CN106784681B - A kind of preparation method of the lithium titanate composite material of granularity integrated distribution - Google Patents
A kind of preparation method of the lithium titanate composite material of granularity integrated distribution Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of the lithium titanate composite material of granularity integrated distribution, belong to new forms of energy new material technical field.Metal salt solution, lithium source solution, chelating agent solution are added in titanium source solution in such a way that sequence is added dropwise, and form milky colloidal sol.Colloidal sol water-bath gelation, gelation presoma after processing, carry out carbon coating and obtain composite modified lithium titanate composite material.The present invention controls titanium source hydrolysis degree, controls the size distribution of product, then to the further centralization of size distribution.While size distribution is concentrated, the doping of metal ion and the great conductivity for improving lithium titanate material of the cladding of carbon improve the cycle performance and high rate performance of material.
Description
Technical field
The invention belongs to a kind of technical field of lithium batteries, are related to a kind of system of the lithium titanate composite material of granularity integrated distribution
Preparation Method.
Technical background
Since lithium ion battery be born since, the negative electrode material studied mainly has: carbon material, nitride, tin-based material,
Silica-base material, nano-oxide etc..In numerous negative electrode materials, still carbon materials of the current really large-scale application in production
Material.But due to insert lithium after carbon electrode current potential and lithium metal current potential very close to, when over-charging of battery, lithium metal may carbon electricity
Pole surface is precipitated and forms Li dendrite, so as to cause short circuit；And mostly electrolyte is unstable under this current potential, electrolyte
It is easily decomposed in electrode surface, generates combustible gas mixture, there is security risks；In addition, Li in carbon electrode+Insertion will draw
The volume deformation for playing 10%, cause it is intergranular discontinuous, cause electrode/electrolyte and electrode/afflux body interface it is loose with
It peels off.These factors all promote researchers to modify original negative electrode material and study on the modification, and constantly look for performance
Excellent novel cathode material for lithium ion battery.
Li4Ti5O12The current potential of opposite lithium electrode is 1.55V, theoretical capacity 175mAh/g, and experiment specific capacity reaches
165mAh/g or more.Li+Insertion and deintercalation have little effect material structure, referred to as " zero strain " material, have circulation
Function admirable, discharging voltage balance, intercalation potential it is high and be not easy to cause lithium metal be precipitated, can be in most liquid electrolyte
The good characteristics such as the use of burning voltage section, coulombic efficiency high (close to 100%), the wide, clean and environmental protection of material source, under having
Charging times necessary to generation lithium ion battery are more, the characteristic of charging process faster, safer.In addition, Li4Ti5O12Also have
There is apparent charge and discharge platform, platform capacity has apparent voltage jump up to 90% or more of discharge capacity at the end of charge and discharge
Etc. characteristics.
Lithium titanate is a kind of composite oxides being made of lithium metal and low potential transition metals Ti, from the 1970s
By since being studied as superconductor, because it is intermittent always relative to the high potential of lithium piece and lower energy density
It is of interest by people, before and after 1999, people just lithium titanate with spinel structure is had conducted extensive research.It is lacked as having
Sunken spinel structure, lithium titanate provides three-dimensional diffusion channel for the migration of lithium ion, just because of Li+Insertion and deintercalation
Almost the structure of material is not influenced, lithium titanate battery usually has excellent cycle performance, discharging voltage balance, intercalation potential
It is high and be not easy to cause analysis lithium, it can be used in the stable region of most liquid electrolyte, lithium titanate is commonly referred to as zero and answers
Become material, lithium titanate is used as cathode not will form SEI film, reduce the irreversible capacity consumption of lithium ion battery, metatitanic acid
Lithium has the three-dimensional channel that quickly moves for lithium ion, and that potential plateau is wide, has extended cycle life, does not form SEI etc. is excellent
Electrochemical properties are ideal active materials.But the electron electric conductivity of lithium titanate is poor, polarizes in electrochemical reaction process
Seriously, and big calorimetric is generated, to electrode using unfavorable, therefore, the control to lithium titanate material size distribution and is mixed at carbon coating
Miscellaneous, metal cation doping seems and is even more important.
Summary of the invention
The purpose of the present invention is being directed to disadvantages mentioned above existing in the prior art, a kind of metatitanic acid of granularity integrated distribution is provided
The preparation method of lithium composite material, the composite material size distribution centralization that the method for the present invention is prepared, and can overcome
Lithium titanate material conductivity and the low disadvantage of ionic diffusion coefficient, to improve the circulation and high rate performance of material.
