Lithium cobalt oxides and methods of making same

FIELD OF THE INVENTION

The present invention relates to lithium cobalt oxides for use as positive electrode materials for rechargeable lithium and lithium-ion secondary batteries, and to methods of making lithium cobalt oxides.

BACKGROUND OF THE INVENTION

LiCoO

2

is currently being used in over 95% of commercial lithium and lithium-ion secondary batteries as the active positive electrode material. The current production rate of lithium and lithium-ion batteries is about 30 million units per month with each unit containing about 10-15 g of LiCoO

2

(i.e., 300-450 metric tons/month).

LiCoO

2

can be made by a number of different methods by reacting a lithium salt and a cobalt salt. However, these methods often involve lengthy reaction times thereby reducing the rate of LiCoO

2

production.

Therefore, there is a need in the art to provide a method of preparing LiCoO

2

that demonstrates good performance in rechargeable lithium and lithium-ion secondary batteries and that can be produced with a relatively short reaction time.

SUMMARY OF THE INVENTION

The present invention includes lithium cobalt oxides having hexagonal layered crystal structures and methods of making same. The lithium cobalt oxides of the invention have the formula Li

w

Co

1−x

A

x

O

2+y

wherein 0.96≦w≦1.05, 0≦x≦0.05, −0.02≦y≦0.02 and A is one or more dopants. Preferably, 0.98≦w≦1.02 and 0≦x≦0.02.

The lithium cobalt oxides of the invention preferably have a position within the principal component space defined by the following relationship:

ax

i

+by

i

≦c

wherein x

i

={right arrow over (S)}

i

&Circlesolid;{right arrow over (P)}

c1

; y

i

={right arrow over (S)}

i

&Circlesolid;{right arrow over (P)}

c2

; the vector {right arrow over (S)}

i

is the x-ray spectrum for the Li

w

Co

1−x

A

x

O

2+y

compound; the vectors {right arrow over (P)}

c1

and {right arrow over (P)}

c2

are determined by measuring the x-ray powder diffraction values {right arrow over (S)}

i

between 15° and 120° using a 0.020 step size and CuKα rays for a large sample set of lithium cobalt oxides and using the regression of {right arrow over (S)}

i

of the sample set against the capacity fade after 50 cycles of a lithium coin cell that includes a lithium negative electrode and the lithium cobalt oxide as the positive electrode material and that is cycled between 3.0 and 4.3V at a constant current of C/3 during both charge and discharge cycles; and the values a, b and c are determined by using only the x

i

and y

i

values for Li

w

Co

1−x

A

x

O

2+y

compounds in the sample set that have a capacity fade after 50 cycles of less than or equal to 15%.

More preferably, the lithium cobalt oxides of the invention have a position within the principal component space defined by the following relationship:

x

i

+0.77

y

i

≦−6

wherein x

i

={right arrow over (S)}

i

&Circlesolid;{right arrow over (P)}

c1

; y

i

={right arrow over (S)}

i

&Circlesolid;{right arrow over (P)}

c2

; {right arrow over (S)}

i

is the x-ray spectrum for the Li

w

Co

1−x

A

x

O

2+y

compound; and {right arrow over (P)}

c1

and {right arrow over (P)}

c2

are determined by measuring the x-ray powder diffraction values sh between 15° and 120° using a 0.020 step size and CuKα rays for a large sample set of lithium cobalt oxides and using the partial least squares regression (PLSR) of {right arrow over (S)}

i

of the sample set against the capacity fade after 50 cycles of a lithium coin cell that includes a lithium negative electrode and the lithium cobalt oxide as the positive electrode material and that is cycled between 3.0 and 4.3V at a constant current of C/3 during both charge and discharge cycles. For example, {right arrow over (P)}

c1

and {right arrow over (P)}

c2

can be defined by the coefficients provided in Table 1 (wherein 2θ is the scattering angle of x-ray powder diffraction measurements using CuKα rays).

The lithium cobalt oxides of the invention can be used in the positive electrode of a rechargeable lithium or lithium-ion secondary battery in accordance with the invention. For the lithium cobalt oxides of the invention, the capacity fade of a lithium coin cell having a lithium negative electrode and using the lithium cobalt oxide as the positive electrode material when cycled between 3.0 and 4.3V at a constant current of C/3 during both charge and discharge cycles after 50 charge/discharge cycles is preferably less than or equal to 15%, more preferably less than or equal to 10%. Moreover, the initial specific discharge capacity is preferably greater than or equal to 154 mAh/g.

The lithium cobalt oxides of the invention are prepared by heating a lithium source compound, a cobalt source compound and optionally one or more source compounds that include dopants A at a temperature below about 850° C. to produce Li

w

Co

1−x

A

x

O

2+y

and heating the Li

w

Co

1−x

A

x

O

2+y

compound at a temperature from about 900° C. and 1000° C. to form and enhance the hexagonal layered crystal structure of the Li

w

Co

1−x

A

x

O

2+y

compound. The temperature in the first heating step is preferably from about 500° C. to about 850° C. and the temperature in the second heating step is preferably from about 950° C. to about 980° C. The source compounds in the first heating step can be heated at more than one temperature below about 850° C. In addition, the Li

w

Co

1−x

A

x

O

2+y

compound in the second heating step can be heated at more than one temperature from about 900° C. to about 1000° C. Preferably, the first heating step comprises heating the source compounds for a period of time of from about 30 minutes to about 3 hours and the second heating step comprises heating the source compounds for a period of time of from about 30 minutes to about 7 hours. The lithium source compound preferably used with the invention is selected from the group consisting of Li

2

CO

3

and LiOH and the cobalt source compound is preferably selected from the group consisting of Co

3

O

4

and Co(OH)

2

. The lithium cobalt oxide is preferably cooled after the heating steps at a rate of from 8° C./min to 140° C./min, more preferably from 10° C./min to 100° C./min.

