LITHIUM TITANIUM OXIDE-TIO_2 COMPLEX FOR SECONDARY BATTERY, PREPARING METHOD THEREOF, AND SECONDARY BATTERY INCLUDING SAME

Hereinafter, the present invention is hereinafter with reference to the drawing objects is provided to a person with skill in the art in the embodiment herein detailed in the embodiment and implementation for to 2000. However methods taught herein can be embodied in the form of several different in the embodiment is not limited to implementation and positive examples. The present invention is described in drawing and unambiguously account for when the dispensed portion that is independent, like part subjected to a similar drawing code is configured to receive through the entire specification.

The entire specification herein, synthetic resin assistant "connected" when any portion, this "connected directly" as well as when, its intermediate outer tube when "electrically connected" to another element comprises a unit.

The entire specification herein, that the "on" position when any member other members, as well as any other elements member between the two members when joined to another member to if there is a comprises a unit.

The entire specification herein, any components that "comprising" when any portion, particularly the opposite substrate under the outside number but without other components further can include other components which means that the other.

The degree to which the terms of "about" used in the specification, "substantially" or the like in which the tolerance number number unique to the meanings cited in the bath and materials used for the installation be at or in close proximity to the sense numerical, mentioned herein to aid in the understanding of accurate absolute or regenerating a disclosure content using the non-conscience are used to prevent giving self abuse.

The entire specification herein used is the degree to which the terms of "the -" or "- steps" which means "- stage for the" does not.

The entire specification herein, the term "combinations thereof (are)" e [khwu[khwu] citye [khwu[khwu] city type representation comprising of components selected from the group consisting of a representation of a form more mixed or combinations as means, said means including at least one selected from the group consisting of components to each other.

The entire specification herein, "A and/or B" of substrate, "A or B, or A and B" big.

The entire specification herein, " TiO₂ (B) "or" bronze type TiO₂ " The term bronze (bronze) titanium dioxide crystal form of adefovir (TiO₂ ) Meaning that the other.

The entire specification herein, the term "lithium titanate (LTO) composite" meaning that the material including a lithium titanate (lithium titanium oxide, LTO) provided, e.g., particles are formed of a porous fiber-type carbon material including therein a plurality of LTO again may be disclosed.

The entire specification of the present disclosure, " lTO provided tiO₂ (B) composite " the term LTO composite and TiO₂ (B) material including a big.

The entire specification herein, terms "carbon nanotube (carbon nanotube; CNT)" 1 the dog 3 different carbon atoms comprising carbon atoms provide the means by which combined with the honeycombed body planar carbon structure has rolled in tubular, normal diameter from about 1 to about 100 nanometers (nm) and, nanometers (nm) in length from a few tens of micrometers (micro m) having a high aspect ratio (aspect ratio) by big carbon material. Various kinds where the carbon nanotube is, among the one or more number of a wall in longitudinal direction to wrap around the axis 2 (a multi-walled nanotube; MWCNT) wall multi-walled nanotubes, with single-wall nanotubes (a single-walled nanotube; SWCNT) 1 composed of only two walls can be divided into.

Hereinafter, one embodiment of the present disclosure detailed but, number herein are herein not be one.

One aspect of the herein, titanium precursor solution containing glycolic acid to yield - glycol acid is added titanium; titanium - said mixing to yield a mixed solution containing glycolic acid and acidic solution; adding said mixed solution lithium titanate composite hydrothermally reacting wherein, said cyclooxygenase TiO on by said lithium titanate composite₂ The nanoparticles are formed, secondary battery lithium titanate - TiO₂ Complex number a number bath method under public affairs substrate.

the number tank method, first, by the addition of glycolic acid solution containing glycolic acid to yield a titanium precursor titanium - 2000.

In one embodiment of the present disclosure, including but said titanium precursor solutions may also include solvent and solvent may be number 1 number 2, the one number are not disclosed. Said number 1 solvent, e.g., hydrogen peroxide may be provided including, said number 2 solvent is, for example, ammonia may be but including, the one number are not disclosed.

In one embodiment of the present disclosure, said titanium precursor solutions may also include TiO (OH)₂ , Other number of drug TiO₂ , Ti (OH)₄ , Titanium powder, and combinations thereof may be selected from the group consisting titanium precursor including but composed, the one number are not disclosed.

