CN104577078A - Lithium ion battery cathode active substance and manufacturing method thereof - Google Patents

Lithium ion battery cathode active substance and manufacturing method thereof Download PDF

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Publication number
CN104577078A
CN104577078A CN201310515826.7A CN201310515826A CN104577078A CN 104577078 A CN104577078 A CN 104577078A CN 201310515826 A CN201310515826 A CN 201310515826A CN 104577078 A CN104577078 A CN 104577078A
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China
Prior art keywords
copper
active material
tin
electrode active
negative electrode
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CN201310515826.7A
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尹柏春
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XIANGTAN ZHONGDA NEW MATERIAL SCIENCE & TECHNOLOGY DEVELOPMENT Co Ltd
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XIANGTAN ZHONGDA NEW MATERIAL SCIENCE & TECHNOLOGY DEVELOPMENT Co Ltd
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Priority to CN201310515826.7A priority Critical patent/CN104577078A/en
Publication of CN104577078A publication Critical patent/CN104577078A/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
    • H01M4/36—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
    • H01M4/387—Tin or alloys based on tin
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Secondary Cells (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a lithium ion battery cathode active substance and a manufacturing method thereof. A cathode active substance layer consists of the following components in percentage by weight: 20-50% of carbon (C), 20% of copper (Cu), 1-5% of phosphorus (P) and the balance being tin (Sn). By taking the tin-carbon-copper-phosphorus alloy as a cathode active substance, the lithium battery has high capacitance maintenance characteristic in high load and low load. According to the manufacturing method of the lithium ion battery cathode active substance, the heating temperature is low, and the energy consumption is low.

Description

A kind of lithium ion battery negative pole active materials and manufacture method thereof
Technical field
The present invention relates to lithium ion battery material technical field, particularly a kind of ion battery negative electrode active material and manufacture method thereof.
Background technology
Along with portable type electronic product is day by day by universal, the feature of electronics miniaturization, needs battery to have the Energy transmission of less volume and Geng Gao ratio.Lithium ion battery is widely used in electronic product because of its energy density advantages of higher.
The key of high energy density cells is the electrode material exploitation of high capacity capacity.For reversible electrode material, have the open structural material such as stratiform or tunnel structure the most applicable, this class formation provides pipeline that lithium ion easily passes in and out and mobility fast.
What current lithium ion battery negative material on the market adopted is graphitic carbon material, because the characteristic of graphite material and partial order, is conducive to a large amount of embedding and the turnover of lithium ion.And graphite bears the formation of that face level hole passage in material, lithium ion can be impelled stored therein in a large number, and be conducive to the raising of electrode specific capacity.Simultaneously, because the gravimetric energy density of graphite is higher, and the structure of material itself has higher systematicness, so the irreversible capacitance of first time electric discharge can be lower, graphite cathode material has the effect of smooth working voltage in addition, has advantage to the use of electronic product and the design of charger.
But when graphite material is as negative material, theoretical specific capacity only has 372mAh/g, limit the further raising of lithium ion battery energy Ratios, the difficult demand meeting the electronic product battery of the high energy ratio day by day improved.And graphite material as the negative material of lithium battery when discharging first, can form one deck solid electrolyte film on its surface, solid electrolyte film can consume lithium ion, forms irreversible capacity thus.More have very, electrolyte is easily embedding altogether with it in the process of Lithium-ion embeding, and in this process of moving out, electrolyte is reduced, and the gaseous product generated causes graphite flake layer to peel off, cause forming solid electrolyte film further, increase irreversible capacity, cyclical stability declines simultaneously.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of ion battery negative electrode active material and manufacture method thereof, to solve the problem.
Technical problem to be solved by this invention adopts following technical scheme to realize:
A kind of ion battery negative electrode active material, is characterized in that, comprise carbon (C), copper (Cu), phosphorus (P) and tin (Sn).
Preferably, the mass percent shared by described carbon, copper, phosphorus and tin, carbon (C) is 20 to 50wt%, copper (Cu) is 5 to 20wt%, phosphorus (P) is 1 to 5wt%, and tin (Sn) is for add up to 100 percentage by weights with aforementioned elements.Wherein " wt% " represents mass percent.
Preferably, the mass percent shared by described carbon, copper, phosphorus and tin, carbon (C) is 35 to 45wt%, copper (Cu) is 15 to 20wt%, phosphorus (P) is 2 to 4wt%, and tin (Sn) is for add up to 100 percentage by weights with aforementioned elements.Wherein " wt% " represents mass percent.