The present invention further includes a method of analyzing a compound to determine if the compound is suitable for use as the active positive electrode material in a lithium or lithium-ion secondary battery. The method of the invention comprises determining a principal component space defined by the relationship ax

i

+by

i

≦c, wherein x

i

={right arrow over (S)}

i

&Circlesolid;{right arrow over (P)}

c1

; y

i

={right arrow over (S)}

i

&Circlesolid;{right arrow over (P)}

c2

; the vector {right arrow over (S)}

i

is the x-ray spectrum for the compound; the vectors {right arrow over (P)}

c1

and {right arrow over (P)}

c2

are determined by measuring the x-ray powder diffraction values {right arrow over (S)}

i

for a predetermined range of 2θ values using a predetermined step size by sampling a plurality of samples of compounds having the same general formula as the compound and using the regression of {right arrow over (S)}

i

of the sample set against predetermined battery performance data for the samples by incorporating the samples as the positive electrode active material in a lithium or lithium-ion secondary battery. The x

i

and y

i

values for the compounds in the sample set that have the predetermined battery performance data are then used to determine a, b and c. The compound is analyzed by measuring the x-ray diffraction spectra for the compound to obtain x and y values and determining whether the x and y values meet the relationship ax

i

+by

i

≦c and thus whether the compound possesses the battery performance and x-ray diffraction spectra suitable for use as the active positive electrode material.

The lithium cobalt oxides of the invention have good cycleability properties including good initial specific capacities and capacity fades and thus are desirable for use in rechargeable lithium and lithium-ion batteries. In addition, the lithium cobalt oxides of the present invention can be produced quickly in less than 10 hours and thus can be produced at a rate desired in the art.

These and other features and advantages of the present invention will become more readily apparent to those skilled in the art upon consideration of the following detailed description, which describes both the preferred and alternative embodiments of the present invention.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1

illustrates the positions of several samples in a principal component space as defined by the axes {right arrow over (P)}

c1

and {right arrow over (P)}

c2

with the dotted line representing x+0.77y=−6 in accordance with a preferred embodiment of the invention.

FIG. 2

illustrates the capacity fade after 50 cycles versus x+0.77y with the dotted line defining the principal component space of the samples of the invention having the desired x-ray powder diffraction values and a fade of less than or equal to 15% in accordance with a preferred embodiment of the invention.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS OF THE INVENTION

In the following detailed description, preferred embodiments are described in detail to enable practice of the invention. Although the invention is described with reference to these specific preferred embodiments, it will be understood that the invention is not limited to these preferred embodiments. But to the contrary, the invention includes numerous alternatives, modifications and equivalents as will become apparent from consideration of the following detailed description and accompanying drawings.

The present invention is directed to lithium cobalt oxides having the formula Li

w

Co

1−x

A

x

O

2+y

wherein 0.96≦w≦1.05, 0≦x≦0.05, −0.02≦y≦0.02 and A is one or more dopants. Preferably, 0.98≦w≦1.02 and 0≦x≦0.02. The dopants A are elements other than Co including metals and non-metals such as Ni, Mn, Ti, Zr, V, Mo, Mg, Ca, Sr, Ba, Al, Ga, Si, Ge, Sn, and combinations thereof. Preferably, the dopants A are selected to produce an oxidation state N wherein +2.5≦N≦+3.5, and preferably N is about 3. The average oxidation state N is based on the molar amounts of the dopants used and the valences of the dopants used. For example, if the dopants are 40% Ti

4+

and 60% Mg

2+

, on a molar basis, the average oxidation state N would be (0.4)(+4)+(0.6)(+2)=+2.8.

The lithium cobalt oxides of the invention have a hexagonal layered crystal structure that is substantially single-phase and substantially free of localized cubic spinel-like structural phases on the surface of the crystal or within the crystal. The substantially single-phase, hexagonal layered structures of the compounds of the invention can be characterized, for example, by their powder x-ray diffraction patterns.

The lithium cobalt oxides of the present invention preferably have an initial specific discharge capacity of greater than or equal to 154 mAh/g and a capacity fade after 50 cycles of less than or equal to 15%. Specifically, when the lithium cobalt oxides are used as the positive electrode material in a lithium coin cell having a lithium negative electrode and the cell is cycled between 3.0 and 4.3V at a constant current of C/3 (3 hours for complete charge or discharge) during both the charge and discharge cycles, the cells have a capacity fade of less than or equal to 15% after 50 charge/discharge cycles. In these coin cells, NRC 2325 coin cell hardware and Celgard 3501 separators can be used. The electrolyte is typically 1M LiPF

6

in a 50:50 mixture of ethylene carbonate and dimethyl carbonate solvents. In addition, the positive electrode consists generally of 85% active material (by weight), 10% super S™ carbon black and 5% polyvinylidene fluoride (PVDF) as a binder polymer, coated on aluminum foil.

The lithium cobalt oxides of the invention have a capacity fade of less than or equal to 15% after 50 cycles and can also be characterized by their x-ray powder diffraction patterns, which describe the crystal properties of the lithium cobalt oxides. In particular, the lithium cobalt oxides of the invention can be characterized by their positions in a principal component space determined by conducting principal component analysis of x-ray powder diffraction spectra between 15° and 120° using a 0.02° step size and CuKα rays. In the principal component analysis, each x-ray spectrum is treated as a vector {right arrow over (S)}

i

.