Then, said acidic solution containing glycolic acid and titanium - a mixed sample solution substrate.

In one embodiment of the present disclosure, said acidic solution is sulfuric acid, hydrochloric acid, nitric acid, and combinations thereof may be selected from the group consisting solution including but composed, the one number are not disclosed.

In one embodiment of the present disclosure, the pH of said acidic solution that are synthesized TiO₂ Of can be determined, said acidic the solution has a pH 0. 4 to about pH 1. 0 of acidic solution including but may be, the number one are not disclosed. E.g., said acidic solution pH of about pH 0. 4 to about pH 1. 0, about pH 0. 4 to about pH 0. 8, about pH 0. 4 to about pH 0. 6, about pH 0. 6 to about pH 1. 0, or about pH 0. 8 to about pH 1. Wednesday 0 but, the one number are not disclosed.

In one embodiment of the present disclosure, the step of mixing said solution, about 2% to about 3% said acidic solution said mixed solution including mixing a volume of volume but as may be, the number one are not disclosed. For example, about 2% to about 3 volume % volume mixing solutions for said acidic solution, about 2 volume % to about 2. 5 volume %, or about 2. 5 volume % to about 3% volume handler, the one number are not disclosed.

In one embodiment of the present disclosure, using only said acidic solution is preferably small, e.g., when said use sulfuric acid as an acidic solution, the molar concentration of sulfate about 0. 24 M to about 0. 59 M handler, the one number are not disclosed.

Then, performing reaction by adding said mixed solution lithium titanate composite.

In one embodiment of the present disclosure, about 10 μm to about 50 μm of said lithium titanate composite can be a sized, the one number are not disclosed. For example, a size of 10 μm to about 50 μm said lithium titanate composite, about 10 μm to about 40 μm, about 10 μm to about 30 μm, about 10 μm to about 20 μm, about 20 μm to about 50 μm, about 30 μm to about 50 μm, or about 40 μm to about 50 μm handler, the one number are not disclosed.

In one embodiment of the present disclosure, comprises said lithium titanate composite lithium titanate (lithium titanium oxide, LTO). For example, the lithium titanate said Li₄ Ti₅ O₁₂ But in the uncompressed domain representation, the one number are not disclosed.

In one embodiment of the present disclosure, about 30 nm to about 200 nm particle size of lithium titanate said handler, the one number are not disclosed. For example, 30 nm to about 200 nm a size of said lithium titanium oxide particles, about 30 nm to about 150 nm, about 30 nm to about 90 nm, about 30 nm to about 70 nm, about 30 nm to about 50 nm, about 50 nm to about 200 nm, about 70 nm to about 200 nm, about 90 nm to about 200 nm, or between about 150 nm to about 200 nm handler, the number one are not disclosed.

In one embodiment of the present disclosure, said lithium titanate composite fiber-type carbon material may be further including but, the one number are not disclosed. For example, the carbon nanotube or carbon fibers and the like can be said fiber-type carbon material, said carbon nanotube is, for example, single-walled (a single-walled), double-walled (a double-walled), thin multi-walled (a multi-walled thin), multi-walled (a multi-walled), bundle type (roped), and combinations thereof including the composed but may be selected from the group consisting, the number one are not disclosed.

In one embodiment of the present disclosure, about 20 nm to about 80 nm mean average diameter of the fiber-type carbon material handler, the one number are not disclosed. E.g., about 20 nm to about 80 nm mean average diameter of the fiber-type carbon material, about 20 nm to about 70 nm, about 20 nm to about 60 nm, about 20 nm to about 50 nm, about 20 nm to about 40 nm, about 20 nm to about 30 nm, about 30 nm to about 80 nm, about 40 nm to about 70 nm, or between about 50 nm to about 60 nm handler, the number one are not disclosed.

In one embodiment of the present disclosure, said content of about 1 wt % to about 4 wt % for said fiber-type lithium titanate composite carbon material handler, the one number are not disclosed. For example, the content of about 1 wt % to about 4 wt % said fiber-type carbon material, about 1 wt % to about 3 wt %, about 1 wt % to about 2 wt %, about 2 wt % to about 4 wt %, or about 3 wt % to about 4 wt % can have, preferably about 2 wt % content in said fiber-type of carbon material handler, the one number are not disclosed.