Preferably, negative electrode active material also comprises conductive agent, the glutinous material such as bonding agent or viscosity adjusters.
Wherein said conductive agent is graphite fibre or metallic fiber or metal dust; Described adhesive is vinylidene fluoride or styrene butadiene ribber or ethylene propylene diene rubber; Described viscosity adjusters is CMC.
Preferably, the thickness of negative electrode active material is between 10um to 200um.
A manufacture method for ion battery negative electrode active material, is characterized in that, comprises the following step:
Step 631: form mixed powder
Get appropriate tin, copper, phosphor powder formation mixed powder;
Step 623: form tin-copper-phosphorus alloy material
In an inert gas environment, this mixed powder is added thermosetting one tin-copper-phosphorus alloy material;
Step 633: form tin-copper-phosphorus alloy powder;
Again in inert gas environment, cooling tin-copper-phosphorus mixture material is also placed on ball mill grinding in ball mill, and obtains tin-copper-phosphorus alloy powder.
Preferably, in described step 631, pass into inert gas, inert gas can be following gas: nitrogen (N 2), argon gas (Ar), carbon monoxide (Co) and carbon dioxide (CO 2).
Preferably, in described step 632, heating-up temperature is at least 300 0c.
Have choosing, in described step 632, heating-up temperature is 300 0c to 1100 0c.
Preferably, in described step 632, heating-up temperature is 700 0c.
Compared with prior art, the present invention has following beneficial effect: first, the present invention as negative electrode active material, and utilizes iron lithium phosphate as positive electrode active materials using tin-carbon-copper-phosphorus alloy, makes characteristic when lithium battery high load capacity and underload with high capacitance sustainment rate; The second, current lithium ion battery negative material needs through 2800 0c high temperature graphitization, energy consumption is higher, and the temperature of ion battery negative electrode active material manufacture method heating provided by the invention is low, and energy consumption is low.
Embodiment
In order to better the present invention is described, below by specific embodiment, the present invention is described further.
Lithium battery comprises: positive pole, negative pole, separator and electrolyte.Wherein, positive pole comprises positive electrode active material layer and positive electrode collector, and positive electrode active material layer is coated in positive electrode collector.Separator is separated positive pole and negative pole, to avoid short-circuiting effect.Electrolyte is configured among positive pole and negative pole, and ion can be moved freely between positive pole and negative pole.
Described negative electrode active material becomes by 20 to 50wt%(mass percent) carbon (C), the copper (Cu) of 5 to 20wt%, the phosphorus (P) of 1 to 5wt% and add up to the tin of 100 percentage by weights (Sn) to form with aforementioned elements.
A kind of more excellent scheme is that described negative electrode active material layer is by 35 to 45wt%(mass percent) carbon (C), the copper (Cu) of 15 to 20wt%, the phosphorus (P) of 2 to 4wt% and add up to the tin of 100 percentage by weights (Sn) to form with aforementioned elements.
Positive pole mainly comprises positive electrode collector and positive electrode active material layer, and positive electrode active material layer is coated in two sides or the one side of positive electrode collector.The material of positive electrode collector is the metal formings such as aluminium foil, nickel foil or stainless steel foil.And positive electrode active material layer contains in 1 or of more than two kinds can the positive electrode of occlusion or release lithium, also can mix the binders such as electric conducting material and polyvinylidene fluoride such as material with carbon element according to need simultaneously.Can occlusion or release lithium positive electrode comprise titanium sulfide (TIS 2), sulfuration niobium (NbSe 2) or vanadium oxide (V 2o 5) etc. containing the metal sulfide of lithium, metal selenide or metal oxide etc., then or lithium-containing compound.In addition, the material with carbon element of above-mentioned positive electrode active material layer can be the one in graphite, difficult graphite voltinism carbon, easily graphite voltinism carbon and carbonaceous material etc.
Described lithium-containing compound is broadly divided into the composite oxides containing lithium and transition metal, or contain the phosphate cpd of lithium and transition metal, especially with containing at least one in cobalt (Co), nickel (Ni) and manganese (Mn), higher voltage can be obtained thus.The chemical formula of the composite oxides containing lithium and transition metal can be expressed as LixMIO 2; And the phosphate cpd containing lithium and transition metal can be expressed as LiMIIPO 4, wherein, MI and MII represents the transition metal of more than a kind.X and y value is different because of charged state, and general x is more than or equal to and 0.05 is less than or equal to 1.1, y is more than or equal to 0.05 and is less than or equal to 1.1.
