CN109888245A - Titanium niobium oxygen/carbon composite and its preparation method and application that Lacking oxygen and carbon coating are adjusted - Google Patents
Titanium niobium oxygen/carbon composite and its preparation method and application that Lacking oxygen and carbon coating are adjusted Download PDFInfo
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- CN109888245A CN109888245A CN201910221605.6A CN201910221605A CN109888245A CN 109888245 A CN109888245 A CN 109888245A CN 201910221605 A CN201910221605 A CN 201910221605A CN 109888245 A CN109888245 A CN 109888245A
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Abstract
The invention discloses the titanium niobium oxygen (Ti that a kind of Lacking oxygen and carbon coating are adjusted2Nb10O29‑x)/carbon composite and its preparation method and application prepares Ti by hydro-thermal method and high temperature sintering methods2Nb10O29, Ti is obtained finally by being sintered in acetylene high temperature2Nb10O29‑x@C target product, target product have biggish specific surface area, Ti2Nb10O29‑x@C nano particle can increase the contact area of electrolyte and electrode, provide bigger more effectively active reaction area, meanwhile, electronics conduction velocity is accelerated, chemical property is improved.Ti of the present invention2Nb10O29‑x@C-material has the characteristics that high circulation service life, high-energy and power density, particularly suitable as lithium ion battery negative material, has broad application prospects in fields such as mobile communication, electric car, solar power generation and aerospaces.
Description
Technical field
The present invention relates to lithium ion battery negative material fields, and in particular to a kind of titanium niobium of Lacking oxygen and carbon coating adjusting
Oxygen/carbon composite and its preparation method and application.
Background technique
Electronic product consumption market expands rapidly so that increasing for the demand of high-performance, high stable battery material
Add.The storage lithium structure that titanium niobate lithium storage materials have had, to determine its chemical property possessed.It is currently mainly used
Negative electrode material include graphite and lithium titanate etc., but all there is a problem that serious, graphite is easy due to its low voltage platform
It forms SEI (Solid Electrolyte Interphase, solid electrolyte interface) film and causes Li dendrite, may cause quick-fried
It is fried, though and lithium titanate is higher without generating SEI film, its low theoretical capacity (175mAh g because of voltage platform-1) make energy storage
It shows not ideal enough.Compared with the negative electrode material that these are common, niobic acid titanium compound is with bigger theoretical capacity and relatively
Security and stability.But niobic acid titanium compound equally exists some disadvantages, for example its electronic conductivity is low, lithium ion diffusion coefficient
It is smaller etc..
Summary of the invention
It is an object of the invention to for the not high lower lithium titanate lithium of graphite and theoretical capacity of current security performance from
Sub- cell negative electrode material provides the titanium niobium oxygen (Ti of a kind of Lacking oxygen and carbon coating adjusting2Nb10O29-x)/carbon composite and its
Preparation method and application, the Ti2Nb10O29-xFor@C electrode material with high power density, high-energy density and high safety are steady
It is qualitative.
A kind of titanium niobium oxygen (Ti of Lacking oxygen and carbon coating adjusting2Nb10O29-xThe preparation method of)/carbon composite, including
Following steps:
1) columbium pentachloride and isopropyl titanate are dissolved in ethanol solution, are uniformly mixed to form mixed solution, added
Enter into polytetrafluoroethylene (PTFE) autoclave, seal and heat, hydrothermal temperature is 140 DEG C -220 DEG C, and the hydro-thermal time is 4-28 hours, cold
But after, sample is taken out, drying is washed, obtains intermediate product, intermediate product is sintered under the conditions of 600-900 DEG C in tube furnace
0.5-4 hours, obtain target predecessor (Ti2Nb10O29)；
2) the target predecessor (Ti for obtaining step 1)2Nb10O29) be put into tube furnace and be passed through acetylene gas 200-900
It is sintered 1-5 hours under the conditions of DEG C, obtains titanium niobium oxygen/carbon composite (i.e. Ti of Lacking oxygen and carbon coating adjusting2Nb10O29-x@C
Material).
In the present invention, by Ti2Nb10O29It is passed through acetylene gas sintering, obtains Ti2Nb10O29-x@C-material, x table in molecular formula
Show Lacking oxygen (i.e. scarce oxygen atom), is to restore oxygen atom by acetylene to be formed, x is to be randomly generated, and is not counted specifically
Value.Ti2Nb10O29-x@C-material can effectively improve electronics conduction velocity, to improve its chemical property.Ti2Nb10O29-x@C
It can be used as the lithium ion battery negative material with high-energy density, high power density and high safety stability.
In step 1), the molar ratio of the columbium pentachloride and isopropyl titanate is 3~7:1, further preferably 4~6:
1, most preferably 5:1.