To achieve the above object, technical solution of the present invention is as follows:
A kind of preparation method of the lithium titanate composite material of granularity integrated distribution, step include:
(1) material solution is prepared: titanium source is dissolved in the titanium source solution that 0.1~0.5 g/ml is formulated as in dehydrated alcohol,
Aluminium isopropoxide is dissolved in the metal ion solution for obtaining 0.01~0.1g/ml in dehydrated alcohol, Lithium acetate dihydrate is dissolved in volume
The lithium source solution that 0.05~0.2 g/ml is obtained in dehydrated alcohol and water than 3:10, by chelating agent it is soluble in water 0.1~0.6
The chelating agent solution of g/ml, it is spare；
(2) size distribution control process: titanium source solution, metal ion solution, lithium source solution and chelating agent solution are stirring
It mixes down and is successively added drop-wise in reactor, 15~35 DEG C of 2~10h of reaction obtain leucosol, then water-bath gradient adds under stiring
5~20h of heat, forms the gelation presoma of semisolid；
(3) granularity centralization process: by the gelation presoma drying of step (2), it is broken for powder, is then sintered, breaks
Broken, screening obtains the presoma modifier that granularity is 200~300 mesh；
(4) carbon coating: the side that the presoma modifier and carbon source 10~5:1 in mass ratio of step (3) preparation pass through ball milling
Formula mixes, 700~800 DEG C of 10~20h of sintering in nitrogen atmosphere, is crushed, screening, obtains the metatitanic acid lithium composite of granularity integrated distribution
Material.
In step (1), the titanium source is the combination of one or both of butyl titanate and isopropyl titanate；
In step (1), the lithium source is the combination of one or both of Lithium acetate dihydrate and lithium hydroxide；
In step (1), the chelating agent is one of citric acid, oxalic acid and acetic acid or a variety of.
In step (2), the titanium source solution, metal ion solution, lithium source solution and chelating agent solution, titanium atom, gold
Belong to ion, lithium ion, chelator molecule molar ratio be 1:0.01~0.1:0.8~0.9:0~0.4；
In step (2), the dropwise addition, rate is 30~120 drops/min；
In step (2), the water-bath gradient-heated, temperature gradient is respectively 40~55 DEG C of heating 1~10h, 55~70
DEG C 1~5h of heating, 70~80 DEG C be heated to the volatilization of second alcohol and water completely, each temperature gradient correspond to speed of agitator be followed successively by 200~
400r/min, 400~600r/min, 600~700r/min.
In step (3), the sintering, preferably in oxygen atmosphere 400~600 DEG C 2~10h of processing；
In step (3), described is broken, and preferably ball milling or sand milling is broken.
In step (4), the carbon source is one of glucose, PEG and sucrose or a variety of.
Technical solution of the present invention has the beneficial effect that
Preparation method of the present invention can mix the metal ion of doping and titanium source and lithium source on atomic level.It is solidifying
Gelatinization process adjusts revolving speed and temperature by gradient, guarantees the controllability of size distribution, while Doped ions are realized most
Whole uniform and consistency, improves the ionic diffusion coefficient of lithium titanate.In granularity centralization process, presoma is compared with low temperature first
It is pre-sintered under degree, mitigates high temperature and reunite, size distribution is become narrower by broken, screening, guarantees the high consistency of subsequent product.
It is final to realize the lithium titanate composite material that granularity integrated distribution is prepared, overcome lithium titanate material conductivity and ion to spread system
The low disadvantage of number, improves the circulation and high rate performance of material.
Detailed description of the invention
Fig. 1 is the particle size distribution figure of lithium titanate composite material made from embodiment 1；
Fig. 2 is 1C discharge capacity-cycle-index performance chart of lithium titanate composite material made from embodiment 1；
Fig. 3 is the high rate performance curve graph of lithium titanate composite material made from embodiment 2；
Fig. 4 is the electron microscope of lithium titanate composite material made from embodiment 3；
Fig. 5 is 1C discharge capacity-cycle-index performance chart of lithium titanate composite material made from comparative example 1.
Specific embodiment
The present invention is further described combined with specific embodiments below, without departing from the idea case in the present invention described above,
The various replacements or change made according to ordinary skill knowledge and customary means, are included within the scope of the present invention.
Embodiment 1
A kind of preparation method of the lithium titanate composite material of granularity integrated distribution, step include:
(1) material solution is prepared:
The pure butyl titanate of 20g analysis, which is dissolved in 20ml ethanol solution, obtains titanium source solution；
0.06g aluminium isopropoxide is dissolved in 5ml ethanol solution and obtains metal ion solution；
4.8918g Lithium acetate dihydrate, which is dissolved in 6ml water and 20ml dehydrated alcohol mixed solution, obtains lithium source solution；
4g citric acid, which is dissolved in 10ml dehydrated alcohol, obtains chelating agent solution.
