CN108054372A - A kind of dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative materials and preparation method thereof - Google Patents
A kind of dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative materials and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to ion cathode material lithium technical fields, disclose a kind of dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative materials and preparation method thereof.The present invention is with absolute ethyl alcohol, two water of zinc acetate, ethanolamine, glucose etc. for raw material, strictly control time and the temperature of its hydro-thermal reaction, so as to which dried persimmon shape nucleocapsid C/ZnO materials are made, the dried persimmon shape nucleocapsid C/ZnO of this special appearance greatly improves the electric conductivity and stability of existing ZnO negative materials, so as to significantly improve its chemical property.On the one hand stress variation caused by volume change in charge and discharge process can be reduced, the pattern of another aspect dried persimmon shape increases specific surface area, effectively improves the cycle performance of lithium ion battery.In addition, the presence of carbon improves the electric conductivity of ZnO negative materials.
Description
Technical field
The present invention relates to ion cathode material lithium technical field, more particularly, to a kind of dried persimmon shape nucleocapsid C/ZnO
Lithium ion battery negative material and preparation method thereof.
Background technology
The energy and material are support mankind nowadays civilization and ensure the most important material base of social development.Lithium ion battery
Due to high, the memory-less effect higher than energy with operating voltage, the distinguishing features such as environmentally safe and be widely used, such as
The fields such as the ideal source of the electronic devices miniaturization such as portable instrument, electric vehicle, mobile phone.Excite a large amount of scientific research people
Research and exploration of the member to ion cathode material lithium, at present the theoretical specific capacity of graphite material there was only 375mAh/g, gradually cannot
Meet application requirement of mankind's today's society to battery.
The negative material of lithium ion battery realizes the embedding of lithium ion primarily as the main body of storage lithium in charge and discharge process
Enter and deintercalation.From the point of view of the development of lithium ion, the research of negative material plays decisive role to the appearance of lithium ion battery.Often
The lithium ion battery negative material seen, such as graphite cathode material, titanium system negative material, but graphite cathode material is due to its current potential
With the current potential of metal lithium electrode very close to so when battery iterative cycles and when overcharging, the easy precipitating metal lithium of graphite surface can be because
Formed dendrite and it is short-circuit, be also easy to cause thermal runaway when the temperature is excessively high.Titanium system negative material electric conductivity is very poor, and compared with
The current potential of lithium metal is higher and measures the characteristics of relatively low.For oxide cathode material, such as SnO2, MoS2 and transiting metal oxidation
Object, in these materials, transition metal oxide is expected to become next-generation high-performance due to possessing high power capacity and high safety performance
Lithium ion battery negative material.
Theoretical capacity when zinc oxide (ZnO) is as lithium ion battery negative material is up to 978 mAh/g.It is but block
When ZnO is used as lithium ion battery negative material, electron conductivity is low, and volume change is big in charge and discharge process, and electrical contact loss is big,
Compared with other transition metal oxides, chemical property is poor.There are many research work at present by carrying out nanometer to ZnO
Change, solve the intrinsic defect that the structure of ZnO itself is brought to a certain extent.ZnO is prepared into a series of with nano junction
The composite material of structure, such as zero dimension ZnO nano-structure, one-dimensional nano structure, two-dimentional ZnO nano-structure, multidimensional ZnO nano-structure with
And it is rodlike, spherical etc., although changing the intrinsic appearance structures of ZnO, electrical-contact area can be increased, improve lithium ion battery
Cycle performance.But the lithium ion insert the distance of bulk ZnO micron particles is longer, it is relatively low to the storage capacity of lithium ion, initially
Discharge capacity is relatively low.ZnO nano-structure is in cycling several times, and discharge capacity is decreased obviously, and reversible capacity is low.Therefore, obtain
Reversible capacity, good circulation performance and the excellent high rate performance high with ZnO electrode material is kept is still a very big challenge.
The content of the invention
The technical problem to be solved by the present invention is to overcome Zn and the low electron conduction of ZnO material itself and slow lithium ion
Diffusion rate reduces the cycle performance and high rate performance of material；In addition, the formation of LiZn alloys brings the notable change of volume
Change, cause the cycle performance of crushing and the electrical isolation of active material, battery capacity sharp-decay and difference.A kind of specific capacity is provided
Height, good cycle, efficiency for charge-discharge be high and the dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative material systems of stable structure
Preparation Method.
