CN1848485A - Method for producing lithium battery positive pole material by carbon-covering method - Google Patents

Method for producing lithium battery positive pole material by carbon-covering method Download PDF

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CN1848485A
CN1848485A CNA200510034031XA CN200510034031A CN1848485A CN 1848485 A CN1848485 A CN 1848485A CN A200510034031X A CNA200510034031X A CN A200510034031XA CN 200510034031 A CN200510034031 A CN 200510034031A CN 1848485 A CN1848485 A CN 1848485A
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carbon
liv
phosphate
source compound
lifepo
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CN100461506C (en
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喻维杰
吕向阳
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RONGDA ELECTRIC POWER MATERIALS CO Ltd GUANGZHOU
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RONGDA ELECTRIC POWER MATERIALS CO Ltd GUANGZHOU
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02E60/10—Energy storage using batteries

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Abstract

The present invention discloses a method for preparing lithium cell positive electrode material LiFePO4, Li3V2 (PO4)3, LiV2O5, LiV2O4 and LiVO2 by using carbon-covering process. Said method includes the following steps: placing the material to be sintered into a crucible or a high-temperature stainless steel container, covering upper surface of said raw material mixture with carbon granules or carbon powder, the covered thickness is 0.2-5cm, sealing said container, placing said material container in a tunnel kiln, high-temperature sintering, cooling so as to obtain the invented anode material.

