CN110137481A - Carbon coating oxygen defect titanium niobate negative electrode material and preparation method thereof and lithium battery - Google Patents

Carbon coating oxygen defect titanium niobate negative electrode material and preparation method thereof and lithium battery Download PDF

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CN110137481A
CN110137481A CN201910508405.9A CN201910508405A CN110137481A CN 110137481 A CN110137481 A CN 110137481A CN 201910508405 A CN201910508405 A CN 201910508405A CN 110137481 A CN110137481 A CN 110137481A
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oxygen defect
titanium
negative electrode
electrode material
carbon coating
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杨志远
王聪
张天赐
陈中华
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Hubei Lithium Nuo Amperex Technology Ltd
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Hubei Lithium Nuo Amperex Technology Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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Abstract

The invention discloses a kind of carbon coating oxygen defect titanium niobate negative electrode material and preparation method thereof and lithium batteries, belong to technical field of lithium batteries.The preparation method includes that surfactant reacts with niobium source, titanium source Hybrid Heating and oxygen defect titanium niobium oxide is made through first time calcination processing, after oxygen defect titanium niobium oxide is mixed with carbon source again, carbon coating oxygen defect titanium niobate negative electrode material is made through second of calcination processing；Wherein, surfactant, niobium source and titanium source mass ratio are as follows: (0.5~1.0): (0.6~1.8): (0.2~0.4).The negative electrode material that the present invention designs is due to oxygen defect and carbon-coated synergistic effect, so that the chemical property of entire titanium niobium oxide negative electrode material is greatly improved.