The present invention, for raw material, using simple hydro-thermal method, is obtained with absolute ethyl alcohol, two water of zinc acetate, ethanolamine, glucose etc.
Obtained the lithium ion battery negative material with high reversible capacity, good cycle performance and high rate performance.
The purpose of the present invention is achieved through the following technical solutions：
A kind of dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative material preparation methods are provided, are comprised the following steps：
S1. solid carbon ball is prepared；
S2. zinc acetate is completely dissolved in organic solvent, then sequentially adds ethanolamine, wherein solid carbon ball, zinc acetate：Second
Hydramine：The mass ratio of solid carbon ball is 1~3:2.04~4.08：0.6~0.9, it is transferred to after stirring evenly in reaction kettle,
Hydro-thermal reaction is carried out at 150~180 DEG C, the reaction time is 2~6h, is centrifuged after having reacted and obtains black product, and dry；
S3. by dried product first with 600~800 DEG C calcining, calcination time be 2~6h, obtain black product, then again with
400~600 DEG C of calcinings, calcination time are 2~6h, the final dried persimmon shape nucleocapsid C/ZnO lithium-ion electrics for obtaining white product
Pond negative material.
The principle of the present invention is, the fixation of the additive amount of solid carbon ball and ZnO is proportional, strictly controls its hydro-thermal reaction
Time and temperature, so as to which dried persimmon shape nucleocapsid C/ZnO materials, the dried persimmon shape nucleocapsid C/ of this special appearance is made
ZnO greatly improves the electric conductivity and stability of existing ZnO negative materials, so as to significantly improve its chemical property.One side
Face can reduce stress variation caused by volume change in charge and discharge process, and the pattern of another aspect dried persimmon shape increases specific surface
Product effectively improves the cycle performance of lithium ion battery.In addition, the presence of carbon improves the electric conductivity of ZnO negative materials.
Further, the present invention also provides the preparation method of the solid carbon ball, comprise the following steps：
S11. concentration is prepared as 0.04~0.133g/ml glucose solutions, then adds in and hydro-thermal reaction is carried out in reaction kettle, temperature
It spends for 120~160 DEG C, the reaction time is that for 24 hours, natural cooling after having reacted is centrifuged to pH to 7, then dried, will be dried
Product is calcined, and obtains solid carbon ball.
Further, calcining heat is 700~800 DEG C in step S11, and calcination time is 2~6h.
Preferably, organic solvent described in step S2 is ethyl alcohol.
Preferably, acetic acid zinc concentration described in step S2 is 0.02~0.1g/ml.
Preferably, the zinc acetate is completely dissolved in by ultrasound in organic solvent.
Preferably, mixing time is 6h in step S2.
The present invention also provides a kind of dried persimmon shape nucleocapsid C/ZnO lithium ion batteries being prepared using the above method to bear
Pole material, the negative material applied to lithium ion battery.
Compared with prior art, the present invention has following advantageous effect：
This dried persimmon shape structure that the present invention synthesizes increases specific surface area, effectively improves the cycle performance of lithium ion battery,
Reduce stress variation caused by volume change in charge and discharge process.The efficiency for charge-discharge of lithium ion battery is improved, can also be made
Lithium ion freely embedded and deintercalation in charge and discharge process has pole to the raising of the cycle performance and efficiency for charge-discharge of material
Big facilitation.In addition, the presence of carbon improves the electric conductivity of ZnO negative materials.
The dried persimmon shape C/ZnO that the present invention synthesizes is improved the cycle performance of lithium ion battery and initial charge/discharge appearance,
The high rate performance of lithium ion battery and high reversibility and good cycle performance are also improved simultaneously.
The dried persimmon shape nucleocapsid C/ZnO negative materials that the present invention synthesizes have specific capacity high, and good cycle is at low cost,
The advantages that pollution-free.Dried persimmon shape nucleocapsid C/ZnO cathode material preparation methods are simple for process, easy to operate simultaneously.
The dried persimmon shape nucleocapsid C/ZnO negative materials that the present invention synthesizes have the electric discharge of good electrochemical stability Xun Huan
Capacity reaches 422.39mA h/g, shows that this dried persimmon shape C/ZnO materials have high specific capacity.And by 100 times cycle after,
Its discharge capacity remains at 330.26mA h/g, shows that this dried persimmon shape C/ZnO material structures are stablized, has extended cycle life.Persimmon
Pie C/ZnO carries out cycling it for 100 times under the current density of 40mA/g that coulombic efficiency is 91.6% for the first time.This is further demonstrated that
Dried persimmon shape nucleocapsid C/ZnO negative materials have good stable charge/discharge and excellent cycle performance.