Description

Method for preparing lithium battery anode material by carbon coating method
Technical Field
The invention relates to a preparation method of a lithium ion battery anode material, in particular to LiFePO4、Li3V2(PO4)3、LiV2O5、LiV2O4And LiVO2A preparation method of the cathode material.
Background
With the progress of science and technology, people have stronger and stronger requirements on movable energy sources. Since the beginning of the last 90 s, lithium ion batteries are considered to be an ideal choice for high-capacity and high-power batteries due to their high energy density and good cycle performance. Lithium intercalation compound positive electrode materials are the most important constituent of lithium ion batteries. Its performance and cost constrain and determine the performance and cost of the battery.
LiCoO2The material is widely applied to small rechargeable batteries, but the material is expensive due to shortage of cobalt resource and LiCoO2The insecurity of overcharge of (a), which determines that it cannot be applied to the manufacture of a large-capacity lithium ion battery. LiMn2O4The material is superior to LiCoO in price and safety performance2The material has low specific capacity, and particularly has poor high-temperature cycle performance, so that the application of the material is limited. LiNiO2The positive electrode material has poor thermal stability and safety performance, and is difficult to apply.
LiFePO of olivine-type structure4After the material is discovered to have the performance of lithium ion deintercalation and intercalation in 1997, the material is widely considered as an ideal anode material of a lithium ion battery because of no toxicity, environmental friendliness, rich and cheap raw material resources, higher specific capacity and good cycle performance, and particularly because the high-temperature stability of the material is the best among all the discovered lithium ion anode materials. Through metal cation doping, carbon coating, conductive metal superfine powder doping and other methodsWith its conductivity, LiFePO4Have begun to be used in the manufacture of notebook computer batteries andan electric bicycle battery. It will be the best choice for the power battery positive electrode material.
Due to LiFePO4In the material, iron is divalent, and under the high-temperature condition, divalent iron ions are very easily oxidized by air or oxygen, and the following reaction occurs:
this makes the preparation of the material very difficult.
From about LiFePO4US5910382, to the latest US6811924, and chinese, japanese and european patents, whether high temperature solid phase reaction, hydrothermal synthesis or mechanical alloying, require protection from oxidation of ferrous ions in a reducing non-oxidizing atmosphere or inert atmosphere during sintering or heat treatment. In the US patent application US2002/0086214A, although mention is made of the preparation of LiFePO by reduction of ferric iron with carbon4However, the preparation process must also be carried out with argon protective gas.
All references to the preparation of LiFePO since 19994The published papers, without exception, employ a reducing non-oxidizing atmosphere or an inert atmosphere to protect against oxidation of ferrous ions.
For Li3V2(PO4)3、LiV2O5、LiV2O4And LiVO2The preparation method of the cathode material also adopts a reducing non-oxidizing atmosphere or an inert atmosphere for protection.
The high-temperature preparation must be carried out in a non-oxidizing atmosphere (such as argon or high-purity nitrogen), the material must be protected in the non-oxidizing atmosphere before being cooled to 100-200 ℃, and the sintering furnace must have good air tightness. Thus, it is impossible to use LiCoO2The tunnel kiln used for sintering is used for continuous production. Batch production is inefficient and requires large amounts of protective gas to be consumed, thereby increasing manufacturing costs.
Disclosure of Invention
The invention aims to provide a method for continuously producing LiFePO by adopting a common tunnel kiln without protection of a reducing non-oxidizing atmosphere or an inert atmosphere4、Li3V2(PO4)3、LiV2O5、LiV2O4And LiVO2The preparation method of the anode material greatly improves the production efficiency and reduces the manufacturing cost.
The technical measures adopted by the invention are as follows:
for LiFePO4、Li3V2(PO4)3、LiV2O5、LiV2O4And LiVO2Preparing the anode material, namely filling the material to be sintered into a crucible or a high-temperature stainless steel container, covering the upper surface of the raw material mixture with carbon particles or carbon powder, wherein the covering thickness is 0.2-5cm, adding a double-layer upper cover with good sealing property into the container, putting the material container on a push plate, and pushing the material container into a tunnel kiln. The material is pushed out from the outlet of the tunnel kiln after being sintered and is cooled by air or wind.
At high temperatures, the coated carbon consumes all of the oxygen in the container and consumes oxygen that may enter the container to protect the sinter from oxidation. At the same time, the following reactions take place at high temperatures:
the CO produced has reducibility, and the CO can reduce metal high-valence ions possibly existing in the material, thereby ensuring that the product is a single pure phase.
Preparation of LiFePO by carbon coating method4、Li3V2(PO4)3、LiV2O5、LiV2O4And LiVO2The positive electrode material is prepared by covering a carbon layer with a certain thickness on a raw material to be sintered, reducing metal ions by utilizing the reducibility of CO generated by carbon reaction at high temperature, and consuming oxygen in a charging container by utilizing carbonto prevent the generated material from being oxidized, and the specific implementation steps are as follows:
(1) for LiFePO4A source of lithiumProportionally mixing the compound, iron source compound and phosphateMixing, wherein the mol ratio of Li to Fe to P is (0.95-1.1) to 1;
for Li3V2(PO4)3Mixing a lithium source compound, a vanadium source compound and phosphate according to a proportion, wherein the molar ratio of Li to V to P is (2.8-3.2) to 2 to 3;
for LiV2O5Mixing a lithium source compound and a vanadium source compound according to a proportion, wherein the molar ratio of Li to V is (0.6-1) to 2;
for LiV2O4Mixing a lithium source compound and a vanadium source compound according to a proportion, wherein the molar ratio of Li to V is (0.6-1.1) to 2;
for LiVO2Mixing a lithium source compound and a vanadium source compound according to a proportion, wherein the molar ratio of Li to V is (0.5-1.2) to 1;
(2) grinding the mixed materials or performing ball milling by adopting a mechanical alloy method to fully and uniformly mix the materials;
(3) loading into a material box, covering a carbon layer with a thickness of 0.5-3cm on the material, and covering the material box with a double-layer upper cover. Placed on a push plate, pushed into a tunnel kiln, or placed in a bell jar kiln. Sintering at the temperature of 500-900 ℃ for 3-50 hours, cooling to 100-200 ℃ after discharging, and pouring out the carbon layer on the surface to obtain the prepared product.
