the battery containing said negative, among which, the negative includes: rhombic black phosphorus with orthogonal structure applied by an inorganic solid electrolyte crystal film in 20-5000 artificially

Description

Negative pole of lithium rechargeable battery and preparation method thereof and the lithium rechargeable battery that comprises this negative pole
Technical field
The present invention relates to negative pole of a kind of lithium rechargeable battery and preparation method thereof, and the lithium rechargeable battery that comprises this negative pole.Relate in particular to a kind of inorganic solid electrolyte crystal film that manually applies, described crystal film has good lithium ion conductivity and can form the negative pole its preparation method of lithium rechargeable battery of effective SEI film and the lithium rechargeable battery that comprises this negative pole with existing lithium ion carbonic ester electrolyte.
Background technology
Current society is the society of information develop rapidly, and interrogating fast, accurate, a large amount of storage and transmission information is the requirement of information age.The development of portable electric appts such as mobile phone, notebook computer, palmtop PC, in light weight, lithium rechargeable battery capacious is had higher requirement.1), its theoretical specific capacity has only 372mAh/g, thereby limited the further raising of lithium rechargeable battery specific capacity what present commercial ion secondary battery cathode material lithium usually adopted is the graphite-like material with carbon element, and its weak point is:; 2), tap density causes volumetric specific energy low for a short time, its tap density is generally at 0.8g/cm 3
Summary of the invention
The lithium rechargeable battery that technical problem to be solved by this invention provides negative pole of a kind of lithium rechargeable battery and preparation method thereof and comprises this negative pole, this negative pole comprise one deck and have good lithium ion conductivity and the inorganic solid electrolyte crystal film good with carbonic ester electrolyte compatibility.This lithium ion secondary battery negative pole can prepare with a kind of straightforward procedure.
Technology solution of the present invention is as follows:
A kind of negative pole of lithium rechargeable battery comprises: the oblique side's black phosphorus with orthohormbic structure; Manually apply one deck inorganic solid electrolyte crystal film on black phosphorus, described crystal film has the thickness of 20-5000 and comprises a kind of ionic conductivity at least 1 * 10 -10The lithium ion conduction material of S/cm.
Described lithium ion conduction material is Li xPO y, wherein, 2＜X＜4 and 3＜Y＜5.
Described lithium ion conduction material is Li 3PO 4
Described lithium ion conduction material is Li aPO bN CA is 2-4 herein, and b is 3-5, and c is 0.1-0.9.
Described lithium ion conduction material is Li 2.9PO 3.3N 0.46
A kind of method for preparing lithium ion secondary battery negative pole in strong oxidant solution, is advanced oxidation processes with black phosphorus, and with the compound effects deposition one deck solid electrolyte crystal film that contains lithium, described crystal film contains a kind of ionic conductivity and is at least 1 * 10 -10The lithium ion conduction material of s/cm; Strong oxidizer is selected from and comprises ammonium persulfate, nitric acid, hydrogen peroxide and sulfuric acid; Lithium-containing compound is selected from and comprises n-BuLi, tert-butyl lithium, hexafluoro phosphorus lithium, LiBF4, lithium citrate, lithium naphthalene and lithium hydroxide.
Above-mentioned lithium ion conduction material is Li xPO y, wherein, 2＜X＜4 and 3＜Y＜5.
Above-mentioned lithium ion conduction material is Li 3PO 4
A kind of lithium rechargeable battery, its negative pole are to deposit one deck to have the thickness of 20-5000 and contain a kind of ionic conductivity and be at least 1 * 10 on the black phosphorus base material -10The crystal film of the lithium ion conduction material of s/cm; Positive pole comprises a kind of combination that is selected from by cobalt acid lithium, lithium nickelate, LiMn2O4, cobalt lithium nickelate, nickel LiMn2O4, LiFePO4, cobalt phosphate lithium any or two or more arbitrary proportions wherein; The main salt of electrolyte can be wherein a kind of of lithium hexafluoro phosphate, LiBF4, hexafluoroarsenate lithium, lithium perchlorate, perfluoro alkyl sulfonic acid lithium; Solvent composition can be the combination of one or more arbitrary proportions in vinyl carbonate, dimethyl carbonate, diethyl carbonate, propylene carbonate, two methyl ethyl carbonates, carbonic acid first propyl ester, diethoxyethane, the 2-methyltetrahydrofuran.