Description of the drawings
Fig. 1 is dried persimmon shape nucleocapsid C/ZnO negative material XRD diagram.
Fig. 2 is dried persimmon shape nucleocapsid C/ZnO negative material scanning electron microscope (SEM) photographs.
Fig. 3 passes through 1 time, 10 times, the charging and discharging curve of 100 times for dried persimmon shape nucleocapsid C/ZnO negative materials.
Fig. 4 be dried persimmon shape nucleocapsid C/ZnO negative materials is carried out under the current density of 40mA/g 100 times cycle follow
Ring performance map.
Specific embodiment
It is further illustrated the present invention with reference to specific embodiment.Following embodiment is only illustrative examples, not structure
Into inappropriate limitation of the present invention, the multitude of different ways that the present invention can be limited and covered by the content of the invention is implemented.It is unless special
Do not mentionlet alone bright, the present invention reagent, compound and the equipment that use is the art conventional reagent, compound and equipment.
Embodiment 1
The present embodiment provides a kind of dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative material preparation methods, including following step
Suddenly：
S1. solid carbon ball is prepared；
S2. 50ml ethyl alcohol is measured in 100ml beakers with graduated cylinder, weigh two water of 3g zinc acetates and be placed in and fill in ethyl alcohol beaker, surpass
Sound makes two water of zinc acetate fully dissolve, and measuring 4ml ethanolamines with buret adds in containing in two water of zinc acetate, ethanol solution, weighs
Solid carbon ball 0.9g stirs 6h, transfers the solution into reaction kettle in above-mentioned mixed solution, and it is anti-that hydro-thermal is carried out at 180 DEG C
Should, reaction time 6h obtains black product, dries in an oven after being centrifuged；
S3. dried product is obtained black product, will be obtained black in tube furnace with 800 DEG C of calcinings, calcination time 6h
Color product is in Muffle furnace with 600 DEG C of calcinings, calcination time 6h, the final dried persimmon shape nucleocapsid C/ for obtaining white product
ZnO lithium ion battery negative materials.
Wherein, the preparation method of solid carbon ball is as follows described in step S1：
S11. 50ml deionized waters are weighed in 100ml beakers with 100ml graduated cylinders, it is molten that the stirring of 4g glucose is added in beaker
It solves, carries out hydro-thermal reaction after stirring 1h in addition reaction kettle, temperature is 160 DEG C, and the reaction time is for 24 hours, to have reacted rear naturally cold
But, centrifuge to pH to 7, then dry, dried product is put into tube furnace and is calcined, calcining heat is 800 DEG C, is forged
The burning time is 6h, obtains solid carbon ball.
Wherein, the key of the dried persimmon shape nucleocapsid C/ZnO of special appearance is formed in the present embodiment in step S2
The additive amount of solid carbon ball and ZnO are time and temperature that be fixed proportional, and strictly controlling its hydro-thermal reaction.
The present embodiment with absolute ethyl alcohol, two water of zinc acetate, ethanolamine, glucose etc. for raw material, using simple hydro-thermal method,
Preparation method is simple, easy to operate, at low cost, pollution-free, the dried persimmon shape nucleocapsid C/ZnO negative electrode of lithium ion battery being prepared
Material, the dried persimmon shape nucleocapsid C/ZnO of this special appearance greatly improve the electric conductivity and stabilization of existing ZnO negative materials
Property, so as to significantly improve its chemical property.On the one hand stress caused by volume change in charge and discharge process can be reduced to become
Change, the pattern of another aspect dried persimmon shape increases specific surface area, effectively improves the cycle performance of lithium ion battery.In addition, carbon
Presence improve the electric conductivity of ZnO negative materials, there is high reversible capacity, good cycle performance and high rate performance.