Preparation of LiFePO by carbon coating method4、Li3V2(PO4)3、LiV2O5、LiV2O4And LiVO2The preparation method of the anode material comprises the step of selecting carbon particles, carbon powder or easily carbonized organic matters as the carbon layer.
Preparation of LiFePO by carbon coating method4、Li3V2(PO4)3、LiV2O5、LiV2O4And LiVO2A method for preparing the cathode material, the lithium source compound is selected from Li2CO3LiOH, lithium oxalate, lithium acetate or lithium phosphate.
Preparation of LiFePO by carbon coating method4、Li3V2(PO4)3Method for producing positive electrode material, phosphorusThe acid salt source is selected from ammonium phosphate, ammonium hydrogen phosphate, ammonium dihydrogen phosphate, and LiFePO4Can also be prepared optionallyFrom iron phosphate or ferrous phosphate.
A process for preparing LiFePO cathode material by carbon coating method features that the iron source can be ferrous oxalate, ferric oxide, ferric phosphate or ferrous phosphate.
Preparation of Li by carbon coating method3V2(PO4)3、LiV2O5、LiV2O4And LiVO2The preparation method of the anode material comprises the step of selecting a vanadium source compound from V2O5Or V2O3。
Preparation of LiFePO by carbon coating method4、Li3V2(PO4)3、LiV2O5、LiV2O4And LiVO2The preparation method of the anode material comprises the step of selecting a material box from ceramic materials or high-temperature stainless steel materials.
Drawings
FIG. 1 shows an anode material LiFePO prepared by a carbon coating method4XRD spectrum of (1).
Detailed Description
Example 1
1/3 moles of Fe3 (PO)4)21/3 moles of NH4H2PO4And 0.5 mol of Li2CO3Mixing, placing into corundum crucible, covering a layer of 0.5cm thick carbon powder layer on the material, covering double-layer upper cover on the crucible, placing the crucible on push plate, pushing into tunnel kiln, sintering at 610 deg.C for 8 hr, discharging, cooling, and cooling with fan. After determining that all materials in the crucible are cooled to below 200 ℃, opening a crucible cover, pouring out the upper layer carbon powder, and then taking out the materials to obtain LiFePO4。
Example 2
1/3 moles of Fe3 (PO)4)2And 1/3 moles of Li3PO4After mixing, putting corundum inIn the crucible, a layer of carbon powder layer with the thickness of 0.5cm is covered on the material, a double-layer upper cover is added on the crucible, the crucible is placed on a push plate and pushed into a tunnel kiln, the sintering is carried out for 8 hours at the temperature of 650 ℃, and then the crucible is taken out of the furnace and cooled, and the cooling is accelerated by a fan. After determining that all materials in the crucible are cooled to below 200 ℃, opening a crucible cover, pouring out the upper layer carbon powder, and then taking out the materials to obtain LiFePO4。
Example 3
0.5 mol of Li2CO31 mol of FePO4Mixing, placing into corundum crucible, covering a layer of 1cm thick carbon powder layer on the material, covering double-layer upper cover on the crucible, placing the crucible on push plate, pushing into tunnel kiln, sintering at 620 deg.C for 8 hr, discharging, cooling, and cooling with fan. After determining that all materials in the crucible are cooled to below 200 ℃, opening a crucible cover, pouring out the upper-layer carbon particles, and then taking out the materials to obtain LiFePO4。
Example 4
0.5 mol of Li2CO31 mol FeC2O4.2H2O and 1 mol of NH4H2PO4Mixing, placing into corundum crucible, covering a layer of 1cm thick carbon particle layer on the material, covering double-layer upper cover on the crucible, placing the crucible on a push plate, pushing into a tunnel kiln, sintering at 620 deg.C for 8 hr, discharging, cooling, and cooling with fan. After determining that all materials in the crucible are cooled to below 200 ℃, opening a crucible cover, pouring out the upper-layer carbon particles, and then taking out the materials to obtain LiFePO4。
Example 5
0.5 mol of Fe2O31 mol of NH4H2PO4And 0.5 mol of Li2CO3Mixing, placing into a stainless steel container, covering a layer of 1cm thick carbon particles on the material, covering the container with a double-layer upper cover, placing the crucible on a push plate, pushing into a tunnel kiln, sintering at 610 deg.C for 8 hr, discharging, cooling, and cooling with fan. After determining that all materials in the crucible are cooled to below 200 ℃, opening a crucible cover, pouring out the upper-layer carbon particles, and thentaking out the materials to obtain LiFePO4。
Example 6
Will consist of LiOH2O、FeC2O4.2H2O and NH4H2PO4500 g of ball-milling mixed material prepared by a mechanical alloying method is put into a corundum crucible, and a layer of carbon with the thickness of 1cm is covered on the materialAnd (3) coating the grains, adding a double-layer upper cover to the crucible, putting the crucible on a push plate, pushing the crucible into a tunnel kiln, sintering for 8 hours at 600 ℃, discharging and cooling, and accelerating cooling by a fan. After determining that all materials in the crucible are cooled to below 200 ℃, opening a crucible cover, pouring out the upper-layer carbon particles, and then taking out the materials to obtain LiFePO4。
Example 7
1 mol of V2O53/2 mol of Li2CO3And 3 moles of NH4H2PO4Mixing, placing into corundum crucible, covering a layer of 0.5cm thick carbon powder layer on the material, covering double-layer upper cover on the crucible, placing the crucible on a push plate, pushing into a tunnel kiln, sintering at 800 deg.C for 8 hr, discharging, cooling, and cooling with fan. After all the materials in the crucible are determined to be cooled to below 150 ℃, the crucible cover is opened, the carbon powder on the upper layer is poured out, and then the materials are taken out to obtain Li3V2(PO4)3。
Example 8
1 mol of V2O5And 0.5 mol of Li2CO3Mixing, placing into corundum crucible, covering a layer of 0.5cm thick carbon powder layer on the material, covering double-layer upper cover on the crucible, placing the crucible on push plate, pushing into tunnel kiln, sintering at 650 deg.C for 8 hr, discharging, cooling, and cooling with fan. After determining that all materials in the crucible are cooled to below 150 ℃, opening a crucible cover, pouring out the upper layer carbon powder, and then taking out the materials to obtain LiV2O5。
Example 9
1 mol of V2O50.5 mol of Li2CO3Mixing, placing into corundum crucible, covering with 1cm thick carbon particle layer, covering with double-layer upper cover, pushing the crucibleOn the plate, the plate is pushed into a tunnel kiln, sintered for 8 hours at 700 ℃, taken out of the furnace and cooled, and the cooling is accelerated by a fan. After all the materials in the crucible are determined to be cooled to below 120 ℃, the crucible cover is opened and poured firstlyTaking out upper layer carbon particles, and then taking out materials to obtain LiV2O4。
Example 10
1 mol of V2O31 mol of Li2CO3Mixing, placing into corundum crucible, covering a layer of 1cm thick carbon particle layer on the material, covering double-layer upper cover on the crucible, placing the crucible on a push plate, pushing into a tunnel kiln, sintering at 700 deg.C for 8 hr, discharging, cooling, and cooling with fan. After determining that all materials in the crucible are cooled to below 120 ℃, opening a crucible cover, pouring out upper-layer carbon particles, and taking out the materials to obtain LiVO2。