It has been discovered using this principal component analysis that the crystal properties that are important to the rechargeable lithium battery performance can be described in the space defined generally by two vectors, namely, principal components {right arrow over (P)}

c1

and {right arrow over (P)}

c2

. These two vectors are preferably determined by using the partial least squares regression of {right arrow over (S)}

i

of a large sample set against the battery performance of the sample. This sample set includes lithium cobalt oxides having a capacity fade of less than or equal to 15% and lithium cobalt oxides having a capacity fade of greater than 15%.

The principal component space that includes the compounds of the invention having a capacity fade of less than or equal to 15% can be defined by the following relationship:

ax

i

+by

i

≦c

wherein x

i

={right arrow over (S)}

i

&Circlesolid;{right arrow over (P)}

c1

(i.e. the projection of {right arrow over (S)}

i

onto {right arrow over (P)}

c1

); y

i

={right arrow over (S)}

i

&Circlesolid;{right arrow over (P)}

c2

(i.e. the projection of {right arrow over (S)}

i

onto {right arrow over (P)}

c2

); the vector {right arrow over (S)}

i

is the x-ray spectrum for the Li

w

Co

1−x

A

x

O

2+y

compound. The vectors {right arrow over (P)}

c1

and {right arrow over (P)}

c2

defining the principal component space can be determined by measuring the x-ray powder diffraction values {right arrow over (S)}

i

between 15° and 120° using a 0.02° step size and CuKα rays for a large sample set of lithium cobalt oxides and using the regression of {right arrow over (S)}

i

of the sample set against the capacity fade after 50 cycles of a lithium coin cell that includes a lithium negative electrode and the lithium cobalt oxide as the positive electrode material and that is cycled between 3.0 and 4.3V at a constant current of C/3 during both charge and discharge cycles. The values a, b and c of the above relationship can then be determined by using the x

i

and y

i

values for Li

w

Co

1−x

A

x

O

2+y

compounds in the sample set that have a capacity fade after 50 cycles of less than equal to 15%, i.e., the Li

w

Co

1−x

A

x

O

2+y

compounds prepared according to the invention.

The vector {right arrow over (S)}

i

is the x-ray diffraction spectrum of the ith sample and can be written as

{\vec{S}}_{i} = (\begin{matrix} ⋮ \\ s_{ij} \\ ⋮ \end{matrix})

where the element S

ij

is the jth data point in the x-ray diffraction spectrum. In a partial least squares regression, the vector {right arrow over (S)}

i

is autoscaled before the regression takes place. The autoscaling of {right arrow over (S)}

i

is defined by

\vec{S_{i}^{as}} = (\begin{matrix} ⋮ \\ s_{ij}^{as} \\ ⋮ \end{matrix})

where the autoscaled element

s_{ij}^{as} = \frac{s_{ij} - {\overline{s}}_{j}}{{(\frac{1}{n - 1} \overset{n}{\sum_{i}} {(s_{ij} - {\overline{s}}_{j})}^{2})}^{1 / 2}}

and {overscore (s)}

j

is the mean of s

ij

.

In the preferred embodiment of the invention, the regression is carried out with the commercial software Pirouette 2.7 available from Infometrix Inc., and the details of the matrix bidiagonalization algorithm is described in R. Manne, “Analysis of two partial least squares algorithms for multivariate calibration”, Chemom. Intell. Lab. Syst. 2, 187-197 (1987).

In accordance with a preferred embodiment of the invention, by using principal component analysis, the lithium cobalt oxides of the invention have a position within the principal component space defined by the following relationship:

x

i

+0.77

y

i

≦−6

wherein x

i

={right arrow over (S)}

i

&Circlesolid;{right arrow over (P)}

c1

; y

i

={right arrow over (S)}

i

&Circlesolid;{right arrow over (P)}

c2

; {right arrow over (S)}

i

is the x-ray spectrum for the Li

w

Co

1−x

A

x

O

2+y

compound; and {right arrow over (P)}

c1

and {right arrow over (P)}

c2

are determined by measuring the x-ray powder diffraction values {right arrow over (S)}

i

between 15° and 120° using a 0.02° step size and CuKα rays for a large sample set of lithium cobalt oxides and using the partial least squares regression (PLSR) of {right arrow over (S)}

i

of the sample set against the capacity fade after 50 cycles of a lithium coin cell that includes a lithium negative electrode and the lithium cobalt oxide as the positive electrode material and that is cycled between 3.0 and 4.3V at a constant current of C/3 during both charge and discharge cycles. In particular, the vectors {right arrow over (P)}

c1

and {right arrow over (P)}

c2

can be defined by the coefficients provided in Table 1 below (wherein 2θ is the scattering angle for the x-ray powder diffraction measurements using CuKα rays). These measurements where obtained using a Rigaku RINT-2000 unit that includes a graphite monochrometer, a rotating anode x-ray source having a current of 150 mA and a voltage of 50 kV, anti-scattering slits set at 0.50, and anti-divergence slits set at 0.5°. Alternative x-ray diffraction apparatus can also be used that produce comparable measurements to those produced with the above equipment and parameters.