1), the specific capacity of comparing it with traditional carbon negative pole can improve widely and reach 700mAh/g outstanding effect of the present invention is:; 2), tap density is big, density is generally at 1.27g/cm 3, be convenient to battery like this and can improve volumetric specific energy.
Description of drawings
Charging and discharging curve figure when Fig. 1 does not have crystal film for black phosphorus negative pole of the present invention;
Fig. 2 has deposited Li for black phosphorus negative pole of the present invention aPO bN CThe charging and discharging curve figure second time after the crystal film;
XRD figure spectrum after Fig. 3 discharges and recharges for black phosphorus negative pole of the present invention does not have crystal film;
XRD figure spectrum before Fig. 4 discharges and recharges for black phosphorus negative pole of the present invention does not have crystal film;
Fig. 5 has deposited Li for black phosphorus negative pole of the present invention 3PO 4The charging and discharging curve figure second time after the crystal film.
Embodiment
Embodiment 1
It is 10% nitric acid (HNO that the 5 gram black phosphorus powder that 200 orders are sieved are put into 100 milliliters strong oxidizer concentration 3) carried out oxidation processes at normal temperatures 10 hours in the solution, and then with the distilled water washing, put into drying box then 120 ℃ of oven dry 12 hours down.And then be that binding agent, N-methyl pyrrolidone are organic solvent with the vinylidene fluoride, acetylene black is conductive agent, by black phosphorus: acetylene black: vinylidene fluoride=90: 4: the 6 mixed slurry that stirs is coated on the copper foil of affluxion body, 120 ℃ of oven dry 16 hours down.Be immersed in the lithium-containing compound n-BuLi/ethane solution of arbitrary proportion 12 hours then, with putting into vacuum drying chamber after the dimethoxy ethane washing, be incubated 48 hours and promptly get lithium ion secondary battery negative pole required for the present invention again temperature programming to 160 ℃.
With the above-mentioned lithium ion secondary battery negative pole that makes, positive electrode is that cobalt acid lithium, electrolyte are that lithium hexafluoro phosphate, solvent are vinyl carbonate and diethyl carbonate, and volume ratio is 1: 1, and barrier film is the CeLgrd2300 microporous barrier, make 063048 battery, the capacity of measuring this battery is 1385mAh.
Embodiment 2
With the above-mentioned lithium ion secondary battery negative pole that makes, positive electrode is a LiMn2O4, and electrolyte is the hexafluoro lithium borate, and solvent is that vinyl carbonate and diethyl carbonate volume ratio are 1: 3, and barrier film is the CeLgrd2300 microporous barrier, makes 063048 battery., the capacity of measuring this battery is 1345mAh.
Embodiment 3
With the above-mentioned lithium ion secondary battery negative pole that makes, positive electrode is that lithium nickelate, electrolyte are that chloric acid acid lithium, solvent solvent are vinyl carbonate and diethyl carbonate, and volume ratio is 1: 1, and barrier film is the CeLgrd2300 microporous barrier, make 063048 battery, the capacity of measuring this battery is 1425mAh.
Embodiment 4:
Under inert gas atmosphere, utilize a target with crystal deposition to the black phosphorus electrode, described crystal film comprises that a kind of lithium ion conductivity is at least 1 * 10 -10S/cm lithium ion conduction material.
Described lithium ion conduction material is Li xPO y, wherein, the compound that 2＜X＜4 and 3＜Y＜5 are represented, and it is stable under nitrogen atmosphere.
Described lithium ion conduction material is Li aPO bN CA is 2-4 herein, and b is 3-5, and c is 0.1-0.9.
Inert gas is selected from helium, neon and argon gas, because above-mentioned gas can not produce accessory substance with black phosphorus generation chemical reaction.
Described target can be Li 3PO 4The perhaps Li that mixes with suitable mixed proportion 2O and P 2O 5Mixture.
At pressure is 5 millitorrs, and radio-frequency power is under 300W and the argon gas atmosphere, and the use diameter is 4 inches Li 3PO 4Target formed one deck Li in 10 minutes at the black phosphorus electro-deposition 3PO 4Crystal film
Described deposition process is undertaken by suitable method, for example: plating, electron beam evaporation, vacuum thermal evaporation, laser ablation, chemical vapor deposition, thermal evaporation, plasma chemical vapor deposition, laser chemistry gas deposition or injection gas deposition.Various equivalent modifications is appreciated that described deposition is not limited to said method, and it comprises the method for any routine.
