CN105552346A - Titanium niobate/carbon composite electrode material and preparation method thereof - Google Patents
Titanium niobate/carbon composite electrode material and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
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- 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
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The invention discloses a preparation method of a titanium niobate/carbon composite electrode material belonging to the lithium ion battery material technical field. According to the method, ball mill mixing is carried out to titanium dioxide, niobium oxide and carbon source according to a certain proportion; the dried mixture is calcined under the protection of an inert gas, thus obtaining the titanium niobate/carbon composite electrode material. The invention also discloses the titanium niobate/carbon composite electrode material prepared by the preparation method. According to the invention, the conductivity of the material is improved through carbon coverage; meanwhile, a certain inhibiting effect on the particle size increasing phenomenon of the titanium niobate is realized through carbon coverage; the material shows excellent rate capability and cycle performance when being used as the lithium ion battery anode material; in addition, the material and the preparation method of the invention are featured by simple preparation technology, convenient operation and low production cost and are easy in large-scale industrial production.
Description
Technical field
The application belongs to field of lithium ion battery material, specifically, relates to a kind of titanium niobate/carbon composite electrode material and preparation method thereof.
Background technology
Lithium ion battery is widely used in the electronic product such as mobile phone, digital camera, and at present to field infiltration and developments such as electric tool, electric motor car, electrical network energy storage, this just requires that lithium ion battery has high energy density, power density and fail safe.The lithium ion battery negative material of Current commercial is mainly based on graphite-like material with carbon element, although it has good cycle performance and cheap price, because its intercalation potential is low, easily causes safety issue at high current charge-discharge or when overcharging.In addition, the high rate performance of material with carbon element is poor, can not carry out fast charging and discharging.Therefore, the high-performance negative material of development of new is badly in need of.
In recent years, niobium based compound (such as: Nb
2o
5, LiNb
3o
8, TiNb
2o
7deng) owing to having high oxidation-reduction potential (1.0-2.0V), the decomposition of organic electrolyte effectively can be suppressed, there is higher fail safe.In addition, the reversible discharge specific capacity of niobium based compound is generally at about 300mAh/g, suitable with business-like material with carbon element.So niobium based compound starts to get more and more people's extensive concerning.Recently, people's reported first such as Lin titanium niobate (TiNb
6o
17) show excellent chemical property as novel lithium ion battery negative material, first discharge specific capacity under 0.1C multiplying power is 383mAh/g, after 100 circulations, 178mAh/g. (ChunfuLin is remained under 5C multiplying power, GuizhenWang, ShuiweiLin, JianbaoJi, LiLu.TiNb
6o
17: anewelectrodematerialforlithium-ionbatteries.Chem.Commun .2015,51:8970-8973.).Although the better performances of titanium niobate material under low range prepared by the people such as Lin, its performance under large multiplying power need further raising.TiNb
6o
17similar with other niobium based compound, its electronics and ionic conductivity lower, this is also the main cause causing its high rate performance undesirable.
Summary of the invention
In view of this, the application is for TiNb
6o
17the problem that the high rate performance that material causes because its conductivity is low is low, provides a kind of titanium niobate/carbon composite electrode material and preparation method thereof, and this preparation method's technique is simple, easy to operate, is easy to large-scale production, and the high rate performance of product is excellent.
In order to solve the problems of the technologies described above, this application discloses a kind of preparation method of titanium niobate/carbon composite electrode material, comprising the following steps:
A, take titanium dioxide, niobium oxide and carbon source, these three kinds of materials are placed in ball grinder, are decentralized medium with ethanol, and ball milling on ball mill, makes raw material fully mix;
B, step a gained mixture is dry, obtain presoma;
C, step b gained presoma to be calcined under inert gas shielding, after Temperature fall to normal temperature, namely obtain titanium niobate/carbon composite electrode material.
Further, the atomic ratio of Ti and Nb in step a in titanium dioxide and niobium oxide is 1:5.5-1:6.5; The quality of described carbon source is the 0.5%-50% of titanium dioxide and niobium oxide gross mass.
Further, the titanium dioxide in step a is one or more in rutile titanium dioxide, anatase titanium dioxide, P25 type titanium dioxide; Niobium oxide in step a is one or more in columbium dioxide, niobium pentaoxide, columbium sesquioxide.
Further, the carbon source in step a is one or more in citric acid, glucose, sucrose, carbon black, acetylene black, graphite, Graphene, graphene oxide.
Further, the rotational speed of ball-mill in step a is 200-850 rev/min, and described Ball-milling Time is 0.5-30 hour.
