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Carbonated complex oxides and method for making the same

A compound, carbon film technology, used in chemical instruments and methods, phosphorus compounds, electrode heat treatment, etc., can solve problems such as quality degradation, product vicious changes, battery cyclability or harmful charge potential

Inactive Publication Date: 2009-10-14
福斯泰克锂公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the inventors have surprisingly noticed that LiFePO with carbon deposition 4 , especially powdered LiFePO with high specific surface area 4 , or LiFePO in the form of a coating of the current collector in order to form the cathode 4 , its quality degrades during exposure to air or during operation or storage
This leads to a deleterious change in the product or the formation of impurities which in turn can have a detrimental effect on the cyclability or charge potential of batteries containing phosphate

Method used

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  • Carbonated complex oxides and method for making the same
  • Carbonated complex oxides and method for making the same
  • Carbonated complex oxides and method for making the same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1a

[0081] C-LiFePO 4 Synthesis

[0082] Preparation containing stoichiometric amounts of FePO 4 ·(H 2 O) 2 (1mol, purchased from Budenheim, grade E53-81) and Li 2 CO 3 (1mol, purchased from Limtech, purity 99.9%), and a mixture of 5% polyethylene block polyethylene glycol (purchased from Aldrich) containing 50% ethylene oxide, and it was added to isopropanol, mixed About 10h, then remove the solvent. In the material thus obtained, the polymer holds the phosphate and carbonate particles together.

[0083]The mixture was treated under nitrogen flow at 700 °C for 2 h to obtain the battery-grade material C-LiFePO 4 , followed by vacuum drying at 100 °C, and the final material was stored in a glove box under an argon atmosphere with a dew point of -90 °C.

[0084] The specific surface area of ​​the material is 13.6m 2 / g, the carbon content is 1.8% by weight.

[0085] Ground material C-LiFePO 4 sensitivity to water

[0086] The material obtained was jet-milled under compre...

Embodiment 1b

[0091] C-LiFe 0.5 mn 0.5 PO 4 Synthesis

[0092] By adding a stoichiometric amount of the precursor LiH 2 PO 4 , FeC 2 o 4 2H 2 O and (CH 3 COO) 2 Mn 4H 2 O mixed to prepare the compound LiFe 0.5 mn 0.5 PO 4 . The mixture was subsequently triturated in heptane, then dried in air and gradually heated to 40 °C to decompose the acetate and oxalate groups. The temperature was maintained for 8 hours. During the treatment, iron (II) is oxidized to iron (III).

[0093] The mixture was then ground again in an acetone solution containing 39.7% by weight of acetyl groups and 5% of cellulose acetate (carbon precursor) relative to the mixture.

[0094] After drying, the mixture was heated to 700°C in a tube furnace at a rate of 6°C / min. The temperature was maintained for 1 hour, and then the sample was cooled for 40 minutes, ie, the sample was cooled at a cooling rate of about 15° C. / minute. Keep the tube furnace under reducing gas flow (CO / CO 2 : 1 / 1).

[0095] In thi...

Embodiment 1c

[0099] C-LiFe 0.98 Mg 0.02 PO 4 Synthesis

[0100] Preparation of compound LiFe by melting method 0.98 Mg 0.02 PO 4 . Mix compound Fe in a molar ratio of 0.49 / 0.5 / 0.98 / 0.02 2 o 3 , Li 2 CO 3 , NH 4 ) 2 HPO 4 and MgHPO 4 , the mixture was then heated to 980° C. under argon in a graphite crucible, held at this temperature for 1 hour to melt it, and then cooled to about 50° C. within 3 hours.

[0101] The thus obtained compound LiFe was then 0.98 Mg 0.02 PO 4 at 90cm 3 12 g of zirconia beads with a diameter of 20 mm in isopropanol for 10 minutes and then 440 g of zirconia beads with a diameter of 3 mm for 90 minutes to obtain a powder with an average particle size of 1.12 μm.

[0102] The LiFe obtained after grinding 0.98 Mg 0.02 PO 4 The powder was mixed with 7% by weight of cellulose acetate, then dried and treated at 700 °C under argon for 1 hour to obtain carbon deposits containing 1.32% by weight and a specific surface area of ​​19.2 m 2 / g material C-L...

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Abstract

The invention relates to a method for preparing a carbonated complex oxide having a very low water content, and to the use thereof as a cathode material. The carbonated complex oxide is made of particles of an olivine-structure AMXO4 compound bearing on a portion at least of their surface a carbon film deposited by pyrolysis. A is Li alone or partially replaced with at most 10 at % of Na or K. M is FeII alone or partially replaced with at most 50 at % of one or more other metals selected from Mn, Ni and Co and / or with at most 10 at % of one or more aliovalent or isovalent metals other than Mn, Ni or Co and / or with at most 5 at % of FeIII. XO4 is PO4 alone or partially replaced with at most 10 molar % of SO4 and SiO4. The material has a water content lower than 1000 ppm.

Description

technical field [0001] The present invention relates to a process for the preparation of carbon-treated composite oxides having a very low water content, and their use as cathode materials. Background technique [0002] During the last 20 years, lithium-ion batteries have become the main energy sources of mobile electronic devices due to their high energy density and high cycle life. However, unlike using LiCoO on the cathode 2 Associated safety concerns limit the possibility of developing reliable lithium-ion batteries on a large scale. There are proposals to replace LiCoO with lithium iron phosphate 2 As cathode material (cf. US-5 910 382, ​​US-6 391 493 and US-6 514 640). The safety issue is thus resolved by the P-O covalent bond, which stabilizes the fully charged cathode in terms of oxygen release. Phosphate LiFePO with olivine structure 4 show non-optimal kinetics induced by low intrinsic conductivity due to PO 4 Polyanions are responsible for the covalent bonds....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58C01B32/80H01M10/0525H01M10/36
CPCY02E60/122H01M4/5825H01M10/0525C01B25/45Y02E60/10C01B32/80H01M4/58H01M4/0402H01M4/0471H01M4/136H01M4/1397H01M4/622H01M4/625H01M2004/028H01M2220/30
Inventor N·拉韦M·戈捷T·拉尔斯梁国宪C·米绍
Owner 福斯泰克锂公司
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