In one embodiment of the present disclosure, it may be but said lithium titanate composite including porous, the one number are not disclosed.

In one embodiment of the present disclosure, about 50 nm to about 200 nm of said lithium titanate composite including but may be detected, the one number are not disclosed. For example, about 50 nm to about 200 nm pore size of the lithium titanate composite, about 50 nm to about 180 nm, about 50 nm to about 150 nm, about 50 nm to about 120 nm, about 50 nm to about 100 nm, about 50 nm to about 80 nm, about 80 nm to about 200 nm, about 100 nm to about 200 nm, about 120 nm to about 200 nm, about 150 nm to about 200 nm, or about 180 nm to about 200 nm handler, the number one are not disclosed.

In one embodiment of the present disclosure, said secondary battery lithium titanate - TiO₂ The composite is formed by said cyclooxygenase TiO on said lithium titanate composite₂ Nanoparticles are formed may be, e.g., said lithium titanate composite and pores to said TiO₂ The nanoparticles is formed but, the one number are not disclosed. Said lithium titanate - TiO₂ Composite acetate containing glycolic acid water-soluble properties said titanium - adsorption said lithium titanate composite within the pores of the honeycomb hereinafter for the pores of the inner TiO said lithium titanate composite₂ Nanoparticles can be formed. Lithium titanate composite TiO on₂ Nanoparticles of active material when applied in the circulating path to excellent rate characteristics can be improve the charge-discharge capacity simultaneously.

In one embodiment of the present disclosure, said TiO₂ The nanoparticles may have a bronze type crystal structure including but may be, the number one are not disclosed.

In one embodiment of the present disclosure, said TiO₂ About 20 nm to about 100 nm can be a sized of the nanoparticles, the one number are not disclosed. E.g., said TiO₂ 20 nm to about 100 nm a size of nanoparticles, about 20 nm to about 90 nm, about 20 nm to about 80 nm, about 20 nm to about 70 nm, about 20 nm to about 60 nm, about 20 nm to about 50 nm, about 20 nm to about 40 nm, about 20 nm to about 30 nm, about 30 nm to about 100 nm, about 40 nm to about 100 nm, about 50 nm to about 100 nm, about 60 nm to about 100 nm, about 70 nm to about 100 nm, about 80 nm to about 100 nm, or between about 100 nm to about 90 nm handler, the number one are not disclosed.

In one embodiment of the present disclosure, said temperature of about 160 °C to about 200 °C can be a reaction carried out in, the one number are not disclosed. For example, the temperature of the reaction said about 160 °C to about 200 °C, about 160 °C to about 190 °C, about 160 °C to about 180 °C, about 160 °C to about 170 °C, about 170 °C to about 200 °C, about 180 °C to about 200 °C, or about 190 °C to about 200 °C handler, the one number are not disclosed.

E.g., about 160 °C to about 200 °C said reaction at a temperature of preferably about 24 it can be performed during the time, the one number are not disclosed. Said reaction conditions in, said temperature higher than about 200 °C reaction, other number of drug rutile style type and can be which are mixed, when less than about 160 °C, crystalline drop TiO₂ (B) it is made by synthesizing a decrease in the rate characteristics and, when said about 24 hours reaction time, other number of drug rutile style type and which are mixed can be, in one case about 24 time hereinafter, not satisfactory crystalline TiO₂ (B) can be synthesized.

In one embodiment of the present disclosure, for a bronze type TiO said said lithium titanate composite₂ About 10 weight % to about 50% by weight filler handler, the one number are not disclosed. For example, a bronze type TiO said₂ About 10 weight % to about 50% by weight filler, about 10 weight % to about 40% by weight, about 10 weight % to about 30% by weight, about 10 weight % to about 20% by weight, about 20 weight % to about 50% by weight, about 20 weight % to about 40% by weight, about 20 weight % to about 30% by weight, about 30 weight % to about 50% by weight, about 30 weight % to about 40% by weight, or about 40 weight % to about 50% by weight handler, the one number are not disclosed. Said secondary battery lithium titanate - TiO₂ Said complex is a bronze type TiO₂ About 20% by weight filler when electrochemical but crucial when a power-on, the one number are not disclosed. Said TiO₂ Content of nanoparticles formed by the initially non-reversible capacity but, said TiO₂ When an excess filler, lowering the efficiency of charge can be.