Further, the baking temperature in step b is 60-110 DEG C.
Further, the inert atmosphere in step c is one in nitrogen, argon gas or its mist.
Further, in step c, calcining heat is 700-1400 DEG C; Calcination time is 1-56 hour.
Further, the calcination time in step c is 6-40 hour.
Disclosed herein as well is a kind of titanium niobate/carbon composite electrode material prepared by above-mentioned preparation method, the carbon content in this titanium niobate/carbon composite electrode material is 0.5-20wt%.
Compared with prior art, the application can obtain and comprise following technique effect:
1) the present invention utilizes step high temperature solid-state method fabricated in situ titanium niobate/carbon composite electrode material, improves the conductivity of material, and the coated increase of the particle to the titanium niobate phenomenon of carbon-coating has certain inhibitory action simultaneously.
2) preparation technology of the present invention is simple, easy to operate, cheap, is easy to large-scale industrial and produces.
3) titanium niobate/carbon composite electrode material that prepared by the present invention has excellent circulation performance, and the specific discharge capacity under 5 and 10C multiplying power after 50 circulations remains on 225.5 and 214.3mAh/g, does not almost decay.
Certainly, the arbitrary product implementing the application must not necessarily need to reach above-described all technique effects simultaneously.
Accompanying drawing explanation
Accompanying drawing described herein is used to provide further understanding of the present application, and form a application's part, the schematic description and description of the application, for explaining the application, does not form the improper restriction to the application.In the accompanying drawings:
Fig. 1 is the XRD figure of titanium niobate/carbon composite electrode material that the embodiment of the present application 1 prepares;
Fig. 2 is the stereoscan photograph of titanium niobate/carbon composite electrode material that the embodiment of the present application 1 prepares;
Fig. 3 is the transmission electron microscope photo of titanium niobate/carbon composite electrode material that the embodiment of the present application 1 prepares;
Fig. 4 is the chemical property curve chart of titanium niobate/carbon composite electrode material under 5 and 10C multiplying power that the embodiment of the present application 1 prepares.
Embodiment
Drawings and Examples will be coordinated below to describe the execution mode of the application in detail, by this to the application how application technology means solve technical problem and the implementation procedure reaching technology effect can fully understand and implement according to this.
Embodiment 1
A, take rutile titanium dioxide and niobium pentaoxide by atomic ratio Ti:Nb=1:5.88, and then take a certain amount of citric acid, wherein, the quality of citric acid is 5% of carbon dioxide and niobium oxide gross mass, these three kinds of materials are placed in ball grinder, be decentralized medium with ethanol, with 600 revs/min of ball millings 24 hours on ball mill, raw material fully mixed;
B, step a gained mixture is dry at 71 DEG C, obtain presoma;
C, by step b gained presoma under argon shield, at 1300 DEG C calcine 52 hours, namely obtain titanium niobate/carbon composite electrode material after Temperature fall to normal temperature.
The experimental result of titanium niobate/carbon composite electrode material prepared by embodiment 1 as Figure 1-Figure 4.
Fig. 1 is the XRD figure of titanium niobate/carbon composite electrode material that the present embodiment 1 prepares, and as seen from the figure, the diffraction maximum of sample and the standard diffraction peak of titanium niobate match, and do not find other impurity peaks, illustrates that the sample of preparation is purer.
Fig. 2 is the stereoscan photograph of titanium niobate/carbon composite electrode material that the present embodiment 1 prepares, and can find from figure, and sample presents column pattern, and sample size is about 0.7-1.2 micron.
Fig. 3 is the transmission electron microscope photo of titanium niobate/carbon composite electrode material prepared by the present embodiment 1; Can be found there is the carbon-coating of thin layer in titanium niobate edge of materials by figure, size is about 1-2 nanometer.
Fig. 4 is the chemical property curve chart under 5 and 10C multiplying power of titanium niobate/carbon composite electrode material prepared by the present embodiment 1.From figure, the first discharge specific capacity of sample under 5 and 10C multiplying power is respectively 225.2 and 221mAh/g, and the specific discharge capacity after 50 circulations remains on 225.5 and 214.3mAh/g, and capacity is not almost decayed.
Embodiment 2
A, take rutile titanium dioxide and columbium dioxide by atomic ratio Ti:Nb=1:6.35, and then take a certain amount of acetylene black, wherein, the quality of acetylene black is 2% of carbon dioxide and niobium oxide gross mass, these three kinds of materials are placed in ball grinder, be decentralized medium with ethanol, with 280 revs/min of ball millings 19 hours on ball mill, raw material fully mixed;
B, step a gained mixture is dry at 78 DEG C, obtain presoma;
C, by step b gained presoma under nitrogen protection, calcines 35 hours, namely obtains titanium niobate/carbon composite electrode material after Temperature fall to normal temperature at 950 DEG C.
