Method for preparing positive electrode active material precursor for lithium secondary battery, positive electrode active material precursor, and positive electrode active material, positive electrode, and lithium secondary battery prepared by using same

A technology for cathode active materials and precursors, applied in the field of preparing cathode active material precursors for lithium secondary batteries, cathode active material precursors, and cathode active materials prepared by using the precursors, cathodes, and lithium secondary batteries , can solve problems such as poor thermal stability, battery rupture, fire, etc., and achieve the effect of improving electrochemical performance

Pending Publication Date: 2022-07-08

LG CHEM LTD

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AI-Extracted Technical Summary

Problems solved by technology

However, LiNiO 2 The limitation is that, with LiCoO 2 Compared to LiNiO 2 Has worse thermal stability, and when an internal short circuit occu...

Method used

In a lithium secondary battery, a separator separates the negative electrode and the positive electrode and provides a moving path for lithium ions, wherein any separator can be used as the separator without particular limitation as long as it is commonly used in lithium secondary batteries. Medium is sufficient, and in particular, a separator having a high moisture retention capacity for electrolytes and low resistance to electrolyte ion transfer can be used. Specifically, porous polymer membranes, for example made of polyolefin polymers such as ethylene homopolymers, propylene homopolymers, ethylene/butylene copolymers, ethylene/hexene copolymers and ethylene/methacrylate copolymers, can be used A porous polymer film prepared by a material; or a laminated structure with more than two layers thereof. In addition, typical porous nonwoven fabrics such as nonwoven fabrics formed of high-melting glass fibers or polyethylene terephthalate fibers can be used. In addition, a coated separator including a ceramic component or a polymer material may be used to ensure heat resistance or mechanical strength, and a separator having a single-layer or multi-layer structure may be selectively used.

Negative electrode current collector is not particularly limited, as long as it has high electrical conductivity and does not cause unfavorable chemical change in battery, and can use for example: copper, stainless steel, aluminium, nickel, titanium, calcined carbon; Copper or stainless steel with a surface treatment of carbon, nickel, titanium, silver, etc.; and aluminum-cadmium alloys. In addition, the negative electrode current collector may generally have a thickness of 3 μm to 500 μm, and similar to the positive electrode current collector, fine unevenness may be formed on the surface of the current collector to improve the adhesion of the negative electrode active material. For example, the ...

Abstract

The present invention relates to a method for preparing a positive electrode active material precursor in which particle growth of the (001) plane is suppressed; a positive electrode active material precursor prepared by the above method; a positive electrode active material prepared by using the positive electrode active material; a positive electrode containing the positive electrode active material; and a lithium secondary battery.

Application Domain

Positive electrodesLi-accumulators +1

Technology Topic

Analytical chemistryBattery cell +1

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Examples

Experimental program(5)
Comparison scheme(2)

Example Embodiment

[0136] Example 1

[0137] NiSO was added in an amount such that the molar ratio of nickel:cobalt:manganese was 88:5:7 4 , CoSO 4 and MnSO 4 Mix in water to prepare an aqueous transition metal solution (first step).

[0138] The vessel containing the aqueous transition metal solution, additional NaOH solution, and NH 4 The aqueous OH solutions were each connected to a 350 L continuous filter tank reactor (CFTR) equipped with a filtration device (filter).

[0139] Subsequently, after 86 L of deionized water was put into the reactor, dissolved oxygen in the water was removed by purging the reactor with nitrogen at a rate of 20 L/min to create a non-oxidizing atmosphere in the reactor. After that, after adding NaOH aqueous solution and NH 4 After the OH aqueous solution, while stirring the mixture at a stirring speed of 700 rpm, a reaction mother liquor having a pH of 11.7 to 11.9 was prepared (second step).

[0140] After that, the transition metal aqueous solution, NH 4 Aqueous OH and NaOH were added to the reactor to induce formation of nickel cobalt manganese hydroxide particles and particle aggregation to form precursor cores (third step). In this case, add an aqueous transition metal solution and NH 4 OH aqueous solution such that NH added per unit time 4 The ratio of the molar concentration of the OH aqueous solution to the molar concentration of the transition metal aqueous solution was 0.3, and the addition amount of the NaOH aqueous solution was adjusted so that the pH of the reaction solution could be maintained at 10.5 to 11.2.

