Highly crystalline lithium transition metal oxides

A lithium transition metal and transition metal technology, applied in the field of powdered lithium transition metal oxides, can solve the problems of low no-load voltage, increased precursor cost, poor overcharge stability, etc.

Inactive Publication Date: 2011-07-06
UMICORE AG & CO KG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Complete removal of sulfur is difficult and increases the cost of the precursor
Sulfate impurities are expected to lead to (a) poor overcharge stability a

Method used

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  • Highly crystalline lithium transition metal oxides
  • Highly crystalline lithium transition metal oxides
  • Highly crystalline lithium transition metal oxides

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1: High crystallinity

[0038] a) Li 1+a m 1-a o 2±b M' k S m , where k, m=0 and M=Ni 1-c-d mn c co d .

[0039] where M=Ni 0.53 mn 0.263 co 0.2 The hydroxide MOOH was used as a precursor.

[0040] Samples were prepared at 920°C, 940°C, 960°C and at 967°C. As expected, the BET surface area decreases with increasing temperature. Li:M is essentially the same (all samples have the same unit cell volume). The electrochemical performance improves with temperature, with the best performance at a sintering temperature of approximately 960-970°C.

[0041] figure 1The X-ray diffraction patterns of 4 samples are shown: The sintering temperatures for samples A-D can be found in Table 1 below. The FWHM (full width at half maximum) is shown for (individual) peaks 101, 006, 102, 104, 105, 110, 108, 113 with respect to the scattering angle (degrees), the FWHM values ​​are as described below sure as that. Peak 003 was excluded as it generally showed poorly f...

Embodiment 2

[0064] Example 2: Improved Safety and Lower Basicity of Ca-Containing Cathodes

[0065] Large-scale (several tons) synthesis of Li from mixed transition metal hydroxides 1+a m 1-a o 2 ±b Ca k S m 2 kinds of cathode materials MP1 and MP2, wherein the mixed transition metal hydroxides contain different amounts of Ca and sulfur. In both cases, the stoichiometry is very similar (a=0.05, M=Mn 1 / 3 Ni 1 / 3 co 1 / 3 , ), but the Ca levels were different: MP1 contained 393 ppm Ca, but MP2 had a typical impurity level of 120 ppm Ca (generally found above 50 but below 150 ppm). Other properties (lithium stoichiometry, particle size, BET surface area, X-ray diffraction pattern) are essentially similar.

[0066] The content of soluble base was measured as follows: 100 ml of deionized water was added to 7.5 g of the cathode, followed by stirring for 8 minutes. Typically allowed to settle for 3 minutes, then the solution was removed and passed through a 1 μm syringe filter to yiel...

Embodiment 3

[0084] Example 3: Optimization of adding Ca and sulfur

[0085] This example is used to demonstrate 2 aspects of the present invention:

[0086] (1) it confirms the observation of Example 2 that Ca "neutralizes" the negative effect of high soluble base content in sulfur-containing cathodes, and

[0087] (2) It proves that only the sulfur-containing and calcium-containing samples according to the present invention show overall good performance.

[0088] This example uses metal composition M=Mn 1 / 3 Ni 1 / 3 co 1 / 3 mixed transition metal hydroxide precursors. The precursor is generally low in Ca but contains some sulfur. Sulfur was removed after preparing primary Li-M-oxide samples (Li:M=1.1) by washing. This primary sample was then used as a precursor and made into a matrix as follows:

[0089] (6a): No addition of sulfur and calcium

[0090] (6b): Add 400ppm of Ca

[0091] (6c): Add 0.5wt% SO 4

[0092] (6d): Add 400ppm Ca and 0.5wt% SO 4 ,

[0093] Then re-sinteri...

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Abstract

A powderous lithium transition metal oxide having a layered crystal structure Li1+aM1-aO2+-b M'k Sm with -0.03 < a < 0.06, 0 <= m <= 0.6, m being expressed in mol%, M being a transition metal compound, consisting of at least 95% of either one or more elements of the group Ni, Mn, Co and Ti; M' being present on the surface of the powderous oxide, and consisting of either one or more elements of the group Ca, Sr, Y, La, Ce and Zr, wherein: either k = 0 and M = Ni1-c-dMncCOd, with 0<c<1, and 0<d<1; or 0.015 < k < 0.15, k being expressed in wt% of said lithium transition metal oxide; characterized in that for said powderous oxide, the X-ray diffraction peak at 44.5 +- 0.3 degree, having as index 104, measured with K alpha radiation, has a FWHM value of <= 0.1 degree. By optimizing the sintering temperature of the metal oxide the FWHM value can be minimized.

Description

technical field [0001] The present invention relates to powdered lithium transition metal oxides for use as active cathode materials in rechargeable lithium batteries. More specifically, in Li(Mn-Ni-Co)O 2 In the type of compounds, higher crystallinity is obtained by optimal selection of sintering temperature. Background technique [0002] LiCoO 2 Still the most widely used cathode material for rechargeable batteries. However, there is strong pressure to replace it with other materials for ad hoc reasons. Now, cobalt's scarce resources and concerns about high prices have accelerated this trend. Except LiFePO which has a much lower energy density 4 and Li-Mn-spinel, based on LiNiO 2 layered cathode materials and based on Li(Mn-Ni-Co)O 2 The layered cathode material is an alternative to LiCoO in commercial battery applications 2 the most likely candidate for . It is basically known today that in the quaternary system Li[Li 1 / 3 mn 2 / 3 ]O 2 -LiCoO 2 -LiNiO 2 -LiNi ...

Claims

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Application Information

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IPC IPC(8): C01G45/00C01G51/00C01G53/00C01G23/00
CPCH01M4/505H01M4/525C01G53/50C01P2002/77C01P2006/40C01G51/50C01P2002/74C01P2004/51C01P2006/11C01P2004/61C01P2006/12C01G45/1228Y02E60/122C01P2002/72C01P2004/64C01P2002/52C01G51/42C01P2006/80B82Y30/00Y02E60/10C01G53/00C01G51/00C01G45/00C01G23/00
Inventor 珍斯·马丁·鲍尔森托马斯·劳洪宪杓金基惠
Owner UMICORE AG & CO KG
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