The other one side herein, porous lithium titanate composite and pores formed a bronze type TiO₂ Nanoparticles [TiO₂ (B)] wherein, said one side of the tank by a number according to method herein, secondary battery lithium titanate - TiO₂ Composite number under public affairs substrate.

- TiO lithium titanate for a secondary battery according to one aspect of the present disclosure other₂ The composite is formed, said according to one aspect of the herein - TiO lithium titanate for secondary battery₂ Complex number bath method for subject matter disclosed and overlaps a portions subjected to omit but description, description thereof can be omitted [ess[ess] Compared to force.

In one embodiment of the present disclosure according to lithium titanate - TiO₂ Composite lithium ion rapidly due to a wide specific surface area can be spread, the is made can be due to deterioration of the rate characteristics. In addition, physical and/or chemical of high thereby lithium titanate composite excellent rate can be improve the charge-discharge capacity while maintaining properties.

In one embodiment of the present disclosure according to lithium titanate - TiO₂ When used as a composite cell, said lithium titanate - TiO₂ By way nano-structre composite solid within the lithium diffusion capacity diffusion can be smoothly picked, resistance in addition rate of first and second battery capable of the coaxial cable. In addition, said lithium titanate - TiO₂ Composite cathode active material is used as negative electrode active material of the existing method used carbonaceous material initial irreversible capacity and cycle repeated complex dose-reduced number of points can be solve door.

In one embodiment of the present disclosure, about 50 nm to about 200 nm of said porous lithium titanate composite the pores are sized can be a, the one number are not disclosed. For example, about 50 nm to about 200 nm pore size of the lithium titanate composite, about 50 nm to about 180 nm, about 50 nm to about 150 nm, about 50 nm to about 120 nm, about 50 nm to about 100 nm, about 50 nm to about 80 nm, about 80 nm to about 200 nm, about 100 nm to about 200 nm, about 120 nm to about 200 nm, about 150 nm to about 200 nm, or about 180 nm to about 200 nm handler, the number one are not disclosed.

In one embodiment of the present disclosure, about 10 μm to about 50 μm of said porous lithium titanate composite can be a sized, the one number are not disclosed. For example, a size of 10 μm to about 50 μm said lithium titanate composite, about 10 μm to about 40 μm, about 10 μm to about 30 μm, about 10 μm to about 20 μm, about 20 μm to about 50 μm, about 30 μm to about 50 μm, or about 40 μm to about 50 μm handler, the one number are not disclosed.

In one embodiment of the present disclosure, comprises said porous lithium titanate composite lithium titanate (lithium titanium oxide, LTO). For example, the lithium titanate said Li₄ Ti₅ O₁₂ But in the uncompressed domain representation, the one number are not disclosed.

In one embodiment of the present disclosure, about 30 nm to about 200 nm particle size of lithium titanate said handler, the one number are not disclosed. For example, 30 nm to about 200 nm a size of said lithium titanium oxide particles, about 30 nm to about 150 nm, about 30 nm to about 90 nm, about 30 nm to about 70 nm, about 30 nm to about 50 nm, about 50 nm to about 200 nm, about 70 nm to about 200 nm, about 90 nm to about 200 nm, or between about 150 nm to about 200 nm handler, the number one are not disclosed.

In one embodiment of the present disclosure, said porous lithium titanate composite fiber-type carbon material may be further including but, the one number are not disclosed. For example, the carbon nanotube or carbon fibers and the like can be said fiber-type carbon material, said carbon nanotube is, for example, single-walled (a single-walled), double-walled (a double-walled), thin multi-walled (a multi-walled thin), multi-walled (a multi-walled), bundle type (roped), and combinations thereof including the composed but may be selected from the group consisting, the number one are not disclosed.