Description

Carbon coating oxygen defect titanium niobate negative electrode material and preparation method thereof and lithium battery
Technical field
The present invention relates to oxide cathode materials, belong to chemical cell technical field, more particularly to a kind of carbon coating oxygen Defect titanium niobate negative electrode material and preparation method thereof and lithium battery.
Background technique
Lithium battery is as a kind of main energy storage device, since it is with weight and volume energy density height, cycle life It the features such as length, dynamic performance superiority, plays an important role in many fields.But to electric car and hybrid power vapour More stringent requirements are proposed for the lithium ion battery technology of vehicle.For lithium ion battery negative material, people are had been made quite Big effort, such as metal oxide, metal sulfide, metal carbides, silicon and silicon alloy, but this kind of material is de-/embedding Volume expansion is violent during lithium, and cyclical stability is caused to be deteriorated.Therefore, different substitution negative electrode material occurs and extensive Research, such as lithium titanate and titanium niobium oxide, because they have excellent structural stability, high circulation performance and without SEI film shape At.
Titanium niobium oxide mainly includes TiNb at present2O7、Ti2Nb10O29、TiNb24O62Deng based on Nb5+And Nb3+Between Two electron reactions and Ti4+And Ti3+Between single electron reaction, two class titanium niobium oxide TiNb being widely noticed at present2O7、 Ti2Nb10O29Theoretical capacity be up to 388mAh/g and 396mAh/g respectively, it is higher than lithium titanate theoretical capacity more than 1 times.But titanium Ti in niobium oxide4+And Nb5+All in highest valence state, so there is no not pairs of electronics in titanium niobium oxide, lead to its electronics Conductivity is very low.Therefore, their application is caused to be restricted.
Due to be inserted into lithium ion/extraction process in volume change almost can be ignored, and since its is higher It is inserted into voltage and improves safety, therefore Lacking oxygen material is most popular one of negative electrode material.Lacking oxygen reinforcing material Electric conductivity, in the insertion and extraction process of lithium ion, Lacking oxygen helps to maintain structure, to mention than original electrodes material High circulation performance.Additional lithium ion can be stored in the Lacking oxygen in crystal, to accelerate the diffusion of lithium ion.Oxygen defect With the chemical property of carbon coating collaboration titanium niobium oxide.
Summary of the invention
To solve the problems, such as titanium niobium oxide negative electrode material poorly conductive, the present invention provides a kind of carbon coating oxygen defect niobiums Sour titanium negative electrode material and preparation method thereof and lithium battery.Due to oxygen defect and carbon coating, so that entire titanium niobium oxide cathode material The chemical property of material is greatly improved.
To achieve the above object, the invention discloses a kind of preparation method of carbon coating oxygen defect titanium niobate negative electrode material, It includes that surfactant reacts with niobium source, titanium source Hybrid Heating and the oxidation of oxygen defect titanium niobium is made through first time calcination processing After the oxygen defect titanium niobium oxide is mixed with carbon source again, carbon coating oxygen defect titanium niobate is made through second of calcination processing in object Negative electrode material；Surfactant, niobium source and titanium source mass ratio are as follows: (0.5~1.0): (0.6~1.8): (0.2~0.4).
Preferably, surfactant, niobium source and titanium source mass ratio are as follows: (0.5~1.0): (0.66~1.59): (0.28 ~0.36).
Further, the surfactant includes polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer At least one of object or cetyl trimethylammonium bromide.The surfactant is self-assembly of nano grade titanium of uniform size Niobium oxide, so that carbon coating is easier to coat.
Further, the heating reaction temperature be 180~200 DEG C, the reaction time be 20~for 24 hours.
Further, the first time calcination processing is to be placed in Ar+H2In atmosphere, calcination temperature is 600~800 DEG C, is forged The burning time is 4~6h.
Wherein, the oxygen defect in the oxygen defect titanium niobium oxide may cause electronics and the transmission of ion can be low, but by It is arranged in vacancy, directly increases the contact area of electrode-electric solution matter, and additional lithium ion is stored in Lacking oxygen, contracting The short diffusion length of lithium ion and electronics indirectly accelerates lithium ion diffusion, is conducive to improve whole chemical property.
Further, the gas volume percentage, Ar:H2=(90%~95%): (5%~10%).
Preferably, the gas volume percentage, Ar:H2=95%:5%.
Further, the niobium source includes at least one of niobium pentaoxide, columbium pentachloride or five ethyoxyl niobiums.
Further, the titanium source includes titanium dioxide, butyl titanate, isopropyl titanate, two (levulinic ketone group) titaniums At least one of sour diisopropyl ester, titanium tetrachloride or titanium sulfate.
Further, second of calcination processing is to be placed in argon atmosphere, and calcination temperature is 260~280 DEG C, calcining Time is 2~6h.