Hydrothermal temperature is 160 DEG C -200 DEG C, and the hydro-thermal time is 10-24 hours,
Target predecessor is sintered 1-2 hours under the conditions of 750-850 DEG C in tube furnace,
In step 2), target predecessor (Ti that step 1) is obtained2Nb10O29) be put into tube furnace and be passed through acetylene gas
It is sintered 1.5-2.5 hours under the conditions of 300-600 DEG C.
Titanium niobium oxygen/carbon composite (i.e. Ti that the Lacking oxygen and carbon coating of preparation are adjusted2Nb10O29-x@C-material), have
Biggish specific surface area, Ti2Nb10O29-x@C nano particle can increase the contact area of electrolyte and motor, and providing more more has greatly
The active reaction area of effect, packet carbon accelerate electronics conduction velocity, and this packet carbon technique also produces Lacking oxygen, molecular formula simultaneously
Middle x indicates Lacking oxygen, improves mechanical stress, improves chemical property.
Titanium niobium oxygen/carbon composite that the Lacking oxygen and carbon coating are adjusted is particularly suitable as negative electrode of lithium ion battery
Material.The Ti2Nb10O29@C-material possesses high theoretical capacity (396mAh g-1), in 5 C (1C=396mAh g-1) electricity
Specific capacitance of discharging under current density can reach 310mAh g-1, and electric discharge specific capacitance conservation rate has up to 90% or more after 500 circulations
There are preferable electronic conductivity and higher security and stability, Ti2Nb10O29@C nano average diameter of particles is about 50nm.
The Ti2Nb10O29@C-material is as a kind of new titanium niobium oxygen/carbon composite.
Compared with prior art, the present invention has the advantage that
The method of the present invention prepares Ti by simple hydro-thermal method and high temperature sintering2Nb10O29, finally by logical acetylene high temperature
Sintering obtains Ti2Nb10O29-x@C target product.The preparation method is simple and convenient, easily controllable.
Ti prepared by the present invention2Nb10O29-x@C electrode material has biggish specific surface area, Ti2Nb10O29-x@C nano
Grain can increase the contact area of electrolyte and motor, provide bigger more effectively active reaction area, and packet carbon accelerates electronics biography
Rate is led, this packet carbon technique also produces Lacking oxygen simultaneously, improves mechanical stress, improves chemical property.In the present invention,
Formation, the kinetics disadvantage for overcoming SEI film, keep high-energy density while to realize high power discharge performance,
With formed have high power, high-energy density, high safety stability novel cathode material for lithium ion battery.
Detailed description of the invention
Fig. 1 is Ti obtained in embodiment 12Nb10O29-xThe XRD diagram of@C；
Fig. 2 is Ti obtained in embodiment 12Nb10O29-xThe scanning electron microscope (SEM) photograph of@C；
Fig. 3 is Ti obtained in embodiment 12Nb10O29-xThe transmission electron microscope picture of@C.
Specific embodiment
Below with reference to embodiment, the present invention will be described in detail, but the present invention is not limited to this.
Embodiment 1
Weigh 0.2849g C12H28O460mL dehydrated alcohol is added in Ti, stirs 10 minutes, adds 1.35g NbCl5, five
The molar ratio of niobium chloride and isopropyl titanate is 5:1, is stirred 15 minutes, until being completely dissolved.Solution is moved into after mixing poly-
In tetrafluoroethene autoclave, autoclave is sealed, the hydro-thermal reaction 24 hours under conditions of 200 DEG C.It is cooled to after reaction
25 DEG C of room temperature, solution is outwelled into taking-up sample, and after drying is washed with deionized, 25 DEG C of cooled to room temperature, obtained
Between product.Intermediate product is finally put into 800 DEG C of sintering in tube furnace and obtains target predecessor (Ti within 2 hours2Nb10O29), and lead to
Enter 300 DEG C of acetylene sintering, 2 hours gas and obtains Ti2Nb10O29-x@C target product (the i.e. titanium niobium of Lacking oxygen and carbon coating adjusting
Oxygen/carbon composite).
Fig. 1 is Ti obtained in embodiment 12Nb10O29-xThe XRD diagram of@C, TNO indicates Ti in Fig. 12Nb10O29, TNO-x@C3
Indicate Ti2Nb10O29-x@C target product；Fig. 2 is Ti obtained in embodiment 12Nb10O29-xThe scanning electron microscope (SEM) photograph of@C；Fig. 3 is real
Apply Ti obtained in example 12Nb10O29-xThe transmission electron microscope picture of@C.Ti2Nb10O29@C nano average diameter of particles is about 50nm.