Positive electrode active material layer is heated by microwave heating source to be made, and is coated on a positive electrode collector, and the frequency provided during the heating of microwave heating source is between 0.3GHz to 30GHz.
Negative pole comprises negative collector body, and negative electrode active material layer is coated in two sides or the one side of negative electrode collector.The material of lid negative electrode collector is the metal formings such as Copper Foil, nickel foil or stainless steel foil.
What negative electrode active material layer contained one or more can the negative material of occlusion or release lithium, and such as, the ability containing the occlusions such as tin, copper, phosphorus or release ion is comparatively large and can obtain the material of high-energy-density.
Negative material can be the monomer of metal, alloy or compound, then or has one or more material above-mentioned at least partially.In the present invention, alloy, except being except metallic element of more than two kinds is formed, can be comprise the metallic element of more than a kind and the semimetallic elements of more than a kind, or is comprise the nonmetalloid of more than a kind.Sometimes solid solution, eutectic (mixture), intermetallic compound or this two or more alloy is wherein co-exist in its tissue.
In addition, negative electrode active material layer more comprises an adding material, can be silicon (Si), nickel (Ni), iron (Fe), cobalt (Co), manganese (Mn), zinc (Zn), indium (In), silver (Ag), titanium (Ti), germanium (Ge), bismuth (Bi), one of antimony (Sb) and chromium (Cr).
As can the negative material of occlusion and release lithium, also can use graphite, difficult graphited carbon or the easy carbonaceous material such as graphite voltinism carbon, and these carbonaceous materials also can be public with above-mentioned negative material.The change of crystal structure that carbonaceous material brings when the occlusion of lithium and release is considerably less, such as, makes it with when above-mentioned negative material is public, can obtain high-energy-density, and can obtain the cycle characteristics of excellence, more can play the function as conductive agent.
Negative electrode active material layer also can comprise conductive agent, the glutinous material such as bonding agent or viscosity adjusters.As conductive agent, can be graphite fibre, metallic fiber or metal dust etc.As adhesive, can be fluorine macromolecular compound or the synthetic rubber such as styrene butadiene ribber or ethylene propylene diene rubber etc. such as vinylidene fluoride.As viscosity adjusters, it can be CMC etc.
In addition, the thickness of negative electrode active material layer is between 10um to 200um; A kind of more excellent selection is that thickness is between 30um to 80um.
Separator is for isolating positive pole negative pole, and one side prevents the two poles of the earth contact from causing short circuit current, lithium ion can be allowed to pass through on the other hand.The hard films of the plastic multiple aperture plasma membrane that separator utilizes polytetrafluoroethylene, polypropylene or polyethylene etc. to form or pottery is formed, and also can adopt the structure comprising aforementioned two or more multiple aperture plasma membrane lamination.
Electrolyte can use a class lithium salts or two classes or more class lithium salt mixture as electrolytic salt.Described lithium salts comprises LiClO 4, LiAsF 6, LiPF 6, LiBF 4, LiB (C 6h 5) 4, CH 3sO 3one in Li, LiCl, LiBr and analog.
There is a lithium battery manufacture method for high cycle characteristics, comprise following steps:
Step 510: form positive pole and close.
Positive active material is become anode mixture with conductive agent and adhesive agent hybrid modulation;
Step 520: form anode mixture slurries
Anode mixture is scattered in solvent the anode mixture material forming paste;
Step 530: form positive pole
Anode mixture slurry is coated on the two sides of metal tinfoil paper positive electrode collector, and waits after its drying, compression forming and form positive pole; .