[0141] Subsequently, the reaction was performed while adjusting the addition amount of the aqueous NaOH solution so that the pH of the reaction solution was 11.3 to 11.5, to grow nickel-cobalt-manganese hydroxide particles (fourth step).

[0142] The total reaction time of the precursor core formation step (third step) and the particle growth reaction step (fourth step) was 40 hours.

[0143] Then, the nickel-cobalt-manganese hydroxide particles after the completion of the growth were further reacted for 8 hours for stabilization (fifth step).

[0144] When the reactor was full, the reaction was carried out while continuously draining the filtrate through a filter device in the reactor. Next, the nickel-cobalt-manganese hydroxide particles formed by the above-described process are separated, washed, and then dried to prepare Ni-mixed therein. 0.88 Co 0.05 Mn 0.07 (OH) 2 and Ni 0.88 Co 0.05 Mn 0.07 OOH phase precursor.

Example Embodiment

[0145] Example 2

[0146] In the same manner as in Example 1, except that the precursor core formation step (third step) and the particle growth reaction step (fourth step) were carried out for a total of 53 hours and the stabilization reaction (fifth step) was carried out for 15 hours A cathode active material precursor was prepared.

Example Embodiment

[0157] Experimental Example 1: Particle Characterization

[0158] (1) Grain size of precursor

[0159] The grain sizes of the positive electrode active material precursor particles prepared in Examples 1 and 2 and Comparative Examples 1 to 2 were measured by the following method.

[0160] The X-ray diffraction (XRD) patterns of the precursors prepared in Examples 1 and 2 and Comparative Examples 1 and 2 were measured using an X-ray diffraction analyzer (Rigaku Corporation). The XRD patterns of the positive electrode active material precursor particles prepared in Examples 1 and 2 and Comparative Examples 1 and 2 are shown in figure 2 middle.

[0161] After obtaining the half-value widths of the peaks of the respective crystal planes from the measured XRD patterns, the grain sizes in the respective crystal planes of the precursor were calculated by ellipsoid modeling using the Scherrer formula.

[0162] The measurement results are shown in Table 1 below.

[0163] [Table 1]

[0164]

[0165] As shown in [Table 1], for the positive electrode active material precursors prepared in Examples 1 and 2, it was confirmed that the growth of the (001) crystal plane compared with the positive electrode active material precursors prepared in Comparative Examples 1 and 2 suppressed.

[0166] (2) Average particle size

[0167] In order to examine the particle size distribution of the positive electrode active material precursor particles prepared in Examples 1 and 2 and Comparative Examples 1 and 2, a particle size distribution measuring instrument (Microtrac S3500, Microtrac) was used for The particle size of the positive electrode active material precursor formed in 2 was measured, and the results are shown in [Table 2] below.

[0168] (3) BET specific surface area

[0169] The Bruhe-Emmett-Teller (BET) specific surface areas of the positive electrode active material precursors prepared in Example 1 and Comparative Examples 1 and 2 were examined. The specific surface area of the positive electrode active material precursor was measured by the BET method. Specifically, the specific surface area was calculated from the nitrogen adsorption amount at the liquid nitrogen temperature (77K) using the BELSORP-mini II of Bell Japan Inc., and the results were shown. in [Table 2] below.

[0170] (4) Tap density

[0171] After each 50 g of the positive electrode active material precursors obtained in Examples 1 and 2 and Comparative Examples 1 and 2 was charged into a 200 cc container, the apparent density of the particles was measured by measuring the apparent density under constant conditions obtained by vibrating. Specifically, the tap density of the lithium transition metal oxide particles was measured using a tap density tester (KYT-5000, Seishin Enterprise Co., LTD.). The measurement results are shown in the following [Table 2].

[0172] [Table 2]

[0173]

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Method for preparing positive electrode active material precursor for lithium secondary battery, positive electrode active material precursor, and positive electrode active material, positive electrode, and lithium secondary battery prepared by using same

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