Embodiment 2
Weigh 0.2849g C12H28O460mL dehydrated alcohol is added in Ti, stirs 10 minutes, adds 1.35g NbCl5, five
The molar ratio of niobium chloride and isopropyl titanate is 5:1, is stirred 15 minutes, until being completely dissolved.Solution is moved into after mixing poly-
In tetrafluoroethene autoclave, autoclave is sealed, the hydro-thermal reaction 10 hours under conditions of 160 DEG C.It is cooled to after reaction
25 DEG C of room temperature, solution is outwelled into taking-up sample, and after drying is washed with deionized, 25 DEG C of cooled to room temperature, obtained
Between product.Intermediate product is finally put into 750 DEG C of sintering in tube furnace and obtains target predecessor (Ti within 2 hours2Nb10O29), and lead to
Enter 500 DEG C of acetylene sintering, 2 hours gas and obtains Ti2Nb10O29-x@C target product (the i.e. titanium niobium of Lacking oxygen and carbon coating adjusting
Oxygen/carbon composite).
Embodiment 3
Weigh 0.2849g C12H28O460mL dehydrated alcohol is added in Ti, stirs 10 minutes, adds 1.35g NbCl5, five
The molar ratio of niobium chloride and isopropyl titanate is 5:1, is stirred 15 minutes, until being completely dissolved.Solution is moved into after mixing poly-
In tetrafluoroethene autoclave, autoclave is sealed, the hydro-thermal reaction 15 hours under conditions of 180 DEG C.It is cooled to after reaction
25 DEG C of room temperature, solution is outwelled into taking-up sample, and after drying is washed with deionized, 25 DEG C of cooled to room temperature, obtained
Between product.Intermediate product is finally put into 850 DEG C of sintering in tube furnace and obtains target predecessor (Ti within 1 hour2Nb10O29), and lead to
Enter 600 DEG C of acetylene sintering, 2 hours gas and obtains Ti2Nb10O29-x@C target product (the i.e. titanium niobium of Lacking oxygen and carbon coating adjusting
Oxygen/carbon composite).
Performance test
By Ti made of above-described embodiment 1~32Nb10O29-x@C-material is respectively as anode (by the mass ratio of 75:15:10
The negative electrode active material of experiment preparation is uniformly mixed with binder Kynoar (PVDF1300) and conductive agent acetylene black, is used
N-Methyl pyrrolidone (NMP) is diluted to suitable viscosity coated on the copper foil of LITHIUM BATTERY, is subsequently placed in vacuum oven
It is dried in vacuo 12 hours at 120 DEG C).Metal lithium sheet makees cathode, and electrolyte selects LiPF6, being dissolved in mass ratio is 1:
In the ethylene carbonate (DC) and dimethyl carbonate (DMC) of 1:1 and the mixture of ethylene carbonate (EC), LiPF6Concentration
For 1mol L-1.Button cell is assembled into glove box.Battery performance is tested respectively in blue electric tester.Charging/discharging voltage
For 1.0~2.5V, the circulation measurement Ti in 25 ± 1 DEG C of environment2Nb10O29-xThe reversible charging and discharging capacity of@C-material, charge and discharge
Cycle performance and high-rate characteristics.
The performance test results are as follows:
The Ti of embodiment 1, embodiment 2 and embodiment 32Nb10O29-x@C-material is in 5 C (1C=396mAh g-1) electric current is close
The lower electric discharge specific capacitance of degree is respectively 310mAh g-1、295mAh g-1With 299mAh g-1, and electric discharge specific capacitance is protected after 500 circulations
Holdup is up to 90% or more.As it can be seen that Ti obtained above2Nb10O29-x@C-material charge/discharge capacity is high, good cycling stability.
This is Ti prepared by the present invention2Nb10O29-x@C electrode material has biggish specific surface area, Ti2Nb10O29-x@C receives
Rice grain can increase the contact area of electrolyte and electrode.Packet carbon accelerates electronics conduction velocity, and this packet carbon technique is also simultaneously
Lacking oxygen is produced, mechanical stress is improved, improves chemical property.Therefore, Ti of the present invention2Nb10O29-x@C-material has height
Cycle life, high-energy and power density feature, in fields such as mobile communication, electric car, solar power generation and aerospaces
It has broad application prospects.
Claims (9)
1. titanium niobium oxygen/carbon composite preparation method that a kind of Lacking oxygen and carbon coating are adjusted, which is characterized in that including as follows
Step:
1) columbium pentachloride and isopropyl titanate are dissolved in ethanol solution, are uniformly mixed to form mixed solution, be added to
It in polytetrafluoroethylene (PTFE) autoclave, seals and heats, hydrothermal temperature is 140 DEG C -220 DEG C, and the hydro-thermal time is 4-28 hours, cooling
Afterwards, sample is taken out, washs drying, obtains intermediate product, intermediate product is sintered under the conditions of 600-900 DEG C in tube furnace
0.5-4 hours, obtain target predecessor；
2) the target predecessor that step 1) obtains is put into tube furnace and is passed through under the conditions of 200-900 DEG C of acetylene gas and be sintered 1-
5 hours, obtain titanium niobium oxygen/carbon composite of Lacking oxygen and carbon coating adjusting.