Step 610: form cathode agent
Negative electrode active material is mixed with conductive agent and adhesive agent and is modulated into cathode agent;
Step 620: form cathode agent slurries
Cathode agent is scattered in solvent the cathode agent slurry forming paste;
Step 630: form a negative pole
Cathode agent is coated in metal forming negative electrode collector two sides, and waits after its drying, compression forming and form this negative pole.Wherein, negative pole negative electrode active material layer by 20 to 50wt% carbon, the copper of 5 to 20wt%, the phosphorus of 1 to 5wt% and add up to the tin of 100 percentage by weights (Sn) to form with aforementioned elements;
Step 710: configure a separator
Separator is wound in positive pole and negative pole, and positive pole and negative pole and separator are housed in battery can inside;
Step 720: configure an electrolyte
Electrolyte is injected the inside of battery can, make it soak separator;
Step 730: form lithium battery
Lithium battery is completed via above-mentioned steps two;
The making of negative pole comprises the following step:
Step 631: form mixed powder
Get appropriate tin, copper, phosphor powder form a mixed powder;
Step 623: form tin-copper-phosphorus alloy material
Total at an inert gas environment, this mixed powder is added thermosetting one tin-copper-phosphorus alloy material;
Step 633: form tin-copper-phosphorus alloy powder
Again in inert gas environment, cooling tin-copper-phosphorus mixture material is also placed on ball mill grinding in ball mill, and obtains tin-copper-phosphorus alloy powder.
Wherein, in step 631, also can pass into inert gas, inert gas can be following gas: nitrogen (N 2), argon gas (Ar), carbon monoxide (Co) and carbon dioxide (CO 2).When certain inert gas is nitrogen, effect is best.In addition, in step 632, heating-up temperature is at least 300 0c; When heating-up temperature is 300 0c to 1100 0between C, effectiveness comparison is good; When temperature is 700 0during C, effect is best.
At the battery of this high cycle characteristics, when charging, discharge lithium ion by positive pole, electrolyte by lithium ion transport to negative pole can occlusion and release lithium negative material.When continuing charging again, at open circuit voltage lower than under overcharged voltage state, start lithium metal to separate out to can the surface of negative material of occlusion and release lithium.When then to put, first, discharge lithium ion by negative pole, lithium ion by electrolyte transport to positive pole and by institute's occlusion.When continuing electric discharge again, then continue release lithium ion containing the negative material of lithium in negative pole, the lithium ion discharged continues by electrolyte transport to positive pole and by positive pole occlusion.
Specific embodiment 1:
The present embodiment citing makes positive active material.First the ferric nitrate of 0.2 mole is added in 200ml deionized water and dissolve, the phosphoric acid of 0.2 mole is added after staying dissolving completely, again the pre-configured argon lithia aqueous solution 100ml containing 0.2 mole is added mixing, make lithium ion in solution: iron ion: phosphate anion is according to LiFePO 4metered proportions (1:1:1) mixing, after complete hybrid reaction, form one containing Fe metal ion, Li +and (PO 4) 3-solution; Namely Powdered starting material is obtained again by after this solution drying.Make thing be placed in alumina crucible by this pulverous, then this crucible is placed in microwave agglomerating furnace with the microwave frequency of 2.45GHz, make it under a nitrogen with 700 0c and process 0.5 hour and obtain can be used as the iron lithium phosphate powder of positive active material.
Specific embodiment 2:
Make negative electrode active material layer.First, after the tin powder of the graphitic carbon powder of 35g, the copper powders of 15g, the phosphor powder of 2g and 52g fully being mixed, a mixture is obtained.Lid mixture is placed in quartz boat, a grinding of ball grinder 20 hours in nitrogen, is pulverized thus and obtain copper-phosphorus-carbon-tin powder.
Specific embodiment 3:
Make lithium battery method.First by the iron lithium phosphate powder obtained by embodiment 1 and carbon black and poly-difluoroethylene binder, after (83:10:7) mixes to scale, overlayed on 10um aluminium foil, through 120 0c obtains positive pole after drying 6 hours.And by the copper-phosphorus-carbon-tin powder obtained by embodiment 2 and carbon black and poly-difluoroethylene adhesive, after her ratio (83:10:7) mixes, overlayed on 10um aluminium foil, through 120 0c obtains negative pole after drying 6 hours.
Form separator according to after the order lamination of negative pole, separator and positive pole by micro-porous polyethylene film of rear 25um, repeatedly reel.Then, the 4-fluorine of 40 percentage by weights is mixed, the carbonic acid diformazan grease (DMC) of 3-dioxolane-2-ketone (FEC), 45 percentage by weights, the electrolyte LiPF of 15 percentage by weights 6and modulate electrolyte.And after positive pole and negative pole being contained in the inside of battery can, electrolyte being injected the inside with battery can, make its impregnation separator, to form lithium battery, then test its discharge and recharge character by charge-discharge test machine.
Specific embodiment 4:
Prepare positive pole and a series of negative pole with the method identical with specific embodiment 2, in heating process, add carbon as conductive materials, say the LiFePO of 90wt% 4and the carbon of 10wt% mixes and forms positive active material LiFePO 4/ C, and be made into positive pole further.
