CN107331836A - The carbon nanosheet network structure load germanic acid ferrum nano material of three-dimensional communication and preparation and application - Google Patents
The carbon nanosheet network structure load germanic acid ferrum nano material of three-dimensional communication and preparation and application Download PDFInfo
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- CN107331836A CN107331836A CN201710432552.3A CN201710432552A CN107331836A CN 107331836 A CN107331836 A CN 107331836A CN 201710432552 A CN201710432552 A CN 201710432552A CN 107331836 A CN107331836 A CN 107331836A
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Abstract
The present invention provides a kind of carbon nanosheet network structure load germanic acid ferrum nano material of three-dimensional communication, it is characterized in that, the material is the germanic acid iron nano dot uniform load of uniform particle diameter on the ultra-thin carbon nanosheet of three-dimensional communication, wherein germanic acid iron nano-particle particle diameter is in 5 10nm, the carbon nanosheet thickness of three-dimensional communication is that the mass percent of germanic acid iron and total carbon in 3 10nm, the material is：(0.4‑0.7):(0.6‑0.3).Present invention simultaneously provides the preparation method of such a material and application.
Description
Technical field
The present invention relates to a kind of three-dimensional communication carbon nanosheet network structure load ultra-fine germanic acid ferrum nano material and prepare with
Using belonging to electrode material of secondary lithium ion battery field.
Background technology
As a kind of secondary energy storage device of green non-pollution, lithium ion battery has obtained increasing concern.With biography
The nickel-cadmium cell of system is compared, and it has power density big, and service life is long, the features such as safe.Mobile phone, notebook at this stage
The power supply of the mobile devices such as computer, video camera uses lithium ion battery mostly.With electric automobile (EV), intelligent grid and just
The generation that wearable device of formula etc. requires the device of higher energy is taken, the technology to lithium ion battery generates higher want again
Ask.
It is mainly at present graphite using wider carbon negative pole material in lithium ion battery, its theoretical capacity is only 372mA h/
G, low capacity is difficult to the demand for meeting high power and energy density equipment, so, exploitation have high discharge voltage, high power capacity and
The new type lithium ion battery in longer life-span is the significant challenge faced at present.Recently, germanium bimetallic oxide
(AGeO3Or A2GeO4, A is transition metal) due to its unique storage lithium mechanism and high theoretical specific capacity (>1000mA h/
G) it is considered as a kind of electrode material of the commercial graphite cathode of preferable replacement.After embedding lithium for the first time, germanium bimetallic oxygen
Compound can resolve into the matrix that germanium and lithia and the second phase metal A are collectively constituted, and on the one hand this matrix can be well
Alleviate the volumetric expansion of germanium in charge and discharge process, on the other hand scattered the second phase metal in the base can improve leading for matrix
Electrically, and then superior chemical property is realized.But it is real to appoint its extensive use so in the presence of some challenges, including discharge and recharge
Larger volumetric expansion and poor electric conductivity as common metal oxides in journey.For the two problems, adopt at this stage
The measure taken be mainly nanosizing processing (ACS Appl.Mater.Interfaces 2015,7,24932-24943) and and
The carbon material of good conductivity is carried out compound (Nanoscale, 2014,6,924-930).The particle of nanosizing is in charge and discharge process
Can occur less Volume Changes, while ion transmission path can be reduced, the introducing of carbon material can not only improve electric conductivity
And can effectively alleviate mechanical stress that Volume Changes bring and then improve the electric property of material.Germanic acid iron is used as a kind of germanium
Base transition metal oxide, it has high theoretical specific capacity (1119mA h/g) (Nano Energy, 2014,7,63-71),
Low cost and the features such as green non-pollution, is a kind of potential negative material of tool, but it also faces low electric conductivity and body
The problem of product expansion.Therefore, the germanic acid iron for preparing a kind of Nano grade simultaneously carries out it and carbon compound to be to improve its performance
Effective means.