Claims (7)

1. Carbon-coating method for preparing LiFePO4、Li3V2(PO4)3、LiV2O5、LiV2O4And LiVO2A positive electrode material characterized in that: covering a carbon layer with a certain thickness on the raw material to be sintered, reducing metal ions by utilizing the reducibility of CO generated by carbon reaction at high temperature, and consuming oxygen in a charging container by utilizing carbon to avoid the generated material from being oxidized, wherein the specific implementation steps are as follows:
(1) for LiFePO4Mixing a lithium source compound, an iron source compound and phosphate according to a proportion, wherein the molar ratio of Li to Fe to P is (0.95-1.1) to 1;
for Li3V2(PO4)3Mixing a lithium source compound, a vanadium source compound and phosphate according to a proportion, wherein the molar ratio of Li to V to P is (2.8-3.2) to 2 to 3;
for LiV2O5Mixing a lithium source compound and a vanadium source compound according to a proportion, wherein the molar ratio of Li to V is (0.6-1) to 2;
for LiV2O4A lithium source compound and a vanadium sourceMixing the compounds in proportion, wherein the molar ratio of Li to V is (0.6-1.1) to 2;
for LiVO2Mixing a lithium source compound and a vanadium source compound according to a proportion, wherein the molar ratio of Li to V is (0.5-1.2) to 1;
(2) grinding the mixed materials or performing ball milling by adopting a mechanical alloy method to fully and uniformly mix the materials;
(3) loading into a material box, covering a carbon layer with a thickness of 0.5-3cm on the material, and covering the material box with a double-layer upper cover. Placed on a push plate, pushed into a tunnel kiln, or placed in a bell jar kiln. Sintering at the temperature of 500-900 ℃ for 3-50 hours, cooling to 100-200 ℃ after discharging, and pouring out the carbon layer on the surface to obtain the prepared product.
2. The carbon coating method for preparing LiFePO according to claim 14、Li3V2(PO4)3、LiV2O5、LiV2O4And LiVO2The preparation method of the anode material is characterized in that the carbon layer is made of carbon particles, carbon powder or easily carbonized organic matters.
3. The carbon coating method for preparing LiFePO according to claim 14、Li3V2(PO4)3、LiV2O5、LiV2O4And LiVO2The preparation method of the cathode material is characterized in that the lithium source compound is selected from Li2CO3LiOH, lithium oxalate, lithium acetate or lithium phosphate.
4. The carbon coating method for preparing LiFePO according to claim 14、Li3V2(PO4)3The preparation method of the anode material is characterized in that the phosphate source is selected from ammonium phosphate, ammonium hydrogen phosphate and ammonium dihydrogen phosphate, and LiFePO is used4Can also be selected from iron phosphate or ferrous phosphate.
5. The method for preparing LiFePO cathode material according to the carbon coating method of claim 1, wherein the iron source is selected from the group consisting of ferrous oxalate, ferric oxide, ferric phosphate and ferrous phosphate.
6. The carbon-coating method for preparing Li according to claim 13V2(PO4)3、LiV2O5、LiV2O4And LiVO2The preparation method of the cathode material is characterized in that the vanadium source compound is selected from V2O5Or V2O3。
7. The carbon coating method for preparing LiFePO according to claim 14、Li3V2(PO4)3、LiV2O5、LiV2O4And LiVO2The preparation method of the cathode material is characterized in that the material box is made of ceramic materials or high-temperature stainless steel materials.
CNB200510034031XA 2005-04-12 2005-04-12 Method for producing lithium battery positive pole material by carbon-covering method Expired - Fee Related CN100461506C (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103367743A (en) * 2012-03-27 2013-10-23 Tdk株式会社 Positive electrode material for lithium ion secondary battery, positive electrode for lithium ion secondary battery, and lithium ion secondary battery
US20150283532A1 (en) * 2011-12-22 2015-10-08 Belenos Clean Power Holding Ag Coating and lithiation of inorganic oxidants by reaction with lithiated reductants
CN106159241A (en) * 2016-08-31 2016-11-23 四川剑兴锂电池有限公司 A kind of anode pole piece and the amorphous carbon lithium battery containing this positive plate