Make various lithium battery according to above-described embodiment, and measure its discharge voltage and charge and discharge capacitance sustainment rate, as shown in following table 1, table 2.
Table 1
As shown in table 1, using identical positive active material LiFePO 4under, there is the relation of the negative pole of different components content and the capacity of lithium battery and cycle characteristics.Can be found by embodiment 2-4 to 2-6, fix and change the percentage 3 of copper and phosphorus when carbon content, along with the increase of copper and phosphorus composition, electric capacity sustainment rate becomes downward trend on the contrary.And capacitance, without significantly change, has stable characteristic as seen when initial discharge.When the percentage by weight of the C-Cu-P-Sn in negative electrode active material is respectively 45-15-2-38, lithium battery all has good electric capacity sustainment rate in high capacity or low load.
Table 2
As shown in table 2, in positive pole thing material, add material with carbon element, and when negative material constituent is the same with table 1, result display has identical trend with when not adding material with carbon element in positive active material.But integral capacitor amount sustainment rate, when high capacity or underload, all has obvious liter, especially first capacitance is increased to 3300mAh.

Claims (10)

1. an ion battery negative electrode active material, is characterized in that, comprises carbon (C), copper (Cu), phosphorus (P) and tin (Sn).
2. ion battery negative electrode active material according to claim 1, it is characterized in that, mass percent shared by described carbon, copper, phosphorus and tin, carbon (C) is 20 to 50wt%, copper (Cu) is 5 to 20wt%, phosphorus (P) is 1 to 5wt%, and tin (Sn) is for add up to 100 percentage by weights with aforementioned elements; Wherein " wt% " represents mass percent.
3. ion battery negative electrode active material according to claim 1, it is characterized in that, mass percent shared by described carbon, copper, phosphorus and tin, carbon (C) is 35 to 45wt%, copper (Cu) is 15 to 20wt%, phosphorus (P) is 2 to 4wt%, and tin (Sn) is for add up to 100 percentage by weights with aforementioned elements; Wherein " wt% " represents mass percent.
4. ion battery negative electrode active material according to claim 1, is characterized in that, negative electrode active material also comprises conductive agent, the glutinous material such as bonding agent or viscosity adjusters, and wherein said conductive agent is graphite fibre or metallic fiber or metal dust; Described adhesive is vinylidene fluoride or styrene butadiene ribber or ethylene propylene diene rubber; Described viscosity adjusters is CMC.
5. ion battery negative electrode active material according to claim 1, rise and it is characterized in that, the thickness of negative electrode active material is between 10um to 200um.
6. a manufacture method for ion battery negative electrode active material as claimed in claim 1, is characterized in that, comprise the following step:
Step 631: form mixed powder
Get appropriate tin, copper, phosphor powder formation mixed powder;
Step 623: form tin-copper-phosphorus alloy material
In an inert gas environment, this mixed powder is added thermosetting one tin-copper-phosphorus alloy material;
Step 633: form tin-copper-phosphorus alloy powder;
Again in inert gas environment, cooling tin-copper-phosphorus mixture material is also placed on ball mill grinding in ball mill, and obtains tin-copper-phosphorus alloy powder.
7. the manufacture method of ion battery negative electrode active material according to claim 6, is characterized in that, in step 631, passes into inert gas, and inert gas can be following gas: nitrogen (N 2), argon gas (Ar), carbon monoxide (Co) and carbon dioxide (CO 2).
8. the manufacture method of ion battery negative electrode active material according to claim 6, is characterized in that, in step 632, heating-up temperature is at least 300 0c.
9. the manufacture method of ion battery negative electrode active material according to claim 6, is characterized in that, in step 632, heating-up temperature is 300 0c to 1100 0c.
10. the manufacture method of ion battery negative electrode active material according to claim 6, is characterized in that, in step 632, heating-up temperature is 700 0c.
CN201310515826.7A 2013-10-29 2013-10-29 Lithium ion battery cathode active substance and manufacturing method thereof Pending CN104577078A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109346712A (en) * 2018-09-10 2019-02-15 澳洋集团有限公司 A kind of preparation method of the copper and tin based alloy nanometer anode material of lithium battery

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109346712A (en) * 2018-09-10 2019-02-15 澳洋集团有限公司 A kind of preparation method of the copper and tin based alloy nanometer anode material of lithium battery

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Application publication date: 20150429