TABLE 1

Coefficients of

Principal

Components

2θ (°)

P

c1

P

c2

15

−0.013790

0.011723

15.02

−0.02049

0.005086

15.04

0.006858

−0.020376

15.06

−0.00273

0.013492

15.08

−0.01666

0.000753

15.1

0.000904

0.016155

15.12

−0.02289

0.001471

15.14

0.018222

0.020191

15.16

−0.00612

0.017684

15.18

−0.01378

0.008202

15.2

−0.0095

0.014128

15.22

−0.00584

0.010502

15.24

−0.00241

0.014185

15.26

−0.0042

0.014822

15.28

−0.00359

0.010447

15.3

−0.01418

0.009492

15.32

−0.01268

0.006936

15.34

−0.01096

0.001104

15.36

−0.00484

0.013178

15.38

−0.02337

−0.00186

15.4

−0.0185

0.005159

15.42

−0.01369

0.007337

15.44

−0.00748

0.015817

15.46

−0.00627

0.009999

15.48

0.002923

0.016611

15.5

−0.0327

−0.00277

15.52

−0.00977

0.009888

15.54

−0.01803

0.005404

15.56

−0.0272

−0.00066

15.58

−0.01839

0.006056

15.6

−0.0327

0.000501

15.62

0.001235

0.010506

15.64

0.004628

0.021154

15.66

−0.01218

0.011076

15.68

−0.01306

0.005821

15.7

0.017059

0.026611

15.72

−0.00215

0.017464

15.74

−0.0196

0.00594

15.76

−0.00819

0.015374

15.78

−0.00688

0.011794

15.8

0.01031

0.017391

15.82

−0.01997

−0.00295

15.84

−0.01823

0.006279

15.86

−0.00796

0.011133

15.88

−0.02731

0.001556

15.9

0.008318

0.01921

15.92

−0.0037

0.014344

15.94

0.007567

0.02072

15.96

−0.02027

0.003245

15.98

−0.01705

0.007303

16

−0.01747

0.00762

16.02

−0.0059

0.013742

16.04

−0.02571

0.000434

16.06

0.00123

0.015174

16.08

−0.02673

0.00081

16.1

0.000934

0.018006

16.12

0.017173

0.026867

16.14

−0.0108

0.007938

16.16

−0.00499

0.020462

16.18

−0.00362

0.016295

16.2

−0.00302

0.013994

16.22

−0.01649

0.005174

16.24

0.002657

0.011788

16.26

−0.01986

−0.0036

16.28

−0.01192

0.004226

16.3

−0.0216

0.002932

16.32

−0.03076

0.000359

16.34

−0.01702

0.005958

16.36

−0.02097

0.004851

16.38

−0.01344

0.012995

16.4

−0.01126

0.013165

16.42

0.001416

0.0201

16.44

0.025535

0.029834

16.46

−0.01265

0.005022

16.48

−0.01707

0.005082

16.5

0.005849

0.023367

16.52

0.003071

0.01825

16.54

−0.03934

−0.00869

16.56

−0.01295

0.008321

16.58

−0.00574

0.015581

16.6

−0.02828

−0.00285

16.62

−0.01588

0.006001

16.64

−0.01989

−0.00238

16.66

−0.02108

0.008733

16.68

−0.01442

0.008242

16.7

−0.00424

0.017365

16.72

−0.01095

0.007871

16.74

−0.00145

0.015669

16.76

−0.01792

0.005363

16.78

0.009292

0.023795

16.8

−0.00379

0.015671

16.82

−0.01185

0.007864

16.84

−0.01481

0.001576

16.86

−0.00946

0.009989

16.88

−0.00497

0.015388

16.9

−0.00746

0.01278

16.92

−0.03313

−0.00509

16.94

−0.01766

0.002109

16.96

−0.00494

0.01206

16.98

−0.00709

0.017855

17

−0.01431

0.006401

17.02

−0.01241

0.00343

17.04

−0.02585

−0.00416

17.06

−0.00734

0.00579

17.08

−0.03602

−0.00662

17.1

−0.00885

0.012849

17.12

−0.02162

0.003466

17.14

−0.01382

0.007276

17.16

0.002953

0.018335

17.18

0.006901

0.019663

17.2

−0.00352

0.020061

17.22

−0.02859

0.0027

17.24

−0.01144

0.012464

17.26

−0.03014

−0.00211

17.28

−0.0056

0.008632

17.3

−0.02932

0.000458

17.32

−0.01885

0.006068

17.34

−0.01338

0.009713

17.36

−0.01327

0.004136

17.38

−0.00626

0.012486

17.4

0.002288

0.017792

17.42

−0.00633

0.012048

17.44

−0.02932

−0.00294

17.46

−0.00039

0.014183

17.48

−0.01081

0.008801

17.5

−0.02267

−0.00304

17.52

0.003663

0.017713

17.54

−0.02049

0.000378

17.56

0.0067

0.021219

17.58

−0.01785

0.002949

17.6

0.001532

0.017236

17.62

−0.01238

0.007066

17.64

0.003693

0.012661

17.66

−0.01064

0.009715

17.68

−0.0185

0.00766

17.7

−0.00282

0.013796

17.72

−0.01224

0.007896

17.74

−0.03033

0.001698

17.76

−0.00672

0.014106

17.78

−0.00992

0.012609

17.8

−0.02352

−0.0001

17.82

−0.01922

0.004327

17.84

−0.03537

−0.00201

17.86

−0.00691

0.014539

17.88

−0.00823

0.010325

17.9

−0.01341

0.01078

17.92

0

0.013573

17.94

−0.01114

0.009463

17.96

−0.00572

0.008522

17.98

−0.02047

0.006135

18

−0.01031

0.010396

18.02

−0.00853

0.011528

18.04

−0.00317

0.013069

18.06

−0.01715

0.00713

18.08

−0.00062

0.020628

18.1

−0.00577

0.02002

18.12

−0.02559

0.008019

18.14

−0.01586

0.015835

18.16

0.000448

0.021869

18.18

−0.00187

0.022937

18.2

−0.00621

0.022318

18.22

−0.01021

0.016616

18.24

0.001908

0.025647

18.26

−0.00583

0.022761

18.28

0.00156

0.024646

18.3

−0.00703

0.021783

18.32

−0.00067

0.027247

18.34

−0.01602

0.016852

18.36

−0.01335

0.020628

18.38

−0.01909

0.01856

18.4

−0.02006

0.015536

18.42

−0.02351

0.014997

18.44

−0.02153

0.017015

18.46

−0.0188

0.017999

18.48

−0.01399

0.020999

18.5

−0.01053

0.02539

18.52

−0.00807

0.025661

18.54

−0.01182

0.02357

18.56

−0.01555

0.022593

18.58

−0.01783

0.020098

18.6

−0.01662

0.02401

18.62

−0.01523

0.024262

18.64

−0.01423

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28

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28.02

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28.04

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28.06

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28.1

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28.16

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28.2

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28.6

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29

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29.02

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29.04

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29.06

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29.1

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29.14

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29.16

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29.18

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29.2

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29.22

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29.24

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29.3

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30

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30.02

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30.04

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30.06

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30.08

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30.1

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30.12

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30.16

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30.3

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31

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31.02

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31.04

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31.06

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31.1

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31.14

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31.2

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32

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33

0.006225

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33.02

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33.06

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34

0.002283

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34.02

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35

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36

0.004798

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73

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100

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100.02

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100.1

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100.16