In one embodiment of the present disclosure, about 20 nm to about 80 nm mean average diameter of the fiber-type carbon material handler, the one number are not disclosed. E.g., about 20 nm to about 80 nm mean average diameter of the fiber-type carbon material, about 20 nm to about 70 nm, about 20 nm to about 60 nm, about 20 nm to about 50 nm, about 20 nm to about 40 nm, about 20 nm to about 30 nm, about 30 nm to about 80 nm, about 40 nm to about 70 nm, or between about 50 nm to about 60 nm handler, the number one are not disclosed.

In one embodiment of the present disclosure, the content of carbon material for said porous lithium titanate composite about 1 wt % to about 4 wt % said fiber-type handler, the one number are not disclosed. For example, the content of about 1 wt % to about 4 wt % said fiber-type carbon material, about 1 wt % to about 3 wt %, about 1 wt % to about 2 wt %, about 2 wt % to about 4 wt %, or about 3 wt % to about 4 wt % into the, preferably about 2 wt % content in said fiber-type of carbon material handler, the one number are not disclosed.

In one embodiment of the present disclosure, said TiO bronze type₂ About 20 nm to about 100 nm can be a sized of the nanoparticles, the one number are not disclosed. E.g., said TiO₂ 20 nm to about 100 nm a size of nanoparticles, about 20 nm to about 90 nm, about 20 nm to about 80 nm, about 20 nm to about 70 nm, about 20 nm to about 60 nm, about 20 nm to about 50 nm, about 20 nm to about 40 nm, about 20 nm to about 30 nm, about 30 nm to about 100 nm, about 40 nm to about 100 nm, about 50 nm to about 100 nm, about 60 nm to about 100 nm, about 70 nm to about 100 nm, about 80 nm to about 100 nm, or between about 100 nm to about 90 nm handler, the number one are not disclosed.

In one embodiment of the present disclosure, for a bronze type TiO said said lithium titanate composite₂ About 10 weight % to about 50% by weight filler handler, the one number are not disclosed. For example, a bronze type TiO said₂ About 10 weight % to about 50% by weight filler, about 10 weight % to about 40% by weight, about 10 weight % to about 30% by weight, about 10 weight % to about 20% by weight, about 20 weight % to about 50% by weight, about 20 weight % to about 40% by weight, about 20 weight % to about 30% by weight, about 30 weight % to about 50% by weight, about 30 weight % to about 40% by weight, or about 40 weight % to about 50% by weight handler, the one number are not disclosed. Said secondary battery lithium titanate - TiO₂ Said complex is a bronze type TiO₂ About 20% by weight filler when electrochemical but crucial when a power-on, the one number are not disclosed.

Another aspect of the herein one side, anode, cathode, separator, and organic electrolyte, said anode comprising a metal thin film lithium -, as a negative electrode active material for secondary battery according to said one side of said cathode herein - TiO lithium titanate₂ Composite including, secondary battery number under public affairs substrate.

According to another aspect of present application provides a secondary battery according to one side other herein one side - TiO lithium titanate for secondary battery₂ Composite including, secondary battery relates to search, for a secondary battery according to said one aspect of the herein - TiO lithium titanate₂ Complex number bath method and other - TiO lithium titanate for a secondary battery according to one side₂ Composite and overlaps a content described for portions subjected to omit but description, description thereof can be omitted [ess[ess] Compared to force.

In one embodiment of the present disclosure, said manufactured by mixing said lithium titanate - TiO₂ Composite, conductive number, that the number can be a mixed solvent and binder, the one number are not disclosed. E.g., said cathode, said lithium titanate - TiO₂ Number number suspended in a suitable solvent and a conductive composite engage, said aluminum foil current collector such as drying the suspension application, by pressing number can be high pressure liquid coolant. E.g., said conductive number include conductive metal, conductive carbon, conductive polymer, and combinations thereof can be selected from the group consisting of use and the composed, specifically [khey[khey] Tsien black, carbon black, acetylene black, graphite, activated carbon, super - P (a super-P), conductive polymer resin, and combinations thereof selected from the group consisting of use and it can be composed, the number one are not disclosed. For example, said coupling number include vinylidene fluoride, poly arc furnace nitrile, preferably using a preparation date or polyethylene.