Preferably, the carbon source includes malic acid.This is because malic acid low melting point, can be carbonized in air low temperature； It only needs to calcine 265 DEG C or so in carbon coating and can form carbon coating.
Preferably, the mass ratio of the malic acid and oxygen defect titanium niobium oxide is 1:2.
By second of calcination processing, it has been made and has had amorphous carbon layer and be coated in titanium niobium oxide negative electrode material.Its In, carbon coating layer provides electronics conduction pathway, and facilitates the lithium ion transport between active phase, improves in embedding lithium and takes off Chemical property during lithium；It can also effectively buffer volumes expand, keep structural intergrity.
In order to preferably realize the technology of the present invention purpose, the invention discloses a kind of carbon coating oxygen defect titanium niobate cathode materials Material, it is to be made using above-mentioned preparation method.
In order to preferably realize the technology of the present invention purpose, the invention also discloses a kind of lithium batteries, it includes using above-mentioned Negative electrode material made from preparation method.
The beneficial effects are mainly reflected as follows following aspects:
There are oxygen defects for titanium niobium oxide in the negative electrode material that the present invention designs, this has the titanium niobium oxide table of oxygen defect Face is coated with carbon-coating again, due to the synergistic effect between carbon coating layer and the titanium niobium oxide for having oxygen defect, so that entire negative The electric conductivity of pole material is greatly increased.
Detailed description of the invention
Fig. 1 is electrical performance testing of embodiment of the present invention map；
Fig. 2 is coulombic efficiency comparison diagram for the first time of the embodiment of the present invention.
Specific embodiment
The invention discloses a kind of preparation methods of carbon coating oxygen defect titanium niobate negative electrode material, it includes taking surface-active Agent is dissolved in dehydrated alcohol；It is transferred in reaction kettle after HCl solution, niobium source and titanium source stirring is added, reaction temperature is 180~200 DEG C, the reaction time be 20~for 24 hours.It reacts obtained mixture and is containing Ar+H2It is calcined in atmosphere, calcination temperature is 600~800 DEG C, calcination time is 4~6h, obtains oxygen defect titanium niobium oxide, malic acid is taken to be dissolved in toluene, and aoxidize with oxygen defect titanium niobium Object is mixed, and is then dried in vacuo to obtain mixture low temperature calcination in tube furnace again, and calcination temperature is 260~280 DEG C, is forged The burning time is 2~6h, obtains carbon coating oxygen defect titanium niobium oxide negative electrode material.
In order to better explain the present invention, below in conjunction with the specific embodiment main contents that the present invention is furture elucidated, but The contents of the present invention are not limited solely to following embodiment.
Embodiment 1
A kind of preparation method of carbon coating oxygen defect titanium niobate negative electrode material, it includes:
0.5g polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer P123 is taken to be dissolved in the anhydrous second of 60mL Alcohol is added 3mL 12mol/L HCl and stirs 30min, 0.66g niobium pentaoxide Nb is then added2O5With 0.34g butyl titanate TBOT stirs 30min, is transferred in reaction kettle and reacts for 24 hours for 180 DEG C.After washing, drying, in tube furnace Ar (95%)+H2(5%) 600 DEG C of calcining 4h obtain oxygen defect titanium niobium oxide (Ti in atmosphere2Nb10O29-x)。
The preparation of carbon coating oxygen defect titanium niobium oxide: 1g Ti is taken2Nb10O29-xWith the toluene containing 0.5g malic acid Be mixed, oxygen defect titanium niobate: mixing 12h is stirred at room temperature, then in vacuum environment in mass ratio=2:1 of malic acid Dry 12h at 120 DEG C.Obtaining mixture, 260 DEG C of calcining 6h obtain carbon coating oxygen defect titanium niobium under argon atmosphere in tube furnace Oxide.
Embodiment 2
A kind of preparation method of carbon coating oxygen defect titanium niobate negative electrode material, it includes:
It takes 0.5g cetyl trimethylammonium bromide CTAB to be dissolved in 60mL dehydrated alcohol, 3mL12mol/L HCl stirring is added Then 1.35g columbium pentachloride NbCl is added in 30min530min is stirred with 0.28g isopropyl titanate TTIP, is transferred in reaction kettle 190 DEG C of reaction 22h.After washing, drying, in tube furnace Ar (95%)+H2(5%) 700 DEG C of calcining 5h obtain oxygen defect in atmosphere Titanium niobate (Ti2Nb10O29-x)。
The preparation of carbon coating oxygen defect titanium niobate: 1g Ti is taken2Nb10O29-xWith the mixing of the toluene containing 0.5g malic acid Stirring, oxygen defect titanium niobate: mixing 12h is stirred at room temperature, then at 140 DEG C of vacuum environment in malic acid mass ratio=2:1 Keep dry 11h.Obtaining mixture, 270 DEG C of calcining 4h obtain the oxidation of carbon coating oxygen defect titanium niobium under argon atmosphere in tube furnace Object.
Embodiment 3
A kind of preparation method of carbon coating oxygen defect titanium niobate negative electrode material, it includes:
It takes 1g cetyl trimethylammonium bromide CTAB to be dissolved in 60mL dehydrated alcohol, 3mL 12mol/L HCl stirring is added Then five ethyoxyl niobium Nb (OC of 1.59g is added in 30min2H5)5It is stirred with (levulinic ketone group) the metatitanic acid diisopropyl ester of 0.36g bis- DTA 30min is mixed, 200 DEG C of reaction 20h in reaction kettle are transferred to.After washing, drying, in tube furnace Ar (95%)+H2(5%) in atmosphere 800 DEG C of calcining 4h obtain oxygen defect titanium niobate (Ti2Nb10O29-x)。
The preparation of carbon coating oxygen defect titanium niobate: 2g Ti is taken2Nb10O29-xMixing with the toluene containing 1g malic acid is stirred Oxygen defect titanium niobate: mass ratio=2:1 of malic acid is mixed, mixing 12h is stirred at room temperature, then at 160 DEG C of vacuum environment Keep dry 10h.Obtaining mixture, 280 DEG C of calcining 2h obtain the oxidation of carbon coating oxygen defect titanium niobium under argon atmosphere in tube furnace Object.
Embodiment 4
A kind of preparation method of carbon coating titanium niobate negative electrode material, it includes:
1g polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer P123 is taken to be dissolved in 60mL dehydrated alcohol, 3mL 12mol/L HCl is added and stirs 30min, five ethyoxyl niobium Nb (OC of 1.59g is then added2H5)5) and 0.28g metatitanic acid isopropyl Ester TTIP stirs 30min, is transferred to 200 DEG C of reaction 20h in reaction kettle.After washing, drying, 700 DEG C of calcining 5h are obtained in air To titanium niobate (Ti2Nb10O29)。
The preparation of carbon coating titanium niobate: 2g Ti is taken2Nb10O29With the mixing oxygen defect of the toluene containing 1g malic acid Titanium niobate: mass ratio=2:1 of malic acid is stirred at room temperature mixing 12h, then keeps drying at 160 DEG C of vacuum environment 10h.Obtaining mixture, 270 DEG C of calcining 4h obtain carbon coating oxygen defect titanium niobium oxide under argon atmosphere in tube furnace.
Embodiment 5
A kind of preparation method of oxygen defect titanium niobate negative electrode material, it includes:
1g polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer P123 is taken to be dissolved in 60mL dehydrated alcohol, 3mL 12mol/L HCl is added and stirs 30min, five ethyoxyl niobium Nb (OC of 1.59g is then added2H5)5) and 0.28g metatitanic acid isopropyl Ester TTIP stirs 30min, is transferred to 200 DEG C of reaction 20h in reaction kettle.After washing, drying, 700 DEG C of calcining 5h are obtained in air To titanium niobate (Ti2Nb10O29)。
Embodiment 6
The preparation method of titanium niobium oxide negative electrode material without coating modification, it includes:
0.5g P123 is taken to be dissolved in 60mL dehydrated alcohol；3mL 12mol/L HCl is added and stirs 30min, is then added 0.66g niobium pentaoxide Nb2O530min is stirred with 0.34g butyl titanate TBOT, is transferred to 200 DEG C of reaction 20h in reaction kettle. After washing, drying, 750 DEG C of calcining 5h obtain titanium niobium oxide (Ti in tubular type stove air2Nb10O29)。
Table 1 is carbon coating oxygen defect titanium niobium oxide and the titanium niobium oxide negative electrode material without coating modification in 10C The comparison of discharge capacity and capacity retention ratio after discharge capacity, circulation 100 are enclosed for the first time.
From table 1 it follows that the discharge capacity for the first time of Examples 1 to 3 is 272.1~275.1mAh/g, embodiment 4 Discharge capacity is 250.5mAh/g for the first time, and the discharge capacity for the first time of embodiment 5 is 260.8mAh/g, the electric discharge for the first time of embodiment 6 Capacity is 226.3mAh/g；The discharge capacity for implementing 1~3 after 100 circle of circulation is 254.7~258.1mAh/g, implements 4 electric discharge Capacity is 226.5mAh/g；The discharge capacity for implementing 5 is 237.6mAh/g, and the discharge capacity for implementing 6 is 199.3mAh/g；Implement 1~3 capacity retention ratio is 93.6~94.0%, and the capacity retention ratio for implementing 4~6 is 88.2~91.1%.This may be because The contact area of electrode-electric solution matter is not only increased for the oxygen defect in titanium niobium oxide, and shortens lithium ion and electronics Diffusion length.And carbon coating layer provides electronics conduction pathway, and facilitates the lithium ion transport between active phase, improves Chemical property during embedding and removing；It can also effectively buffer volumes expand, keep structural intergrity.
Fig. 1 is the ac impedance spectroscopy of embodiment 2 and embodiment 6.Pass through the provable chemical property of electrochemical impedance Enhancing.As shown in Figure 1, embodiment 2 has smaller semicircle than embodiment 6, this shows carbon coating oxygen defect titanium niobium oxide electricity Ultimate ratio titanium niobium oxide electrode has lower charge transfer resistance.
Fig. 2 is the coulombic efficiency for the first time of Examples 1 to 6.The coulombic efficiency for the first time for implementing 1~3 is 86.7~87.9%, real The coulombic efficiency for the first time for applying 4~6 is 75.3~82.6%.The charge that the presence of carbon can further enhance combination electrode surface passes It is defeated, and improve coulombic efficiency for the first time.
Above embodiments are only best citing, rather than a limitation of the embodiments of the present invention.Except above-described embodiment Outside, there are also other embodiments by the present invention.All technical solutions formed using equivalent substitution or equivalent transformation, all fall within the present invention It is required that protection scope.