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100.18

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0.002303

101

0.018185

0.009012

101.02

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101.04

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101.06

0.002134

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101.08

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101.1

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101.12

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101.14

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101.16

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101.18

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101.2

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101.3

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101.32

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101.4

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101.44

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101.9

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101.94

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101.98

0.000233

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102

−0.02164

0.001753

102.02

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0.010082

102.04

0.024934

0.033074

102.06

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0.028719

102.08

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102.1

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102.12

0.01071

0.023104

102.14

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102.16

0.006528

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102.18

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102.2

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102.22

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102.24

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102.26

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102.28

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102.3

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102.32

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102.34

0.003785

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102.48

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102.5

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102.52

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102.6

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102.7

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102.8

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102.9

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102.94

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102.98

0.011548

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103

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0.00947

103.02

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103.04

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103.08

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103.1

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103.12

0.001457

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103.14

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103.16

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103.18

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103.2

0.010043

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103.26

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104

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104.02

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104.04

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104.08

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104.1

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104.16

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104.2

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104.26

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105

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105.02

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105.04

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105.06

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105.08

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105.1

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105.12

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105.14

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105.16

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105.18

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105.2

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105.3

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105.32

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106

−0.02273

31 0.00077

106.02

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106.16

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106.18

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106.2

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106.24

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106.26

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107

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107.02

0.001306

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107.04

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107.06

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107.08

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107.1

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107.12

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107.14

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107.16

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107.2

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107.22

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107.3

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107.32

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107.98

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0.011018

108

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108.02

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108.04

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0.01979

108.06

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108.08

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108.1

0.017029

0.021085

108.12

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108.14

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108.16

0.009679

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108.18

0.01137

0.018989

108.2

0.0147

0.022243

108.22

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0.009788

108.24

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0.015997

108.26

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108.28

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108.3

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108.32

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108.34

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108.36

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108.38

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108.4

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108.42

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108.46

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108.56

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0.013434

108.58

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0.013033

108.6

0.005983

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117.62

−0.00806

−0.00898

117.64

0.000098

−0.01125

117.66

0.012757

−0.01294

117.68

0.014287

−0.01728

117.7

0.013474

−0.01888

117.72

0.002099

−0.02524

117.74

0.002039

−0.0261

117.76

−0.00619

−0.02362

117.78

0.010354

−0.01003

117.8

−0.00926

−0.01989