In one embodiment of the present disclosure, said organic electrolyte battery and a lithium salt in an organic solvent can be. Using said contrast material can be publicly known organic solvents, ion degree of dissociation smoothly formed by ion conduction of high dielectric constant (polarity) for has low viscosity, reactive lithium metal preferably smaller in use.

In one embodiment of the present disclosure, organic solvent having said annular carbonates, linear carbonates, cyclic ether current, linear ether, and combinations thereof may be selected from the group consisting but including the composed, the one number are not disclosed. E.g., said organic solvent is propylene carbonate (PC), ethylene carbonate (EC), vinylene purification, diethyl carbonate (DEC), dimethyl carbonate (DMC), methylethyl purification (MEC), tetrahydrofuran (THF), 2 - methyl tetrahydrofuran (2 a-mE THF), dioxolane (DOX), dimethoxy ethane (DME), ethane (DEE) to D [thok[thok] at the time of, γ - butyrolactone (GBL), acetonitrile (AN), alcoholic beverage pawl column (SL), and combinations thereof may be selected from the group consisting of including but composed, the one number are not disclosed.

In one embodiment of the present disclosure, using said contrast material can be publicly known lithium salt, lattice energy is small and has an excellent ion conductivity ten safeties and oxidation a good degree of dissociation cursor is used preferably. Said lithium salt, e.g., lithium sustainable (LiClO₄ ), Lithium [heyk[heyk] It buys [phul[phul] base Oro gun [su[su] pay [thu[thu] (LiPF₆ ), Lithium tetra [phul[phul] Base Oro step [ley[ley] [thu[thu] (LiBF₄ ), Lithium process [phul[phul] Base Oro are this [thu[thu] which it counts (LiAsF₆ ), Lithium tree [phul[phul] base Oro meta alcoholic beverage gun four [thu[thu] (LiCF₃ SO₃ ), Bis - trifluoromethyl sulfonylimides lithium [LiN (CF₃ SO₂ )₂ ], And combinations thereof may be selected from the group consisting but composed, the one number are not disclosed. E.g., said lithium salt as even a higher potential for oxidation is preferably not hereinafter use electrolytes, in particular, LiPF₆ Most preferably is used as the lithium salts.

In one embodiment of the present disclosure, the anode material as said metal thin film lithium -, - lithium nickel composite oxide, lithium - cobalt composite oxide, lithium - nickel - cobalt composite oxide, spinel lithium-manganese - - nickel composite oxide, lithium - manganese - cobalt composite oxide, lithium nickel cobalt - - - manganese composite oxide, lithium - iron phosphate, and combinations thereof may be selected from the group consisting of including but composed, the number one are not disclosed. For example, the lithium - Li said metal thin film_x Mn₂ O₄ , Li_x NiO₂ , Li_x CoO₂ , Li_x Ni_1-y Co_y O₂ , Li_x Mn_2-y Ni_y O₄ , Li_x Mn_y Co_{1 Y} O₂ , Li_x Ni_1-Yz Co_y Mn_z O₂ , Li_x FePO₄ , And combinations thereof may be selected from the group consisting but including the composed, the number is one and not the (said lithium metal thin film x, y, and z each molar ratio 0 ≤ x ≤ 1, 0 ≤ y ≤ 1, 0 ≤ z ≤ 1 and about).

In one embodiment of the present disclosure, according to negative electrode active material enabling high voltage the anode voltage squalane herein are disclosed. In particular, lithium - Li as said metal thin film_a Ni_b Co_c Mn_d O₂ Using compound preferably (double, a, b, c, and d each 0 ≤ a ≤ 1 molar ratio. 1, 0. 1 ≤ b ≤ 0. 5, 0 ≤ c ≤ 0. 9, 0. 1 ≤ d ≤ 0. 5 and, more preferably said b, c, and d and the molar ratio of 0. 3 ≤ b ≤ 0. 4, 0. 3 ≤ c ≤ 0. 4, and 0. 3 ≤ d ≤ 0. 4 randomly choosing).

Hereinafter, with reference to the string in the embodiment herein it relates but, one number to the invention are not disclosed.