(2) size distribution control process: titanium source solution, metal ion solution, lithium source solution, chelating agent solution are being stirred
In the case where successively instilled in reactor by constant pressure funnel, drop rate is that 60 drops/min is obtained then in 25 DEG C of reaction 5h
Leucosol, then leucosol is successively through revolving speed 300r/min temperature 50 C heating water bath 3h, revolving speed 500r/min temperature 60
DEG C heating water bath 2h, 80 DEG C of heating water baths of revolving speed 600r/min temperature to ethyl alcohol and water base volatilization completely, form semisolid
Gelation presoma；
(3) granularity centralization process: by the gelation presoma of step (2) after dry, grinding, 600 DEG C in oxygen atmosphere
It is sintered 3h, product ball mill crushing after sintering, the sieving of 300 mesh screens obtains presoma modifier；
(4) carbon coating: the presoma modifier of step (3) preparation is mixed by way of ball milling with 0.56g glucose, nitrogen
Atmosphere enclose in 750 DEG C of sintering 12h, obtain the lithium titanate composite material of granularity integrated distribution, size distribution is as shown in Figure 1.
Properties of product detection: Fig. 2 is 1C discharge capacity-cycle-index performance chart, 1000 weeks circulation volume conservation rates
95% or so.
Embodiment 2
A kind of preparation method of the lithium titanate composite material of granularity integrated distribution, step include:
(1) material solution is prepared:
The pure butyl titanate of 20g analysis, which is dissolved in 40ml ethanol solution, obtains titanium source solution；
0.02g aluminium isopropoxide is dissolved in 5ml ethanol solution and obtains metal ion solution；
4.8918g Lithium acetate dihydrate, which is dissolved in 6ml water and 20ml ethyl alcohol, obtains lithium source solution；
6g citric acid, which is dissolved in 10ml dehydrated alcohol, obtains chelating agent solution.
(2) size distribution control process: titanium source solution, metal ion solution, lithium source solution, chelating agent solution are being stirred
In the case where using constant pressure funnel sequence instill reactor in, drop rate be 100 drops/min obtained then in 35 DEG C of reaction 3h
To leucosol, then leucosol is successively through revolving speed 300r/min temperature 50 C heating water bath 3h, revolving speed 500r/min temperature
80 DEG C of heating water baths of 60 DEG C of heating water bath 2h, revolving speed 600r/min temperature are complete to ethyl alcohol and water base volatilization, form semisolid
Gelation presoma；
(3) granularity centralization process: by the gelation presoma of step (2) after dry, grinding, 600 DEG C in oxygen atmosphere
It is sintered 4h, product ball mill crushing after sintering, the sieving of 300 mesh screens obtains presoma modifier.
(4) carbon coating: step (3) preparation presoma modifier with modify after presoma and 0.75g glucose pass through
The mode of ball milling mixes, and 800 DEG C of sintering 10h, obtain the lithium titanate composite material of granularity integrated distribution in nitrogen atmosphere.
Properties of product detection: Fig. 3 is high rate performance curve graph, charge-discharge magnification 10C gram volume 160mAh/g.
Embodiment 3
A kind of preparation method of the lithium titanate composite material of granularity integrated distribution, step include:
(1) material solution is prepared:
16.7g isopropyl titanate, which is dissolved in 20ml ethanol solution, obtains titanium source solution；
0.05g aluminium isopropoxide is dissolved in 5ml ethanol solution and obtains metal ion solution；
2.012g lithium hydroxide, which is dissolved in 6ml water and 20ml ethyl alcohol, obtains lithium source solution；
3g acetic acid acid, which is dissolved in 5ml dehydrated alcohol, obtains chelating agent solution.
(2) size distribution control process: titanium source solution, metal ion solution, lithium source solution, chelating agent solution are being stirred
In the case where instilled in reactor using constant pressure funnel sequence, drop rate is respectively 60 drops/min, then in 35 DEG C of reaction 3h,
Leucosol is obtained, then leucosol is successively through revolving speed 300r/min temperature 50 C heating water bath 4h, revolving speed 500r/min temperature
60 DEG C of heating water bath 3h are spent, 80 DEG C of heating water baths of revolving speed 600r/min temperature to ethyl alcohol and water base volatilization completely, it is solid to form half
The gelation presoma of state；
(3) granularity centralization process: by the gelation presoma of step (2) after dry, grinding, 600 DEG C in oxygen atmosphere
It is sintered 4h, product ball mill crushing after sintering, the sieving of 300 mesh screens obtains presoma modifier.
(4) carbon coating: step (3) preparation presoma modifier with modify after presoma and 0.75g glucose pass through
The mode of ball milling mixes, 800 DEG C of sintering 10h in nitrogen atmosphere, obtains the lithium titanate composite material of granularity integrated distribution, structure is as schemed
Shown in 4.