Embodiment 3
A, to take anatase titanium dioxide and three oxidation two girls by atomic ratio Ti:Nb=1:6.16, and then take a certain amount of graphite, wherein, the quality of graphite is 13% of carbon dioxide and niobium oxide gross mass, these three kinds of materials are placed in ball grinder, be decentralized medium with ethanol, with 320 revs/min of ball millings 20 hours on ball mill, raw material fully mixed;
B, step a gained mixture is dry at 90 DEG C, obtain presoma;
C, by step b gained presoma under nitrogen protection, calcines 39 hours, namely obtains titanium niobate/carbon composite electrode material after Temperature fall to normal temperature at 1190 DEG C.
Embodiment 4
A, to take P25 type titanium dioxide and three oxidation two girls by atomic ratio Ti:Nb=1:5.5, and then take a certain amount of glucose, wherein, the quality of glucose is 0.5% of P25 type titanium dioxide and three oxidation two girl's gross masses, these three kinds of materials are placed in ball grinder, be decentralized medium with ethanol, with 200 revs/min of ball millings 30 hours on ball mill, raw material fully mixed;
B, step a gained mixture is dry at 60 DEG C, obtain presoma;
C, by step b gained presoma under nitrogen protection, calcines 56 hours, namely obtains titanium niobate/carbon composite electrode material after Temperature fall to normal temperature at 700 DEG C.
Embodiment 5
A, take rutile titanium dioxide and niobium pentaoxide by atomic ratio Ti:Nb=1:6.5, and then take a certain amount of sucrose, wherein, the quality of sucrose is 20% of rutile titanium dioxide and niobium pentaoxide gross mass, these three kinds of materials are placed in ball grinder, be decentralized medium with ethanol, with 850 revs/min of ball millings 0.5 hour on ball mill, raw material fully mixed;
B, step a gained mixture is dry at 110 DEG C, obtain presoma;
C, by step b gained presoma under nitrogen protection, calcines 1 hour, namely obtains titanium niobate/carbon composite electrode material after Temperature fall to normal temperature at 1400 DEG C.
Embodiment 6
A, take rutile titanium dioxide and niobium pentaoxide by atomic ratio Ti:Nb=1:5.8, and then take a certain amount of sucrose, wherein, the quality of sucrose is 8% of rutile titanium dioxide and niobium pentaoxide gross mass, these three kinds of materials are placed in ball grinder, be decentralized medium with ethanol, with 750 revs/min of ball millings 0.5 hour on ball mill, raw material fully mixed;
B, step a gained mixture is dry at 90 DEG C, obtain presoma;
C, by step b gained presoma under nitrogen protection, calcines 6 hours, namely obtains titanium niobate/carbon composite electrode material after Temperature fall to normal temperature at 1000 DEG C.
Embodiment 7
A, take rutile titanium dioxide and niobium pentaoxide by atomic ratio Ti:Nb=1:6.5, and then take a certain amount of sucrose, wherein, the quality of sucrose is 18% of rutile titanium dioxide and niobium pentaoxide gross mass, these three kinds of materials are placed in ball grinder, be decentralized medium with ethanol, with 800 revs/min of ball millings 0.5 hour on ball mill, raw material fully mixed;
B, step a gained mixture is dry at 70 DEG C, obtain presoma;
C, by step b gained presoma under nitrogen protection, calcines 40 hours, namely obtains titanium niobate/carbon composite electrode material after Temperature fall to normal temperature at 1200 DEG C.
The present invention is directed to the low problem causing poor performance of titanium niobate conductivity, by preparing titanium niobate/carbon composite with the material with carbon element compound of high conductivity, improving the chemical property of material; By organic carbon source (such as: glucose, sucrose, citric acid) high temperature cabonization or directly introduce inorganic carbon source (such as: graphite, carbon black, graphene oxide etc.), the introducing of carbon source has certain inhibitory action to growing up of titanium niobate crystal grain in addition.In preparation method, ball milling speed directly can affect the chemical property of titanium niobate/carbon composite, and its span is 200-850 rev/min, and the low sample mix of rotating speed is uneven, and rotating speed is too high can increase equipment investment cost and energy consumption.Meanwhile, sintering temperature also can affect the chemical property of titanium niobate/carbon composite, and its span is 700-1400 DEG C; Can not synthesize titanium niobate/carbon products when temperature is low or the low chemical property of product crystallization that is synthesized poor, the too high increase energy consumption of temperature, and the particle growth of product, chemical property can be made poor.Carbon content also can affect the chemical property of titanium niobate/carbon composite, and its span is 0.5-20wt%, and carbon content is too low does not have the effect increasing material electric conductivity, the too high high rate performance that can lower material of carbon content, and can increase production cost.