[In the embodiment]

In the embodiment 1: 'LTO Composite 90 Wt % + TiO₂(B) 10 Wt % ' of Composite

First, 5 mmol of TiO (OH)₂ 20 ml 5 ml 30% hydrogen peroxide on a 28% ammonia water and agitating titanium precursor solution number have high pressure liquid coolant, said 7 titanium precursor solution. 5 mmol of glycolic acid (glycolic acid) obtained by adding titanium glycolic acid (Ti glycolate) a transparent conductive layer, 80 °C extra hydrogen peroxide and ammonia was added in a stand-alone number. The, ammonia fractional developing attention by accomplishing.

Said titanium glycol acid 96% sulfuric acid obtained yellow 0. 54 ml have added, entire volume of a silicon wafer is 20 ml solution by adding distilled water. the solution makes color orange color was artificial pearl. lTO-a tiO₂ (B) number of composite when synthesizing amounts of sulfuric acid, rutile style TiO₂ Particles are combined and, when excess, other number of drug TiO type₂ Synthesized particles. The amount of sulfate formed by hydrothermal synthesis 0. 4 ml to 0. 6 ml and, in particular, 0. When the most TiO 54 ml₂ (B) particles are synthesized with a virtual path identifier, the in 0 in the embodiment. 54 ml sulfate some excellent.

Said shape obtained by an orange solution lithium titanate (lithium titanium oxide, LTO) 3 complex. 6 g-gate adding are agitated. Said LTO complex lithium titanate (Li₄ Ti₅ O₁₂ ) And about 2 wt % including material that carbon nanotube (carbon nanotube, CNT).

Teflon (Teflon) stirring said solution 20 ml syrup obtained after 24 hours in 160 °C SUS container sealing with respect to the reaction. Then, reacting said material using distilled water after washing, 100 °C TiO LTO composite 90 wt % and finally added in₂ (B) 10 wt % having a content oflTO-a tiO₂ (B) composite number was high pressure liquid coolant. Of Figure 1 (b) is, in the embodiment according to the lTO-a tiO₂ (B) scanning electron microscope (SEM) Image of composite exhibits.

In the embodiment 2: 'LTO Composite 80 Wt % + TiO₂(B) 20 Wt % ' of Composite

In the in the embodiment, LTO composite 1. 6 g other than said in the embodiment 1 is using the same method as lTO-a tiO₂ (B) composite number when the high pressure liquid coolant, the, said lTO provided tiO₂ (B) complex is 80 wt % and TiO LTO composite₂ (B) 20 wt % content of tank number as take place.

In the embodiment 3: 'LTO Composite 50 Wt % + TiO₂(B) 50 Wt % ' of Composite

In the in the embodiment, LTO composite 0. 4 g other than said in the embodiment 1 is using the same method as lTO-a tiO₂ (B) composite number when the high pressure liquid coolant, the_, Said lTO provided tiO₂ (B) complex is 50 wt % and TiO LTO composite₂ (B) 50 wt % content of tank number as take place.

Comparison example 1: pure LTO Composite

Same material used in said in the embodiment 1 to 3 LTO composite was used. (A) of Figure 1 is, said pure LTO complex exhibits SEM Image.

Characterizing

(A) of Figure 1 is (comparison example 1) SEM of LTO composite 2d, of Figure 1 (b) is 90 wt % provided tiO LTO composite₂ (B) 10 wt % SEM Image of composite of (in the embodiment 1) are disclosed. Said SEM images in hydrothermally synthesis following LTO composite spherical making sure that the memory cell is not cream, TiO₂ (B) formed on LTO composite particles were confirmed.

Figure 2, in the embodiment 1 to 3 of lTO provided tiO₂ (B) complexes, pure water of comparison example 1 LTO composite, and TiO₂ (B) (XRD) graph of X - ray diffraction analysis are disclosed. Following synthesis sequence through said graph structure is stable to maintain LTO complex, TiO₂ (B) particles are formed were confirmed. In addition, said lTO provided tiO₂ (B) TiO in composite₂ (B) increases TiO % by weight of particles₂ (B) (intensity) is associated with increased intensity of peak (peak), peak strength associated with composite LTO lTO provided tiO₂ (B) composite TiO to₂ (B) particles in the form of making sure that the capable of relatively significantly reduced.