Properties of product detection: the visible lithium titanate composite material granularity of the present invention of electron microscope analysis is smaller and distribution is concentrated.
Comparative example 1:
(1) material solution is prepared:
The pure butyl titanate of 20g analysis, which is dissolved in 20ml ethanol solution, obtains titanium source solution；
4.8918g Lithium acetate dihydrate, which is dissolved in 6ml water and 20ml dehydrated alcohol mixed solution, obtains lithium source solution；
4g citric acid, which is dissolved in 10ml dehydrated alcohol, obtains chelating agent solution.
(2) reaction process: in the case of stirring by titanium source solution, metal ion solution, lithium source solution, chelating agent solution
It is successively instilled in reactor by constant pressure funnel, drop rate is respectively 60 drops/min, then in 25 DEG C of reaction 5h, obtains white
Colloidal sol, then leucosol passes through, and 80 DEG C of heating water baths of revolving speed 500r/min temperature to ethyl alcohol and water base volatilization completely, form half
Solid gelation presoma；
(3) sintering process: by the gelation presoma of step (2) after dry, grinding, 800 DEG C of sintering in oxygen atmosphere
10h。
(4) carbon coating: the product of step (3) preparation is mixed by way of ball milling with 0.56g glucose, in nitrogen atmosphere
750 DEG C of sintering 12h, obtain lithium titanate composite material.
Properties of product detection: charge-discharge magnification 10C gram volume 146mAh/g1C discharge capacity-cycle-index performance curve
Figure.
By comparing it is found that the present invention and existing method ratio, lithium titanate composite material high rate performance obtained is more excellent, favorably
In quick charge and discharge.
Claims (9)
1. a kind of preparation method of the lithium titanate composite material of granularity integrated distribution, which is characterized in that step includes:
(1) material solution is prepared: titanium source being dissolved in the titanium source solution that 0.1~0.5g/ml is formulated as in dehydrated alcohol, by isopropyl
Aluminium alcoholates is dissolved in the metal ion solution that 0.01~0.1g/ml is obtained in dehydrated alcohol, and Lithium acetate dihydrate is dissolved in volume ratio 3:
The lithium source solution that 0.05~0.2g/ml is obtained in 10 dehydrated alcohol and water, by chelating agent it is soluble in water 0.1~0.6
The chelating agent solution of g/ml, it is spare；
(2) size distribution control process: by titanium source solution, metal ion solution, lithium source solution and chelating agent solution, under stiring
It is successively added drop-wise in reactor, 15~35 °C of 2~10h of reaction obtain leucosol, then water-bath gradient adds under stiring
5~20h of heat, forms the gelation presoma of semisolid；
(3) granularity centralization process: by the gelation presoma drying of step (2), it is broken for powder, is then sintered, is crushed, sieve
Point, obtain the presoma modifier that granularity is 200~300 mesh；
(4) carbon coating: the presoma modifier and carbon source 10~5:1 in mass ratio of step (3) preparation are mixed by way of ball milling
It closes, 700~800 °C of 10~20h of sintering in nitrogen atmosphere, is crushed, screening, obtains the metatitanic acid lithium composite of granularity integrated distribution
Material；
In step (2), temperature gradient is respectively 40~55 °C of 1~10h of heating, 55~70 °C of 1~5h of heating, 70~80 °C of heating
To second alcohol and water volatilization completely, each temperature gradient correspond to speed of agitator be followed successively by 200~400r/min, 400~600r/min,
600~700r/min.
2. preparation method according to claim 1, it is characterised in that: in step (1), the titanium source be butyl titanate and
The combination of one or both of isopropyl titanate.
3. preparation method according to claim 1, it is characterised in that: in step (1), the lithium source is Lithium acetate dihydrate
With the combination of one or both of lithium hydroxide.
4. preparation method according to claim 1, it is characterised in that: in step (1), the chelating agent be citric acid,
One of oxalic acid and acetic acid are a variety of.
5. preparation method according to claim 1, it is characterised in that: in step (2), the titanium source solution, metal from
Sub- solution, lithium source solution and chelating agent solution, titanium atom, metal ion, lithium ion, chelator molecule molar ratio be 1:
0.01~0.1:0.8~0.9:0~0.4.
6. preparation method according to claim 1, it is characterised in that: in step (2), the dropwise addition, rate be 30~
120 drops/min.
7. preparation method according to claim 1, it is characterised in that: in step (3), described is sintered in oxygen atmosphere
In 400~600 °C of 2~10h of processing.
8. preparation method according to claim 1, it is characterised in that: in step (3), described is broken for ball milling or sand milling
It is broken.
9. preparation method according to claim 1, it is characterised in that: in step (4), the carbon source be glucose,
One of PEG and sucrose or a variety of.
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