As employed some vocabulary to censure special component or method in the middle of specification and claim.Those skilled in the art should understand, and same composition may be called with different noun in different regions.This specification and claims are not used as with the difference of title the mode distinguishing composition." comprising " as mentioned in the middle of specification and claim is in the whole text an open language, therefore should be construed to " comprise but be not limited to "." roughly " refer to that in receivable error range, those skilled in the art can solve the technical problem within the scope of certain error, reach described technique effect substantially.Specification subsequent descriptions is implement the better embodiment of the application, and right described description is for the purpose of the rule that the application is described, and is not used to the scope limiting the application.The protection range of the application is when being as the criterion depending on the claims person of defining.
Also it should be noted that, term " comprises ", " comprising " or its any other variant are intended to contain comprising of nonexcludability, thus make to comprise the commodity of a series of key element or system not only comprises those key elements, but also comprise other key elements clearly do not listed, or also comprise by this commodity or the intrinsic key element of system.When not more restrictions, the key element limited by statement " comprising ... ", and be not precluded within the commodity or system comprising described key element and also there is other identical element.
Above-mentioned explanation illustrate and describes some preferred embodiments of invention, but as previously mentioned, be to be understood that invention is not limited to the form disclosed by this paper, should not regard the eliminating to other embodiments as, and can be used for other combinations various, amendment and environment, and can in invention contemplated scope described herein, changed by the technology of above-mentioned instruction or association area or knowledge.And the change that those skilled in the art carry out and change do not depart from the spirit and scope of invention, then all should in the protection range of invention claims.
Claims (10)
1. a preparation method for titanium niobate/carbon composite electrode material, is characterized in that, comprises the following steps:
A, take titanium dioxide, niobium oxide and carbon source, these three kinds of materials are placed in ball grinder, are decentralized medium with ethanol, and ball milling on ball mill, makes raw material fully mix;
B, step a gained mixture is dry, obtain presoma;
C, step b gained presoma to be calcined under inert gas shielding, after Temperature fall to normal temperature, namely obtain titanium niobate/carbon composite electrode material.
2. the preparation method of titanium niobate/carbon composite electrode material according to claim 1, is characterized in that, the atomic ratio of Ti and Nb in described step a in titanium dioxide and niobium oxide is 1:5.5-1:6.5; The quality of described carbon source is the 0.5%-50% of titanium dioxide and niobium oxide gross mass.
3. the preparation method of titanium niobate/carbon composite electrode material according to claim 1, is characterized in that, the titanium dioxide in described step a is one or more in rutile titanium dioxide, anatase titanium dioxide, P25 type titanium dioxide; Niobium oxide in step a is one or more in columbium dioxide, niobium pentaoxide, columbium sesquioxide.
4. the preparation method of titanium niobate/carbon composite electrode material according to claim 1, is characterized in that, the carbon source in described step a is one or more in citric acid, glucose, sucrose, carbon black, acetylene black, graphite, Graphene, graphene oxide.
5. the preparation method of titanium niobate/carbon composite electrode material according to claim 1, is characterized in that, the rotational speed of ball-mill in described step a is 200-850 rev/min, and described Ball-milling Time is 0.5-30 hour.
6. the preparation method of titanium niobate/carbon composite electrode material according to claim 1, is characterized in that, the baking temperature in described step b is 60-110 DEG C.
7. the preparation method of titanium niobate/carbon composite electrode material according to claim 1, is characterized in that, the inert atmosphere in described step c is one in nitrogen, argon gas or its mist.
8. the preparation method of titanium niobate/carbon composite electrode material according to claim 1, is characterized in that, in described step c, calcining heat is 700-1400 DEG C; Calcination time is 1-56 hour.
9. the preparation method of titanium niobate/carbon composite electrode material according to claim 8, is characterized in that, the calcination time in described step c is 6-40 hour.
10. titanium niobate/the carbon composite electrode material prepared by the preparation method described in claim arbitrary in claim 1-8, is characterized in that, the carbon content in this titanium niobate/carbon composite electrode material is 0.5-20wt%.
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