Embodiment 2
The present embodiment provides a kind of dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative material preparation methods, including following step
Suddenly：
S1. solid carbon ball is prepared；
S2. 30ml ethyl alcohol is measured in 100ml beakers with graduated cylinder, weigh two water of 3g zinc acetates and be placed in and fill in ethyl alcohol beaker, surpass
Sound makes two water of zinc acetate fully dissolve, and measuring 2ml ethanolamines with buret adds in containing in two water of zinc acetate, ethanol solution, weighs
Solid carbon ball 0.6g stirs 6h, transfers the solution into reaction kettle in above-mentioned mixed solution, and it is anti-that hydro-thermal is carried out at 150 DEG C
Should, reaction time 2h obtains black product, dries in an oven after being centrifuged；
S3. dried product is obtained black product, will be obtained black in tube furnace with 600 DEG C of calcinings, calcination time 2h
Color product is in Muffle furnace with 400 DEG C of calcinings, calcination time 2h, the final dried persimmon shape nucleocapsid C/ for obtaining white product
ZnO lithium ion battery negative materials.
Wherein, the preparation method of solid carbon ball is as follows described in step S1：
S11. 30ml deionized waters are weighed in 100ml beakers with 100ml graduated cylinders, it is molten that the stirring of 2g glucose is added in beaker
It solves, carries out hydro-thermal reaction after stirring 1h in addition reaction kettle, temperature is 120 DEG C, and the reaction time is for 24 hours, to have reacted rear naturally cold
But, centrifuge to pH to 7, then dry, dried product is put into tube furnace and is calcined, calcining heat is 700 DEG C, is forged
The burning time is 2h, obtains solid carbon ball.
Embodiment 3
The present embodiment provides a kind of dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative material preparation methods, including following step
Suddenly：
S1. solid carbon ball is prepared；
S2. 40ml ethyl alcohol is measured in 100ml beakers with graduated cylinder, weigh two water of 2g zinc acetates and be placed in and fill in ethyl alcohol beaker, surpass
Sound makes two water of zinc acetate fully dissolve, and measuring 3ml ethanolamines with buret adds in containing in two water of zinc acetate, ethanol solution, weighs
Solid carbon ball 0.7g stirs 6h, transfers the solution into reaction kettle in above-mentioned mixed solution, and it is anti-that hydro-thermal is carried out at 160 DEG C
Should, reaction time 3h obtains black product, dries in an oven after being centrifuged；
S3. dried product is obtained black product, will be obtained black in tube furnace with 650 DEG C of calcinings, calcination time 3h
Color product is in Muffle furnace with 450 DEG C of calcinings, calcination time 3h, the final dried persimmon shape nucleocapsid C/ for obtaining white product
ZnO lithium ion battery negative materials.
Wherein, the preparation method of solid carbon ball is as follows described in step S1：
S11. 50ml deionized waters are weighed in 100ml beakers with 100ml graduated cylinders, it is molten that the stirring of 2g glucose is added in beaker
It solves, carries out hydro-thermal reaction after stirring 1h in addition reaction kettle, temperature is 130 DEG C, and the reaction time is for 24 hours, to have reacted rear naturally cold
But, centrifuge to pH to 7, then dry, dried product is put into tube furnace and is calcined, calcining heat is 750 DEG C, is forged
The burning time is 3h, obtains solid carbon ball.
Embodiment 4
The present embodiment provides a kind of dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative material preparation methods, including following step
Suddenly：
S1. solid carbon ball is prepared；
S2. 50ml ethyl alcohol is measured in 100ml beakers with graduated cylinder, weigh two water of 3g zinc acetates and be placed in and fill in ethyl alcohol beaker, surpass
Sound makes two water of zinc acetate fully dissolve, and measuring 3ml ethanolamines with buret adds in containing in two water of zinc acetate, ethanol solution, weighs
Solid carbon ball 0.8g stirs 6h, transfers the solution into reaction kettle in above-mentioned mixed solution, and it is anti-that hydro-thermal is carried out at 170 DEG C
Should, reaction time 5h obtains black product, dries in an oven after being centrifuged；
S3. dried product is obtained black product, will be obtained black in tube furnace with 750 DEG C of calcinings, calcination time 5h
Color product is in Muffle furnace with 550 DEG C of calcinings, calcination time 5h, the final dried persimmon shape nucleocapsid C/ for obtaining white product
ZnO lithium ion battery negative materials.
Wherein, the preparation method of solid carbon ball is as follows described in step S1：
S11. 30ml deionized waters are weighed in 100ml beakers with 100ml graduated cylinders, it is molten that the stirring of 4g glucose is added in beaker
It solves, carries out hydro-thermal reaction after stirring 1h in addition reaction kettle, temperature is 150 DEG C, and the reaction time is for 24 hours, to have reacted rear naturally cold
But, centrifuge to pH to 7, then dry, dried product is put into tube furnace and is calcined, calcining heat is 750 DEG C, is forged
The burning time is 5h, obtains solid carbon ball.