Number attainments: And electrode for lithium secondary battery Coin type Half cell number of bath

Said in the embodiment 1 to 3, and comparison of the final powder obtained in example 1 electrode active material used therein as a high pressure liquid coolant and coin-shaped half cell electrode for lithium secondary battery (coin half cell) his number.

Said in the embodiment and comparison example according to electrode material: a super-p and KS6: ratio of parts by weight of polyvinylidene fluoride (polyvinylidene fluoride, PVDF) after securing the 89:6:5, N - methylpyrrolidone (n a-methyl-pyrrolidone, NMP) have added to, mixer and are mixed slurry with the same number his high pressure liquid coolant. A super-p and said KS6 fluorescence ratio of 2:8, has been used as conductive number, said PVDF are used as number establishes an adhesive bond.

Drying said mixture slurry is applied on one surface of the aluminum foil, pressing (pressing) process by his number between a cathode and undesirably high pressure liquid coolant. Said battery cathode diameter 1. 11 cm circular specimen by breakable fragile, a negative deflection, lithium metal sheet was used as a positive electrode.

Purification of (EC): ethyl the methyl car this [thu[thu] which it sees (EMC): to a solution blended at a volumetric ratio of a 15:50:30 (DMC) purification of dimethyl 1. 2 M of LiPF₆ When the dissolving used as electrolyte, lithium secondary battery W-a scope number C500 film membrane as separation membrane was high pressure liquid coolant.

Electrode characteristics and cell measuring electrochemical properties

Said in the embodiment 1 to 3, and comparison of the final powder obtained in example 1 electrode active material used therein as said number and coin-shaped half cell electrode for lithium secondary battery prepared by the number attainments according (coin half cell) was compared using electrode characteristics and cell electrochemical properties.

3 charging said lithium secondary cells. 0 V and discharge 1. 0 V in cut-off it is under,, when estimating the characteristic life 0. 1 C embodiment certain interval symmetrically as a transparent conductive layer, when the refresh rate characteristics each 0. 1 C, 0. 5 C, 1. 0 C, 2. 0 C, and 5. 0 C certain interval symmetrically as his embodiment.

Figure 3, in the embodiment 1 to 3, and comparison example 1 of a coin-type half cell number using high pressure liquid coolant life evaluation graph and, for table 1 have shown the same. As also shown in table 1 and 3, said in the embodiment 1, in the embodiment 2, and comparison example 1 initial battery using the lithium is reversibly introduced and 91 respectively. 6%, 89. 2%, and 93. As exhibit 0% efficiency while transition, each battery using the 80 in the embodiment 3. Comparison example 1 initial charge and discharge efficiency is decreased as compared to 4% were confirmed. This TiO₂ (B) which contribute to the formation of irreversible capacity, lTO provided tiO₂ (B) complex number when said TiO bath₂ (B) increased unsaturated fatty acid content of initially non-alkali metal in addition to form that exhibits increased. , the ferroelectric layer according to lTO provided tiO herein₂ (B) composite suitable TiO₂ (B) has been confirmed that the content of 10 wt % to about 20 wt %.

Table 2 in the embodiment 1 and comparison example 1 to 3 is to the high pressure liquid coolant using a coin-type half cell number controls C - rate (C slew rate) in battery capacity respectively. According to lTO provided tiO herein₂ (B) complex TiO₂ (B) charge and discharge capacity is increased when the steam content 20 wt % 15% overall, the LTO complex output characteristics were excellent. This titanium glycolic acid (Ti glycolate) is LTO composite within the pores uniformly adsorbed thereto, as well as composite heat when synthesizing said LTO TiO even pores₂ (B) formed a complex structure becomes uniform both stability of the increments and TiO₂ (B) named in the electromigration into a clinical use other.

For the aforementioned example of description is herein which, in the field of technical idea of person with skill in the art herein is provided herein or essential characteristics without changing other form may be understand easily outputted are disclosed. In the embodiment described above the exemplary non-limiting all sides are understood to which must substrate. For example, monolithic described embodiment in which the components may be dispersed, similarly dispersed described embodiment form made of elements binding may be disclosed.

Description herein are represented by said range of carry rather than claim, in which the meaning of and range claim, as well as some general outline evenly all changing or modified form of range should herein are interpreted.