At this stage, the method for preparing the germanium bimetallic oxide of nanosizing and being combined itself and carbon material is main
Including methods such as hydro-thermal method, added graphite alkene and pyrolysismethods.There is certain peace in traditional hydro-thermal method complex process, preparation process
Full hidden danger, the cost of added graphite alkene method is of a relatively high, is unfavorable for large-scale production.Pyrolysismethod is relative to both approaches, tool
Have with low cost, technique is simple, safety coefficient is high and the advantages of being adapted to volume production.
The content of the invention
The purpose of the present invention is to improve existing pyrolysismethod there is provided a kind of load of three-dimensional communication carbon nanosheet network structure to surpass
Thin germanic acid ferrum nano material and preparation and application.The present invention utilizes improved template pyrolysismethod, by traditional pyrolysismethod
On the basis of add sodium chloride template and realize the nanosizing of particle simultaneously and compound with carbon material, the carbon for preparing three-dimensional communication is received
Rice piece, and have ultra-fine germanic acid iron nano-particle in the surface uniform load of carbon nanosheet, this composite construction is applied to
Lithium ion battery negative material can realize excellent performance, and its preparation method process is simple, can volume production, the material as lithium from
Sub- cell negative electrode material has excellent charge-discharge performance, high rate performance and stability, is a kind of potential material of tool.
Technical scheme realized by following steps,
The carbon nanosheet network structure load germanic acid ferrum nano material of a kind of three-dimensional communication, it is characterised in that the material is
The germanic acid iron nano dot uniform load of uniform particle diameter on the ultra-thin carbon nanosheet of three-dimensional communication, wherein germanic acid iron nano-particle grain
Footpath is in 5-10nm, and the carbon nanosheet thickness of three-dimensional communication is the mass percent of germanic acid iron and total carbon in 3-10nm, the material
For：(0.4-0.7):(0.6-0.3).
The three-dimensional communication carbon nanosheet network structure of said structure loads the preparation method of ultra-fine germanic acid ferrum nano material, its
It is characterised by comprising the following steps：
(1) is mixed into carbon source with the one or more in sucrose, glucose, citric acid, ammonium citrate, using germanium oxide as
Ge source, frerrous chloride is source of iron, using the germanium and iron mol ratio in the carbon in carbon source and ge source, source of iron as (50~10):1:2, with
The mass ratio of germanium and sodium chloride in ge source is (0.01-0.1):1 meter, deionization is added by carbon source, ge source, source of iron and sodium chloride
Dissolved in water, stir wiring solution-forming and with hydrochloric acid conditioning solution PH to 2~3, freezed after solution is homogeneous and obtain presoma, then very
Sky is dried, and obtains mixture；
(2) mixture grind into powder made from step (1) is placed in constant-temperature tubular stove and calcined by：With N2, He or
Ar one kind is mixed as inert gas source, first inert gas is passed through by 200~400ml/min of flow 30-60 minutes with
Exclude air；Again using Ar as carrier gas, carrier gas flux is fixed as 50~200ml/min, with 1~10 DEG C/min programming rate
Tube furnace heat up to 500~650 DEG C, insulation 2-6h is carbonized, and reaction is cooled to room temperature after terminating, and obtains calcined product；
(3) calcined product made from collection steps (2), finely ground, is washed to untill not having NaCl in calcined product, in temperature
Spend to dry at 80~100 DEG C, obtain three-dimensional communication carbon nanosheet network structure and load ultra-fine germanic acid ferrum nano material.
The three-dimensional communication carbon nanosheet network structure loads ultra-fine germanic acid ferrum nano material and is applied to negative electrode of lithium ion battery.
The present invention has advantages below：The present invention prepares dimension connection carbon nanosheet network structure load using simple technique
Ultra-fine germanic acid ferrum nano material, with low cost, safe preparation process is high, green non-pollution.This method is realized and received simultaneously
Riceization and compound with carbon, preferably, and particle size is limited in below 5nm to germanic acid iron nano-particle dispersiveness, and carbon plate has good
Good electric conductivity and stability.The material structure is homogeneous simultaneously, and pattern is excellent, excellent performance, for negative electrode of lithium ion battery tool
There are very high specific capacity and fabulous cycle performance and high rate performance.50 times are circulated under 400mA/g current density to remain to protect
1200mAh/g specific capacity is held, and still keeps under 6.4A/g high current density 650mAh/g specific capacity.