Performance and characterization
Fig. 1 is dried persimmon shape nucleocapsid C/ZnO negative material XRD diagram, as can be seen from the figure the ZnO features prepared by the present invention
Peak is almost overlapped with the peak of the standard card of ZnO, and free from admixture peak, and that this explanation is prepared is the ZnO of high-purity.
Fig. 2 is the scanning electron microscope (SEM) photograph of dried persimmon shape nucleocapsid C/ZnO negative materials, and as can be seen from the figure material is in special
Dried persimmon shape, ZnO uniform closes are coated in carbon ball, and even particle size, grain size is at 4 μm or so.This special dried persimmon shape
Topographical surface increases the contact surface area of ZnO there are stratiform fold, drastically increases the charge and discharge effect of ZnO electrode material
Rate.
Fig. 3 dried persimmon shape nucleocapsid C/ZnO negative materials pass through 1 time, 10 times, the charging and discharging curve of 100 times.It can from figure
To find out that the discharge capacity of the 1st Xun Huan of C/ZnO negative materials up to 422.39mA h/g, shows this dried persimmon shape nucleocapsid C/
ZnO negative materials have high specific capacity.And after 100 Xun Huans, discharge capacity remains at 330.26mA h/g,
Show this dried persimmon shape nucleocapsid C/ZnO negative material stable structure, have extended cycle life.
Fig. 4 dried persimmon shape nucleocapsid C/ZnO negative materials carry out the cycling of 100 Xun Huans under the current density of 40mA/g
Performance map.As can be seen from the figure first discharge specific capacity is 422.39 mA h/g, and coulombic efficiency is 91.6% for the first time.100 times
Discharge capacity reaches 330.26mA h/g after charge and discharge cycles, this further demonstrates that dried persimmon shape nucleocapsid C/ZnO negative materials
With good stable charge/discharge and excellent cycle performance.
Claims (8)
1. a kind of dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative material preparation methods, which is characterized in that including following step
Suddenly：
S1. solid carbon ball is prepared；
S2. zinc acetate is completely dissolved in organic solvent, then sequentially adds ethanolamine, wherein solid carbon ball, zinc acetate：Second
Hydramine：The mass ratio of solid carbon ball is 1~3:2.04~4.08：0.6~0.9, it is transferred to after stirring evenly in reaction kettle,
Hydro-thermal reaction is carried out at 150~180 DEG C, the reaction time is 2~6h, is centrifuged after having reacted and obtains black product, and dry；
S3. by dried product first with 600~800 DEG C calcining, calcination time be 2~6h, obtain black product, then again with
400~600 DEG C of calcinings, calcination time are 2~6h, the final dried persimmon shape nucleocapsid C/ZnO lithium-ion electrics for obtaining white product
Pond negative material.
2. dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative material preparation methods, feature exist according to claim 1
In the preparation method of solid carbon ball is as follows described in step S1：
S11. concentration is prepared as 0.04~0.133g/ml glucose solutions, then adds in and hydro-thermal reaction is carried out in reaction kettle, temperature
It spends for 120~160 DEG C, the reaction time is that for 24 hours, natural cooling after having reacted is centrifuged to pH to 7, then dried, will be dried
Product is calcined, and obtains solid carbon ball.
3. dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative material preparation methods, feature exist according to claim 2
In calcining heat is 700~800 DEG C in step S11, and calcination time is 2~6h.
4. dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative material preparation methods, feature exist according to claim 1
In organic solvent described in step S2 is ethyl alcohol.
5. dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative material preparation methods, feature exist according to claim 4
In acetic acid zinc concentration described in step S2 is 0.02~0.1g/ml.
6. dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative material preparation methods, feature exist according to claim 1
In the zinc acetate is completely dissolved in by ultrasound in organic solvent.
7. dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative material preparation methods, feature exist according to claim 1
In mixing time is 6h in step S2.
8. a kind of dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative materials, which is characterized in that by claim 1~arbitrary
What one dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative material preparation method was prepared.
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| CN107867713A (en) * | 2017-11-09 | 2018-04-03 | 扬州大学 | A kind of ZnO sensing electrode material preparation methods of porous nano pie structure |
| CN107867713B (en) * | 2017-11-09 | 2019-07-05 | 扬州大学 | A kind of ZnO sensing electrode material preparation method of porous nano pie structure |
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