2. preparation method according to claim 1, which is characterized in that in step 1), the columbium pentachloride and metatitanic acid are different
The molar ratio of propyl ester is 3~7:1.
3. preparation method according to claim 2, which is characterized in that in step 1), the columbium pentachloride and metatitanic acid are different
The molar ratio of propyl ester is 4~6:1.
4. preparation method according to claim 3, which is characterized in that in step 1), the columbium pentachloride and metatitanic acid are different
The molar ratio of propyl ester is 5:1.
5. preparation method according to claim 1, which is characterized in that in step 1), hydrothermal temperature is 160 DEG C -200 DEG C,
The hydro-thermal time is 10-24 hours.
6. preparation method according to claim 1, which is characterized in that in step 1), by target predecessor in tube furnace
It is sintered 1-2 hours under the conditions of 750-850 DEG C.
7. preparation method according to claim 1, which is characterized in that in step 2), target forerunner that step 1) is obtained
Object is sintered 1.5-2.5 hours under the conditions of being put into tube furnace and being passed through 300-600 DEG C of acetylene gas.
8. titanium niobium oxygen/carbon that the Lacking oxygen of described in any item preparation method preparations and carbon coating are adjusted according to claim 1~7
Composite material.
9. titanium niobium oxygen/carbon composite that Lacking oxygen according to claim 8 and carbon coating are adjusted is as lithium ion battery
The application of negative electrode material.
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Cited By (10)
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|---|---|---|---|---|
| CN111403718A (en) * | 2020-03-31 | 2020-07-10 | 浙江大学 | Titanium niobium oxide/vertical graphene/titanium carbide-carbon composite material and preparation method and application thereof |
| CN111646510A (en) * | 2020-05-27 | 2020-09-11 | 武汉工程大学 | High-rate titanium niobium oxide microsphere and preparation method and application thereof |
| CN111653764A (en) * | 2020-05-27 | 2020-09-11 | 武汉工程大学 | Nano-silver composite niobium titanium oxide electrode material and preparation method and application thereof |
| CN112551583A (en) * | 2020-12-10 | 2021-03-26 | 哈尔滨工业大学 | Preparation method and application of carbon-coated oxygen-less titanium niobate negative electrode material |
| CN112635768A (en) * | 2020-12-18 | 2021-04-09 | 湖北工业大学 | Polyaniline-coated Ti applied to negative electrode of lithium battery2Nb10O29Preparation method of composite microsphere 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 |
| CN113036135A (en) * | 2021-02-26 | 2021-06-25 | 昆山宝创新能源科技有限公司 | Composite negative electrode material, preparation method thereof, pole piece, battery and device |
| CN114300671A (en) * | 2021-12-28 | 2022-04-08 | 蜂巢能源科技股份有限公司 | Graphite composite negative electrode material and preparation method and application thereof |
| 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 |
| CN115478341A (en) * | 2022-09-15 | 2022-12-16 | 江西赣锋锂电科技股份有限公司 | Preparation method of lithium ion negative electrode composite material |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111403718A (en) * | 2020-03-31 | 2020-07-10 | 浙江大学 | Titanium niobium oxide/vertical graphene/titanium carbide-carbon composite material and preparation method and application thereof |
| CN111646510A (en) * | 2020-05-27 | 2020-09-11 | 武汉工程大学 | High-rate titanium niobium oxide microsphere and preparation method and application thereof |
| CN111653764A (en) * | 2020-05-27 | 2020-09-11 | 武汉工程大学 | Nano-silver composite niobium titanium oxide electrode material and preparation method and application thereof |
| CN112551583A (en) * | 2020-12-10 | 2021-03-26 | 哈尔滨工业大学 | Preparation method and application of carbon-coated oxygen-less titanium niobate negative electrode material |
| CN112635768A (en) * | 2020-12-18 | 2021-04-09 | 湖北工业大学 | Polyaniline-coated Ti applied to negative electrode of lithium battery2Nb10O29Preparation method of composite microsphere 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 |
| CN113036135A (en) * | 2021-02-26 | 2021-06-25 | 昆山宝创新能源科技有限公司 | Composite negative electrode material, preparation method thereof, pole piece, battery and device |
| CN114300671A (en) * | 2021-12-28 | 2022-04-08 | 蜂巢能源科技股份有限公司 | Graphite composite negative electrode material and preparation method and application thereof |
| CN114300671B (en) * | 2021-12-28 | 2024-04-12 | 蜂巢能源科技股份有限公司 | Graphite composite negative electrode material and preparation method and application thereof |
| 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 |
| CN115478341A (en) * | 2022-09-15 | 2022-12-16 | 江西赣锋锂电科技股份有限公司 | Preparation method of lithium ion negative electrode composite material |
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