Brief description of the drawings
Fig. 1 is that the three-dimensional communication carbon nanosheet network structure that the embodiment of the present invention 1 is obtained loads ultra-fine germanic acid iron nanometer material
The SEM photograph of material.From this view it is apparent that three-dimensional communication carbon nanosheet network structure pattern.
Fig. 2 is that the three-dimensional communication carbon nanosheet network structure that the embodiment of the present invention 1 is obtained loads ultra-fine germanic acid iron nanometer material
The SEM photograph of material.From this view it is apparent that the ultra-fine germanic acid iron nano-particle loaded on three-dimensional communication carbon nanosheet surface.
Fig. 3 is that the three-dimensional communication carbon nanosheet network structure that the embodiment of the present invention 1 is obtained loads ultra-fine germanic acid iron nanometer material
The TEM photos of material.From this view it is apparent that three-dimensional communication carbon nanosheet network structure.
Fig. 4 is that the three-dimensional communication carbon nanosheet network structure that the embodiment of the present invention 1 is obtained loads ultra-fine germanic acid iron nanometer material
The TEM photos of material.From this view it is apparent that germanic acid iron nano-particle particle diameter distribution is uniform.
Fig. 5 is that the three-dimensional communication carbon nanosheet network structure that the embodiment of the present invention 1 is obtained loads ultra-fine germanic acid iron nanometer material
The HRTEM photos of carbon nanosheet in material.From this view it is apparent that carbon nanosheet thickness.
Fig. 6 is that the three-dimensional communication carbon nanosheet network structure that the embodiment of the present invention 1 is obtained loads ultra-fine germanic acid iron nanometer material
The HRTEM photos of material.From this view it is apparent that the size of germanic acid iron nano-particle is in 5nm or so.
Fig. 7 is that the three-dimensional communication carbon nanosheet network structure that the embodiment of the present invention 1 is obtained loads ultra-fine germanic acid iron nanometer material
The XRD spectrum of material.
Fig. 8 is that the ultra-fine germanic acid iron of three-dimensional communication carbon nanosheet network structure load obtained using the embodiment of the present invention 1 is received
In the charge-discharge performance figure of negative electrode of lithium ion battery, figure made from rice material：- ■-it is charging curve ,-●-it is to put
Electric curve.
Fig. 9 is that the ultra-fine germanic acid iron of three-dimensional communication carbon nanosheet network structure load obtained using the embodiment of the present invention 1 is received
In the charge-discharge magnification performance map of negative electrode of lithium ion battery, figure made from rice material：- ■-it is charging curve ,-●-it is to put
Electric curve.
Embodiment
The particular content of the present invention is described as follows with reference to specific embodiment：
Embodiment 1：
2.5g ammonium citrates, 0.8g germanium oxides, 1.92g frerrous chlorides and 15g sodium chloride are weighed, mixture is dissolved in
In 100ml deionized water and with hydrochloric acid conditioning solution PH to 2~3, with mixing speed 300r/min magnetic stirring apparatus, stirring
Wiring solution-forming is dissolved, then again using power as 400W ultrasonic device ultrasound 15min, is well mixed.The solution mixed is put into
Refrigerator overnight freezes, after be placed in freeze drier -50 DEG C of vacuum drying, until drying obtains mixture.Milled mixtures,
Take 10g mixed-powder to be placed in Noah's ark, Noah's ark is put into tube furnace, be passed through 300ml/min Ar inert gases 30min rows
500 DEG C of temperature is warming up to except air, then using 200ml/min Ar as carrier gas and with 10 DEG C/min programming rate, insulation 2h enters
Row carburizing reagent, reaction is cooled to room temperature after terminating under Ar atmosphere protections, obtains calcined product.Calcined product is collected, it is finely ground,
It is washed to untill not having NaCl in product, is dried at 80 DEG C, obtains three-dimensional communication carbon nanosheet network structure and load ultra-fine germanium
Sour ferrum nano material, its carbon nanosheet thickness is<5nm, germanic acid iron nano-particle particle diameter is 5nm or so.