117.82

−0.01482

−0.01112

117.84

−0.00147

0.000988

117.86

−0.00406

0.003591

117.88

−0.01675

−0.00263

117.9

−0.01413

0.006744

117.92

−0.02431

−0.00116

117.94

−0.01533

0.01011

117.96

−0.01729

0.010427

117.98

−0.01411

0.013697

118

−0.02792

0.007176

118.02

−0.0308

0.005481

118.04

−0.03761

−0.00118

118.06

−0.02366

−0.0009

118.08

−0.0124

−0.00158

118.1

−0.00641

−0.00618

118.12

−0.00316

−0.01559

118.14

0.012606

−0.01158

118.16

0.002479

−0.0222

118.18

0.011127

−0.015

118.2

−0.00254

−0.02292

118.22

−9.9E−05

−0.01557

118.24

0.00157

−0.01289

118.26

0.006153

−0.0058

118.28

0.022332

0.011982

118.3

−0.01499

−0.01249

118.32

0.003481

0.007818

118.34

−0.02536

−0.01586

118.36

−0.00987

0.005366

118.38

0.007152

0.008617

118.4

−0.02708

−0.00628

118.42

0.01761

0.020169

118.44

0.008643

0.020609

118.46

0.003394

0.011489

118.48

−0.00694

−0.00232

118.5

0.013065

0.019702

118.52

−0.00151

0.006542

118.54

−0.009

0.008803

118.56

0.002038

0.013202

118.58

0.011616

0.020439

118.6

−0.00241

0.013868

118.62

0.013087

0.020164

118.64

0.005878

0.014292

118.66

−0.00471

0.006552

118.68

0.000833

0.014114

118.7

−0.00358

0.00867

118.72

−0.00164

0.005902

118.74

0.009686

0.011759

118.76

0.002378

0.007294

118.78

−0.00507

0.00754

118.8

−0.00858

0.004964

118.82

−0.01092

0.003122

118.84

0.005075

0.013621

118.86

−0.0195

−0.00649

118.88

0.023209

0.02222

118.9

0.015314

0.023298

118.92

−0.00688

0.004848

118.94

−0.01062

0.006513

118.96

0.006225

0.014126

118.98

−0.01323

0.006357

119

−0.01464

0.005723

119.02

−0.01396

0.004828

119.04

0.009927

0.020719

119.06

−0.00086

0.010196

119.08

−0.01956

0.003068

119.1

−0.01526

0.006848

119.12

−0.00488

0.01893

119.14

0.000693

0.020902

119.16

0.003719

0.014355

119.18

−0.02016

−0.00035

119.2

−0.01557

0.008493

119.22

−0.01252

0.011614

119.24

−0.03059

0.001387

119.26

−0.01591

0.009152

119.28

−0.00636

0.015349

119.3

−0.01812

0.011047

119.32

−0.02775

0.009686

119.34

−0.03205

0.004938

119.36

−0.02416

0.012604

119.38

−0.03136

0.008209

119.4

−0.02603

0.01094

119.42

−0.02574

0.011938

119.44

−0.02573

0.010883

119.46

−0.02278

0.00714

119.48

−0.02336

−0.00179

119.5

−0.00678

−0.00024

119.52

−0.00097

−0.00812

119.54

0.015825

−0.00462

119.56

0.018466

−0.00822

119.58

0.018802

−0.00995

119.6

0.014315

−0.00994

119.62

0.00665

−0.00816

119.64

−0.00584

−0.01002

119.66

0.008738

0.001698

119.68

0.000506

−0.00251

119.7

−0.0047

0.001826

119.72

−0.00332

0.004063

119.74

−0.00352

0.002677

119.76

−0.00102

0.011956

119.78

−0.00734

0.011878

119.8

−0.00711

0.008634

119.82

−0.00715

0.012202

119.84

−0.01411

0.007991

119.86

−0.02427

0.007381

119.88

−0.01962

0.013027

119.9

−0.02421

0.011376

119.92

−0.02752

0.01389

119.94

−0.02228

0.015415

119.96

−0.01885

0.008414

119.98

−0.00649

0.009735

120

0.001124

0.008883

The lithium cobalt oxides of the present invention are prepared by first mixing together one or more lithium source compounds, one or more cobalt source compounds, and one or more source compounds that include the dopants A in the desired stoichiometric amounts to produce lithium cobalt oxides having the formula Li

w

Co

1−x

A

x

O

2+y

wherein 0.96w≦1.05, 0≦x≦0.05, −0.02≦y≦0.02. The source compounds (raw materials) can be the pure elements but are typically compounds containing the elements such as oxides or salts thereof. For example, the source compounds are typically hydrated or anhydrous oxides, hydroxides, carbonates, nitrates, sulfates, chlorides or fluorides, but can be any other suitable source compound that will not cause elemental defects in the resulting lithium cobalt oxide compound. The elements for the lithium cobalt oxide compound can each be supplied from separate source compounds or at least two of the elements can be supplied from the same source compounds. In addition, the source compounds can be mixed in any desirable order.

Although the lithium cobalt oxide compounds are preferably prepared by solid state reactions (i.e. dry mixing), it can be advantageous to react the raw materials using wet chemistry such as sol-gel type reactions or spray drying techniques, alone or in combination with solid state reactions. For example, the cobalt and dopant source compounds can be prepared as a solution in a solvent such as water and the cobalt and dopants precipitated out of solution as an intimately mixed compound such as a hydroxide. The mixed compound can then be blended with a lithium source compound. The reaction mixture can also be prepared by suspending source compounds in a solution of other source compounds and spray drying the resulting slurry to obtain an intimate mixture. Typically, the selection of reaction methods will vary depending on the raw materials used and the desired end product. Preferably, in accordance with the present invention, the lithium source compound is selected from the group consisting of Li

2

CO

3

and LiOH and the cobalt source compound is selected from the group consisting of Co

3

O

4

and Co(OH)

2

.

The mixture of source compounds once prepared can be reacted to form the lithium metal oxide. The source compounds are reacted by heating (i.e. firing) the source compounds in a first heating step at a temperature below about 850° C., preferably from about 500° C. to about 850° C., to produce the Li

w

Co

1−x

A

x

O

2+y

compound. The source compounds are heated for a period of time sufficient to react the source compounds to produce a Li

w

Co

1−x

A

x

O

2+y

compound that is substantially free of lithium and cobalt phases. Preferably, the source compounds are heated for a period of time of from about 30 minutes to about 3 hours to produce the Li

w

Co

1−x

A

x

O

2+y

compound. The source compounds can also be heated in the first heating step at more than one temperature within the above temperature range and time period. For example, the source compounds can be heated for 1 hour at 600° C. and for 1 hour at 700° C. to produce the lithium cobalt oxides. Typically, the temperature and time period used in the first heating step is dependent on the raw material used and the desired grain size for the resulting lithium cobalt oxide compound. In particular, larger grain sizes (e.g. 10 microns) can require longer heating times.

Once the Li

w

Co

1−x

A

x

O

2+y

compounds are produced, these compounds are heated in a second heating step at a temperature from about 900° C. and 1000° C., preferably from about 950° C. to about 980° C., to form and enhance the hexagonal layered crystal structure of these compounds. The Li

w

Co

1−x

A

x

O

2+y

compound is preferably heated in the second heating step for a period of time of from about 30 minutes to about 7 hours. The Li

w

Co

1−x

A

x

O

2+y

compound can also be heated in the second heating step at more than one temperature within the above range and time period. Typically, the temperature and time period used for the second heating step is dependent on the grain size of the lithium cobalt oxide compound.

Any suitable apparatus can be used for heating or firing the mixture, such as a rotary calciner, a stationary furnace or a tunnel furnace, that uniformly heats the source compounds (first heating step) or the lithium cobalt oxide (second heating step) to produce the lithium cobalt oxides. Preferably, a rotary calciner is used in accordance with the invention. In addition, any suitable atmosphere such as air and other oxygen-containing atmospheres can be used in accordance with the invention as long as the atmosphere provides the desired oxygen content to form the lithium cobalt oxides.