With undressed black phosphorus as negative pole, metal lithium sheet is to electrode, barrier film is the CeLgrd2300 microporous barrier, electrolyte is 1.0mol/L, LiPF6/EC: DEC, the solvent volume ratio is 1: 1, makes simulated battery in the glove box of relative humidity little 1%, and it the results are shown in Figure 1 to measure the black phosphorus charge-discharge performance.Owing to do not form effective SEI film, cause solvent molecule to take place to embed altogether among Fig. 1, be shown as zero among the discharge capacity figure at 0.8 volt.
The black phosphorus electrode that said method is made is a negative pole, metal lithium sheet is to electrode, barrier film is the CeLgrd2300 microporous barrier, electrolyte is 1.0mol/L, LiPF6/EC: DEC, the solvent volume ratio is 1: 1, makes machine formula simulated battery in the glove box of relative humidity little 1%, measure the black phosphorus charge-discharge performance its results are shown in Figure 2, Fig. 5.Can carry out being effective charge and discharge cycles, discharge capacity Fig. 2 630mAh/g from Fig. 2,5 negative pole of the present invention as can be seen.V represents voltage among Fig. 5, and C represents specific capacity.
Test condition:
Charging and discharging currents density, charging current 1mA/cm 2, discharging current 1mA/cm 2Cut-ff voltage 0-1.0 volt.Experimental result shows that the black phosphorus electrode through behind the artificial deposited crystal film, forms a voltage platform at 0.8 volt during initial charge, and corresponding is to adhere to the fine and close effectively SEI film of one deck on crystal film.Because the formation of this SEI film has stoped the common embedding of organic molecule, discharge capacity is greater than 650mAh/g.Black phosphorus electrode without the deposited crystal film does not form effective SEI film, and solvent molecule takes place to embed altogether, makes the destruction of black phosphorus structure generation essence, and discharge capacity is zero.Fig. 3 is the XRD figure spectrum that does not have after the deposited crystal film charges.
Operation principle: black phosphorus has the same layer structure of image-stone China ink, atom superposes with the σ covalent bond in the aspect, mutual strong bonded, two interlayers only connect with weak Van der Waals force, the crystal structure of this mixing of bonding makes it have special chemical property, and both some atoms, molecule can be embedded between this crystalloid aspect, does not destroy the covalent bond of stacking, interlamellar spacing is changed, generate intercalation compound.In the graphite, a carbon atom is 3 formation σ covalent bonds with ligancy, and only surplus next P electronics participates in forming delocalized pi-bond, and in the black phosphorus, after phosphorus atoms is 3 formation σ covalent bonds with ligancy, has a pair of lonely P electronics to participate in the formation delocalized pi-bond.This explanation black phosphorus can provide the bonding electrons of more and lithium ion coordination.Black phosphorus has the more possibility of height ratio capacity than graphite.The black phosphorus negative pole is in carbonic ester electrolyte systems such as propylene carbonate, vinyl carbonates, and initial charge can not form effective SEI film, causes solvent molecule to take place to embed altogether, the destruction of essence the black phosphorus crystal structure, therefore the black phosphorus electrode is lost activity.But oblique side's black phosphorus of orthohormbic structure; Manually apply one deck inorganic solid electrolyte crystal film on black phosphorus, described crystal film has the thickness of 20-5000 and comprises a kind of ionic conductivity at least 1 * 10 -10Behind the S/cm lithium ion conduction material, experimental results show that initial charge can form effective SEI film at the negative pole of black phosphorus substrate surface deposited crystal film, stop the generation of the black phosphorus structural collapse phenomenon that the common embedding owing to the solvent lithium ion causes.And it allows lithium ion from wherein passing through.
The black phosphorus powder can form the oxide and the acid of phosphorus in the embodiments of the invention 1 at the effect lower surface of strong oxidizer, after the aquae destillata washing, remain in oxide heat drying under the condition that water and oxygen are arranged on black phosphorus surface, its surface can generate a spot of phosphoric acid, because phosphoric acid can form one deck Li on the surface of black phosphorus particle with the compound effects that contains lithium 3PO 4Crystal film.