With obtained material, PVDF, conductive carbon black mass ratio is 8:1:1 meter is applied to copper sheet as negative pole, with 1M's
LiPF6As electrolyte, using lithium piece as positive pole, half-cell is made, it circulates 50 circles under 400mA/g current density still protects
More than 1200mAh/g specific capacity is held, as shown in figure 8, and with excellent circulation performance, it is close in 6.4A/g electric current
Still there is 650mAh/g specific capacity, as shown in Figure 9 under degree.
Embodiment 2：
2.5g ammonium citrates, 0.8g germanium oxides, 1.92g frerrous chlorides and 15g sodium chloride are weighed, mixture is dissolved in
In 100ml deionized water and with hydrochloric acid conditioning solution PH to 2~3, with mixing speed 300r/min magnetic stirring apparatus, stirring
Wiring solution-forming is dissolved, then again using power as 400W ultrasonic device ultrasound 15min, is well mixed.The solution mixed is put into
Refrigerator overnight freezes, after be placed in freeze drier -50 DEG C of vacuum drying, until drying obtains mixture.Milled mixtures,
Take 8g mixed-powder to be placed in Noah's ark, Noah's ark is put into tube furnace, be passed through 300ml/min Ar inert gases 30min rows
600 DEG C of temperature is warming up to except air, then using 200ml/min Ar as carrier gas and with 10 DEG C/min programming rate, insulation 6h enters
Row carburizing reagent, reaction is cooled to room temperature after terminating under Ar atmosphere protections, obtains calcined product.Calcined product is collected, it is finely ground,
It is washed to untill not having NaCl in product, is dried at 80 DEG C, obtains three-dimensional communication carbon nanosheet network structure and load ultra-fine germanium
Sour ferrum nano material.
Embodiment 3：
2.5g ammonium citrates, 0.8g germanium oxides, 1.92g frerrous chlorides and 15g sodium chloride are weighed, mixture is dissolved in
In 100ml deionized water and with hydrochloric acid conditioning solution PH to 2~3, with mixing speed 300r/min magnetic stirring apparatus, stirring
Wiring solution-forming is dissolved, then again using power as 400W ultrasonic device ultrasound 15min, is well mixed.The solution mixed is put into
Refrigerator overnight freezes, after be placed in freeze drier -50 DEG C of vacuum drying, until drying obtains mixture.Milled mixtures,
Take 8g mixed-powder to be placed in Noah's ark, Noah's ark is put into tube furnace, be passed through 300ml/min Ar inert gases 30min rows
650 DEG C of temperature is warming up to except air, then using 200ml/min Ar as carrier gas and with 10 DEG C/min programming rate, insulation 6h enters
Row carburizing reagent, reaction is cooled to room temperature after terminating under Ar atmosphere protections, obtains calcined product.Calcined product is collected, it is finely ground,
It is washed to untill not having NaCl in product, is dried at 80 DEG C, obtains three-dimensional communication carbon nanosheet network structure and load ultra-fine germanium
Sour ferrum nano material.
Embodiment 4：
5g ammonium citrates, 0.8g germanium oxides, 1.92g frerrous chlorides and 15g sodium chloride are weighed, mixture is dissolved in 100ml
Deionized water in and with hydrochloric acid conditioning solution PH to 2~3, with mixing speed 300r/min magnetic stirring apparatus, stirring and dissolving
Wiring solution-forming, then again using power as 400W ultrasonic device ultrasound 15min, is well mixed.The solution mixed is put into refrigerator
In freeze overnight, after be placed in freeze drier -50 DEG C of vacuum drying, until drying obtains mixture.Milled mixtures, take 8g
Mixed-powder be placed in Noah's ark, Noah's ark is put into tube furnace, be passed through 300ml/min Ar inert gases 30min exclude it is empty
Gas, then 500 DEG C of temperature is warming up to using 200ml/min Ar as carrier gas and with 10 DEG C/min programming rate, insulation 8h carries out carbon
Change reaction, reaction is cooled to room temperature under Ar atmosphere protections after terminating, obtains calcined product.Calcined product is collected, finely ground, washing
Untill there is no NaCl into product, dried at 80 DEG C, obtain three-dimensional communication carbon nanosheet network structure and load ultra-fine germanic acid iron
Nano material.