Once the lithium cobalt oxide is at its final preparation temperature, the lithium cobalt oxide is preferably cooled at a rate of from about 8° C./min to about 140° C./min, more preferably from about 10° C./min to 100° C./min. Cooling at a rate of greater than 140° C./min undesirably produces a structure with high crystalline stress and strain that does not have the strength of lithium cobalt oxides cooled at a rate of between 8° C./min and 140° C./min. Moreover, cooling at a rate of less than 8° C./min undesirably results in the formation of localized cubic spinel-like structural phases on the surface of the crystal or within the crystal and thus decreased electrochemical performance. With the lithium cobalt oxides of the invention, the lack of localized hetero-structural phases, e.g., cubic spinel-like phases, within the crystal and on the crystal surface does not induce further phase transformation that impedes the diffusion of the Li

+

ions during the charge and discharge cycles. Thus, the hexagonal layered compounds of the invention have better and more consistent electrochemical performance than prior art compounds that are cooled at slower rates.

The lithium cobalt oxide is preferably uniformly cooled (i.e. quenched) in accordance with the invention. In particular, the lithium cobalt oxide material is preferably cooled at approximately the same rate. For example, the variation between the mean cooling rate and the cooling rate for any specific portion of the material should be less than about 10 percent. In a preferred embodiment of the invention, uniform cooling can be accomplished using a rotary calciner, or a stationary furnace or tunnel furnace with smaller bed depths. The uniformly cooled material prepared according to the invention has greater homogeneity and less variance in its material properties than material that is not uniformly cooled.

The present invention further includes rechargeable lithium and lithium ion secondary batteries that include a positive electrode comprising the lithium cobalt oxides of the invention. Typically, the lithium cobalt oxide compound of the invention is combined with a carbonaceous material and a binder polymer to form a cathode. The negative electrode of the lithium battery can be lithium metal or alloys, or any material capable of reversibly lithiating and delithiating at an electrochemical potential relative to lithium metal between about 0.0 V and 0.7 V. Examples of negative electrode materials include carbonaceous materials containing H, B, Si and Sn; tin oxides; tin-silicon oxides; and composite tin alloys. The negative electrode is separated from the positive electrode material in the cell using an electronic insulating separator. The electrochemical cell further includes an electrolyte. The electrolyte can be non-aqueous liquid, gel or solid and preferably comprises a lithium salt, e.g., LiPF

6

. Electrochemical cells using the lithium cobalt oxide compounds of the invention as positive electrode material can be combined for use in portable electronics such as cellular phones, camcorders, and laptop computers, and in large power applications such as for electric vehicles and hybrid electric vehicles.

The lithium cobalt oxide compounds of the invention allow lithium ions to readily diffuse during both the charge and discharge cycles of the battery. In particular, in the charge cycle for these lithium cobalt oxides wherein z Li per formula unit are electrochemically removed per formula unit, the lithium cobalt oxide takes the formula Li

w−z

Co

1−x

A

x

O

2+y

, wherein 0≦z≦w.

The present invention further includes a method of analyzing a compound to determine if the compound is suitable for use as the active positive electrode material in a lithium or lithium-ion secondary battery. The method of the invention comprises determining a principal component space defined by the relationship ax

i

+by

i

≦c, wherein x

i

={right arrow over (S)}

i

&Circlesolid;{right arrow over (P)}

c1

; y

i

={right arrow over (S)}

i

&Circlesolid;{right arrow over (P)}

c2

; the vector {right arrow over (S)}

i

is the x-ray spectrum for the compound; the vectors {right arrow over (P)}

c1

and {right arrow over (P)}

c2

are determined by measuring the x-ray powder diffraction values {right arrow over (S)}

i

for a predetermined range of 2θ values using a predetermined step size by sampling a plurality of samples of compounds having the same general formula as the compound and using the regression of {right arrow over (S)}

i

of the sample set against predetermined battery performance data for the samples by incorporating the samples as the positive electrode active material in a lithium or lithium-ion secondary battery. The x

i

and y

i

values for the compounds in the sample set that have the predetermined battery performance data are then used to determine a, b and c. The compound is analyzed by measuring the x-ray diffraction spectra for the compound to obtain x and y values and determining whether the x and y values meet the relationship ax

i

+by

i

≦c. If the x and y values meet this relationship, the compound will possess the battery performance and x-ray diffraction spectra suitable for use as the active positive electrode material (as defined by the predetermined battery performance values).

In accordance with the method of analysis described in accordance with the invention, it is important that the compounds in the sample set have the same general formula as the compound being tested. In addition, it is important that the compounds be tested using the same conditions to provide consistent and reliable results. The positive electrode active materials tested using the method of the invention can be any of those known in the art and are preferably lithiated. Preferably, the compound is a compound selected from the group consisting of doped and undoped lithium nickel oxides, lithium cobalt oxides and lithium manganese oxides, and more preferably it is lithium cobalt oxide as discussed above. Different battery performance properties (e.g. fade, specific capacity, and the like), and different thresholds for these properties can be used to determine the principal component space. Preferably, the samples that are used to determine the principal component space are selected based on meeting a threshold predetermined capacity fade after a predetermined number of cycles under predetermined cycling conditions. For example, as discussed above, the predetermined range of 2θ values can be between 15° and 120° using CuKα rays, the predetermined step size can be 0.02°, and the predetermined capacity fade after 50 cycles of a lithium coin cell that includes a lithium negative electrode and the lithium cobalt oxide as the positive electrode material and that is cycled between 3.0 and 4.3V at a constant current of C/3 during both charge and discharge cycles can be less than or equal to 15%. More preferably, the principal component space is defined by the relationship x

i

+0.77y

i

≦−6. Although different methods can be used to determine the regression of {right arrow over (S)}

i

of the sample set, the regression is preferably determined using a partial least squares regression method as discussed above.