Family Cites Families (4)

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JP4491946B2 (en) * 2000-09-29 2010-06-30 ソニー株式会社 Method for producing positive electrode active material and method for producing non-aqueous electrolyte battery
CN1401559A (en) * 2002-10-18 2003-03-12 北大先行科技产业有限公司 Method for preparing ferrous lithium phosphate, and lithium ion cell therewith
US7901810B2 (en) * 2003-06-03 2011-03-08 Valence Technology, Inc. Battery active materials and methods for synthesis
CN1255887C (en) * 2004-03-25 2006-05-10 浙江大学 Method of preparing positive electrode composite material of lithium ion cell contg, ferrous phosphate lithium salt-carbon

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150283532A1 (en) * 2011-12-22 2015-10-08 Belenos Clean Power Holding Ag Coating and lithiation of inorganic oxidants by reaction with lithiated reductants
US11031583B2 (en) 2011-12-22 2021-06-08 Belenos Clean Power Holding Ag Coating and lithiation of inorganic oxidants by reaction with lithiated reductants
CN103367743A (en) * 2012-03-27 2013-10-23 Tdk株式会社 Positive electrode material for lithium ion secondary battery, positive electrode for lithium ion secondary battery, and lithium ion secondary battery
CN106159241A (en) * 2016-08-31 2016-11-23 四川剑兴锂电池有限公司 A kind of anode pole piece and the amorphous carbon lithium battery containing this positive plate

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