Claims (2)
1. the carbon nanosheet network structure load germanic acid ferrum nano material of a kind of three-dimensional communication, it is characterised in that the material is grain
The homogeneous germanic acid iron nano dot uniform load in footpath is on the ultra-thin carbon nanosheet of three-dimensional communication, wherein germanic acid iron nano-particle particle diameter
In 5-10nm, the carbon nanosheet thickness of three-dimensional communication is that the mass percent of germanic acid iron and total carbon in 3-10nm, the material is：
(0.4-0.7):(0.6-0.3)。
2. the three-dimensional communication carbon nanosheet network structure of said structure loads the preparation method of ultra-fine germanic acid ferrum nano material, it is special
Levy and be to comprise the following steps：
(1) is mixed into carbon source with the one or more in sucrose, glucose, citric acid, ammonium citrate, using germanium oxide as ge source,
Frerrous chloride is source of iron, using the germanium and iron mol ratio in the carbon in carbon source and ge source, source of iron as (50~10):1:2, with ge source
Germanium and sodium chloride mass ratio be (0.01-0.1):1 meter, carbon source, ge source, source of iron and sodium chloride is added molten in deionized water
Solution, stirs wiring solution-forming and with hydrochloric acid conditioning solution PH to 2~3, is freezed after solution is homogeneous and obtain presoma, then vacuum is dry
It is dry, obtain mixture；
(2) mixture grind into powder made from step (1) is placed in constant-temperature tubular stove and calcined by：With N2, He or Ar
A kind of or mixing first is passed through inert gas by 200~400ml/min of flow 30-60 minutes to exclude as inert gas source
Air；Again using Ar as carrier gas, carrier gas flux is fixed as 50~200ml/min, heated up with 1~10 DEG C/min programming rate
Tube furnace is to 500~650 DEG C, and insulation 2-6h is carbonized, and reaction is cooled to room temperature after terminating, and obtains calcined product；
(3) calcined product made from collection steps (2), finely ground, is washed to untill not having NaCl in calcined product, is in temperature
Dried at 80~100 DEG C, obtain three-dimensional communication carbon nanosheet network structure and load ultra-fine germanic acid ferrum nano material.
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Citations (2)
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| CN105449214A (en) * | 2016-01-12 | 2016-03-30 | 广西师范大学 | Lithium ion battery cathode material of which nano particles embedded into carbon nanosheet and preparation method of lithium ion battery cathode material |
| CN105585001A (en) * | 2016-03-02 | 2016-05-18 | 三峡大学 | Preparation technique of three-dimensional porous carbon and application of three-dimensional porous carbon in sodium-ion batteries |
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2017
- 2017-06-09 CN CN201710432552.3A patent/CN107331836A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105449214A (en) * | 2016-01-12 | 2016-03-30 | 广西师范大学 | Lithium ion battery cathode material of which nano particles embedded into carbon nanosheet and preparation method of lithium ion battery cathode material |
| CN105585001A (en) * | 2016-03-02 | 2016-05-18 | 三峡大学 | Preparation technique of three-dimensional porous carbon and application of three-dimensional porous carbon in sodium-ion batteries |
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| SHUAIXING JIN, ET AL.: "Synthesis and first investigation of excellent lithium storage performances of Fe2GeO4/ reduced grapheme oxide nanocomposite", 《NANO ENERY》 * |
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Application publication date: 20171107 |