The present invention will now be further demonstrated by the following non-limiting examples.

EXAMPLES

Sample Preparation

Stoichiometric amounts of Li2CO3 and Co3O4 with about 2 molar percent in lithium excess were thoroughly mixed and then fired in air as follows:

Sample S1 was heated at a rate of about 18° C./min from room temperature to 750° C., held at 750° C. for 1 hour, then heated to 950° C. in about 10 minutes, and held at 950° C. for 4 hours, followed by a rapid cooling to room temperature in about 10 minutes.

Sample S2 was heated at a rate of about 18° C./min from room temperature to 800° C., held at 800° C. for 1 hour, then heated to 975° C. in about 10 minutes, and held at 975° C. for 4 hours, followed by a rapid cooling to room temperature in about 10 minutes.

Sample S3 was heated at a rate of about 5° C./min from room temperature to 800° C., held at 800° C. for 3 hour, then heated to 975° C. in about 1 hour, and held at 975° C. for 9 hours, followed by a cooling to room temperature at a rate of about 5° C./min.

Sample S4 was heated at a rate of about 25° C./min from room temperature to 800° C., held at 800° C. for 30 min, then heated to 975° C. in about 10 min, and held at 975° C. for 2 hours, followed by a rapid cooling to room temperature in about 30 minutes.

Comparative sample CS1 was heated at a rate of 3.75° C./min from room temperature to 950° C., held at 950° C. for 5 hours, followed by a cooling to room temperature at a rate of 3.75° C./min.

Coin Cell Testing

NRC 2325 coin cell hardware and Celgard 3501 separators were used. The electrolyte was 1M LiPF

6

in a 50:50 mixture of ethylene carbonate and dimethyl carbonate solvents. The positive electrode consisted of about 85% active material (by weight), 10% Super S™ carbon black and 5% polyvinylidene fluoride (PVDF) as a binder polymer, coated on aluminum foil. The negative electrode was metallic lithium foil. The cell was cycled between 3.0 and 4.3V at a constant current of C/3 (3 hours for complete charge or discharge) during both the charge and discharge cycles.

X-ray Diffraction

A Rigaku RINT-2000 unit that included a graphite monochrometer and a rotating copper anode x-ray source was used. The current and the voltage of the x-ray source were 150 mA and 50 kV, respectively, during operation. The anti-scattering slits and the anti-divergence slits were both set at 0.50. The x-ray diffraction scan was carried out between 15° and 120° 2θ at a step size of 0.02° and the counting time per step was 0.6 seconds.

Samples S1, S2, S3 and S4, and Comparative Sample CS1, were tested in the Li coin cells described above, and the capacity fade after 50 cycles is provided in Table 2. The x-ray diffraction spectra were also obtained as described above. Their x and y values were calculated as described above with respect to the preferred embodiment of the invention and are also provided in Table 2.

In addition to the above samples, commercial samples C1, C2, C3 and C4 were also tested in the Li coin cells described above and their x-ray diffraction spectra were obtained the same way as samples S1, S2, S3, S4 and CS 1. The capacity fade values after 50 cycles, as well as the x and y values are also provided for these commercial samples in Table 2.

TABLE 2

Capacity fade after

samples

x

y

50 cycles

S1

−3.22

−11.05

4%

S2

−18.27

10.74

7%

S3

14.55

−27.76

15%

S4

−1.14

−14.71

4%

CS1

21.53

−18.42

41%

C1

14.46

−21.94

20%

C2

8.86

−16.41

15%

C3

11.91

−17.90

24%

C4

28.51

−31.23

32%

FIG. 1

illustrates the positions of samples S1, S2, S3, and S4; comparative sample CS1; and commercial samples C1, C2, C3 and C4, in a principal component space as defined by the axes {right arrow over (P)}

c1

and {right arrow over (P)}

c2

. The dotted line in

FIG. 1

represents the equation x+0.77y=−6 in accordance with the preferred embodiment of the invention described above. As illustrated in

FIG. 1

, the samples prepared in accordance with the invention are on the left of the dotted line and the comparative and commercial samples are on the right of the dotted line.

FIG. 2

illustrates the capacity fade after 50 cycles versus x+0.77y. The dotted line in

FIG. 2

defines the principal component space of the samples of the invention having the desired x-ray powder diffraction values and a fade of less than or equal to 15% in accordance with the preferred embodiment of the invention discussed above. In particular, the samples according to the invention S 1, S2, S3 and S4 fall within in the principal component space (the box in the lower left portion of the graph) while the comparative sample and commercial examples do not. This demonstrates that the samples according to the invention have the capacity fade and the x-ray diffraction spectra that meet the equation x

i

+0.77y

i

≦−6.

As shown above, the lithium cobalt oxides of the invention have good cycleability properties including good initial specific capacities and capacity fades and thus are desirable for use in rechargeable lithium and lithium-ion batteries. In addition, the lithium cobalt oxides of the present invention can be produced quickly in less than 10 hours and thus can be produced at a rate desired in the art.

It is understood that upon reading the above description of the present invention and studying the accompanying drawings, one skilled in the art could make changes and variations therefrom. These changes and variations are included in the spirit and scope of the following appended claims.

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Lithium cobalt oxides and methods of making same

Information

Patent Number

Date Filed

Date Issued

Inventors

Original Assignees

Examiners

Agents

CPC

US Classifications

Field of Search

US

International Classifications

Term Extension

Abstract

Description

Claims

CROSS REFERENCE TO RELATED APPLICATIONS

US Referenced Citations (64)

Foreign Referenced Citations (33)

Non-Patent Literature Citations (31)

Provisional Applications (1)

Entry
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