Claims (9)

1, a kind of negative pole of lithium rechargeable battery is characterized in that: comprising: the oblique side's black phosphorus with orthohormbic structure; Manually apply one deck inorganic solid electrolyte crystal film on black phosphorus, described crystal film has the thickness of 20-5000 and comprises a kind of ionic conductivity at least 1 * 10 -10The lithium ion conduction material of S/cm.
2, according to right 1 described negative pole, it is characterized in that: the lithium ion conduction material is Li xPO y, wherein, 2＜X＜4 and 3＜Y＜5.
3, negative pole according to claim 2 is characterized in that: the lithium ion conduction material is Li 3PO 4
4, negative pole according to claim 1 is characterized in that: the lithium ion conduction material is Li aPO bN CA is 2-4 herein, and b is 3-5, and c is 0.1-0.9.
5, negative pole according to claim 4 is characterized in that: the lithium ion conduction material is Li 2.9PO 3.3N 0.46
6, a kind of method for preparing lithium ion secondary battery negative pole, it is characterized in that: in strong oxidant solution, black phosphorus is advanced oxidation processes, with the compound deposition one deck solid electrolyte crystal film that contains lithium, described crystal film contain that a kind of ionic conductivity is at least 1 * 10 -10S/cm lithium ion conduction material; Strong oxidizer is selected from and comprises ammonium persulfate, nitric acid, hydrogen peroxide and sulfuric acid; Lithium-containing compound is selected from and comprises n-BuLi, tert-butyl lithium, hexafluoro phosphorus lithium, LiBF4, lithium citrate, lithium naphthalene and lithium hydroxide.
7, according to right 6 described methods, it is characterized in that: the lithium ion conduction material is Li xPO y, wherein, 2＜X＜4 and 3＜Y＜5.
8, method according to claim 6 is characterized in that: the lithium ion conduction material is Li 3PO 4
9, a kind of lithium rechargeable battery is characterized in that: its negative pole is to deposit one deck to have the thickness of 20-5000 and contain a kind of ionic conductivity and be at least 1 * 10 on the black phosphorus base material -10The crystal film of the lithium ion conduction material of S/cm; Positive pole comprises a kind of combination that is selected from by cobalt acid lithium, lithium nickelate, LiMn2O4, cobalt lithium nickelate, nickel LiMn2O4, LiFePO4, cobalt phosphate lithium any or two or more arbitrary proportions wherein; The main salt of electrolyte can be wherein a kind of of lithium hexafluoro phosphate, LiBF4, hexafluoroarsenate lithium, lithium perchlorate, perfluoro alkyl sulfonic acid lithium; Solvent composition can be the combination of one or more arbitrary proportions in vinyl carbonate, dimethyl carbonate, diethyl carbonate, propylene carbonate, two methyl ethyl carbonates, carbonic acid first propyl ester, diethoxyethane, the 2-methyltetrahydrofuran.
CNA2004100514938A 2004-09-16 2004-09-16 Lithium ion secondary battery negative pole and its preparing method and lithium secondary battery including said negative pole Pending CN1750296A (en)

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PCT/CN2005/001267 WO2006029561A1 (en) 2004-09-16 2005-08-16 Negative electrode for lithium ion secondary battery, method of making the same, and lithium ion secondary battery including the same

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Cited By (3)

* Cited by examiner, † Cited by third party
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CN102148401A (en) * 2010-02-04 2011-08-10 深圳市比克电池有限公司 Lithium-ion battery preparation method and battery prepared
CN107482173A (en) * 2017-06-21 2017-12-15 深圳大学 Lithium ion battery anode active material and preparation method thereof, anode plate for lithium ionic cell and lithium ion battery
CN114975863A (en) * 2022-08-01 2022-08-30 深圳市汉嵙新材料技术有限公司 Black phosphorus cathode, preparation method thereof and lithium ion battery

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KR101747402B1 (en) * 2015-10-12 2017-06-14 주식회사 엘지화학 Composite electrode for electrochemical device, method for manufacturing the same, and electrochemical device including the same

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Publication number Priority date Publication date Assignee Title
CN1086845C (en) * 1997-09-25 2002-06-26 中国科学院长春应用化学研究所 Preparation of lithium ion battery carbon material negative pole
US7247408B2 (en) * 1999-11-23 2007-07-24 Sion Power Corporation Lithium anodes for electrochemical cells
US6758404B2 (en) * 2001-08-03 2004-07-06 General Instrument Corporation Media cipher smart card
KR100467436B1 (en) * 2002-10-18 2005-01-24 삼성에스디아이 주식회사 Negative electrode for lithium-sulfur battery, method of preparing same, and lithium-sulfur battery comprising same
CN1209829C (en) * 2003-08-07 2005-07-06 中信国安盟固利电源技术有限公司 Application of black phosphor as cathode material of lithium ion accumulator and accumulator produced

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102148401A (en) * 2010-02-04 2011-08-10 深圳市比克电池有限公司 Lithium-ion battery preparation method and battery prepared
CN107482173A (en) * 2017-06-21 2017-12-15 深圳大学 Lithium ion battery anode active material and preparation method thereof, anode plate for lithium ionic cell and lithium ion battery
CN114975863A (en) * 2022-08-01 2022-08-30 深圳市汉嵙新材料技术有限公司 Black phosphorus cathode, preparation method thereof and lithium ion battery
CN114975863B (en) * 2022-08-01 2022-09-30 深圳市汉嵙新材料技术有限公司 Black phosphorus cathode, preparation method thereof and lithium ion battery

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