Claims (10)

1. a kind of preparation method of carbon coating oxygen defect titanium niobate negative electrode material, it includes that surfactant and niobium source, titanium source are mixed Close heating reaction and through first time calcination processing be made oxygen defect titanium niobium oxide, the oxygen defect titanium niobium oxide again with carbon source After mixing, carbon coating oxygen defect titanium niobate negative electrode material is made through second of calcination processing；Surfactant, niobium source and titanium source Mass ratio are as follows: (0.5~1.0): (0.6~1.8): (0.2~0.4).
2. the preparation method of carbon coating oxygen defect titanium niobate negative electrode material according to claim 1, it is characterised in that: the table Face activating agent includes polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer or cetyl trimethyl bromination At least one of ammonium.
3. the preparation method of carbon coating oxygen defect titanium niobate negative electrode material according to claim 1 or claim 2, it is characterised in that: institute State heating reaction temperature be 180~200 DEG C, the reaction time be 20~for 24 hours.
4. the preparation method of carbon coating oxygen defect titanium niobate negative electrode material according to claim 1 or claim 2, it is characterised in that: institute Stating first time calcination processing is to be placed in Ar+H2In atmosphere, calcination temperature is 600~800 DEG C, and calcination time is 4~6h.
5. the preparation method of carbon coating oxygen defect titanium niobate negative electrode material according to claim 4, it is characterised in that: the gas Body percent by volume, Ar:H2=(90%~95%): (5%~10%).
6. the preparation method of carbon coating oxygen defect titanium niobate negative electrode material according to claim 1 or claim 2, it is characterised in that: institute Stating niobium source includes at least one of niobium pentaoxide, columbium pentachloride or five ethyoxyl niobiums.
7. the preparation method of carbon coating oxygen defect titanium niobate negative electrode material according to claim 1 or claim 2, it is characterised in that: institute State titanium source include titanium dioxide, butyl titanate, isopropyl titanate, two (levulinic ketone group) metatitanic acid diisopropyl esters, titanium tetrachloride, Or at least one of titanium sulfate.
8. the preparation method of carbon coating oxygen defect titanium niobate negative electrode material according to claim 1 or claim 2, it is characterised in that: institute Stating second of calcination processing is to be placed in argon atmosphere, and calcination temperature is 260~280 DEG C, and calcination time is 2~6h.
9. a kind of carbon coating oxygen defect titanium niobate negative electrode material, it is characterised in that: it is using any one in claim 1~8 Item preparation method is made.
10. a kind of lithium battery, it is characterised in that: it includes cathode material made from any one of claim 1~8 preparation method Material.
CN201910508405.9A 2019-06-12 2019-06-12 Carbon coating oxygen defect titanium niobate negative electrode material and preparation method thereof and lithium battery Pending CN110137481A (en)

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CN114477284A (en) * 2022-03-16 2022-05-13 中物院成都科学技术发展中心 Method for preparing titanium niobium oxide
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Publication number Priority date Publication date Assignee Title
US11799077B2 (en) 2020-06-03 2023-10-24 Echion Technologies Limited Active electrode material
WO2022043701A1 (en) * 2020-08-28 2022-03-03 Echion Technologies Limited Active electrode material
WO2022043705A1 (en) * 2020-08-28 2022-03-03 Echion Technologies Limited Active electrode material
US11721806B2 (en) 2020-08-28 2023-08-08 Echion Technologies Limited Active electrode material
US11973220B2 (en) 2020-08-28 2024-04-30 Echion Technologies Limited Active electrode material
CN112701260A (en) * 2020-12-25 2021-04-23 华中科技大学 In-situ carbon-coated titanium niobate composite material and preparation method and application thereof
CN113380994A (en) * 2021-04-26 2021-09-10 厦门大学 Carbon-coated oxide electrode without adhesive and oxygen-containing defects and battery
CN114477284A (en) * 2022-03-16 2022-05-13 中物院成都科学技术发展中心 Method for preparing titanium niobium oxide
CN114477284B (en) * 2022-03-16 2023-12-05 中物院成都科学技术发展中心 Method for preparing titanium niobium oxide

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