CN106941156B - A kind of silicon silver carbon nano-hybrid material and its preparation method and application - Google Patents
A kind of silicon silver carbon nano-hybrid material and its preparation method and application Download PDFInfo
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- CN106941156B CN106941156B CN201710159783.1A CN201710159783A CN106941156B CN 106941156 B CN106941156 B CN 106941156B CN 201710159783 A CN201710159783 A CN 201710159783A CN 106941156 B CN106941156 B CN 106941156B
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Abstract
The present invention discloses a kind of silicon silver carbon nano-hybrid material and its preparation method and application.Silicon silver carbon nano-hybrid material is distributed in continuous carbon Medium Culture by silicon nano, extra small Nano silver grain, and Nano silver grain size range is in 1nm~5nm.The material is that silver salt is dissolved in the curing agent polyamine of epoxy resin using ultrasonic method, and cured, calcining is prepared.Continuous carbon matrix obtained by the present invention effectively inhibits bulk effect of the silicon in cyclic process, experiment is modified by technology, extra small Nano silver grain is introduced in silicon-carbon cathode, the presence of extra small Nano silver grain, which has, to be conducive to form more multi-emitting electric field in charge and discharge process, to construct high speed conductive channel, realizing silicon-based anode high rate performance significantly improves.
Description
Technical field
The invention belongs to macromolecule inorganic nano hybrid material field, it is related to a kind of silicon silver carbon nano-hybrid material and preparation
The application of method and the material in negative electrode of lithium ion battery.
Background technique
Current commercialized lithium ion battery negative material is graphite, theoretical specific capacity 372mAhg-1, as graphite
The alternative material of cathode, the theoretical specific capacity of silicon are as many as ten times of graphite (4200mAhg-1), and silicon is in crustal elements content
In be number two, it is environmental-friendly.Thus it is considered as most potential next-generation negative electrode of lithium ion battery alternative materials.But silicon material
Expect that the defect of itself limits its application.Such as: poorly conductive is difficult to form good conductive mesh in charge and discharge process
Network is unfavorable for lithium ion and is quickly embedded in and deviates from.On the other hand, during charge and discharge, silicon has serious bulk effect
(occurring 300% volume contraction in discharge process), for the modification of silicon based anode material, researcher is mainly in terms of three
Hand: nanosizing, Composite and structure design.
Summary of the invention
A kind of purpose of the invention is in view of the deficiencies of the prior art, a kind of silicon silver carbon nano-hybrid material to be provided, by silicon
Nanoparticle, extra small Nano silver grain are distributed in continuous carbon Medium Culture, and Nano silver grain size range is in 1nm~5nm；The material
It is that silver salt is dissolved in the curing agent polyamine of epoxy resin using ultrasonic method, cured, calcining is prepared.
It is a further object to provide the preparation method of above-mentioned silicon silver carbon nano-hybrid material, this method it is specific
Step is:
Step (1), first by silver salt by ultrasonic dissolution into polyamine, obtain polyamine-silver ion composite material；Its
The mass ratio of middle silver salt and polyamine is 0.01~1:1；
The silver salt is one of silver acetate, silver chlorate, silver fluoride, silver perchlorate etc. or several；
The polyamine is polyetheramine D400, in polyetheramine D230, ethylenediamine, diethylenetriamine, isophorone diamine
One or several kinds；
Silicon nano is added in epoxy resin by step (2), the polyamine-silver ion then obtained with step (1)
Composite material is mixed and stirred for 10-15 minutes, is finally injected the mixture into Teflon mould, and moves into baking oven progress
Solidification.Silicon nano and epoxy resin mass ratio are 0.01~0.2:1.Epoxy resin and polyamine-silver ion composite material
Mass ratio be 5~50:1；
Condition of cure are as follows: temperature uses 80~90 DEG C, and the reaction time is 30~60 minutes；
The silicon nano is having a size of 10~700nm；
The epoxy resin is DER331, E40, E42, one or more of resins such as E44, E51；Epoxy resin
Dosage is calculated according to polyamine dosage and epoxy resin epoxy value and is determined.
Obtained solid is placed in corundum crucible by step (3) by step (2), in tube furnace under inert gas atmosphere
Calcining, obtains silicon silver carbon nano hybridization powder；
Inert gas atmosphere is one of argon gas, nitrogen, argon gas/hydrogen, nitrogen/hydrogen；
The calcination temperature be 500~1100 DEG C, calcination time be 1~for 24 hours；
Nano silver grain size range is in 1nm~5nm in silicon silver carbon nano hybridization powder.
Another object of the present invention is to study obtained silicon silver carbon nano-hybrid material in lithium ion battery negative material
The application of aspect.
The present invention is prepared for the good silicon-carbon cathode of cycle performance using green short-cut method, and the present invention uses function solvent
System: i.e. in all steps of experiment, the processing of solvent it is not related to.It is molten that epoxy resin and curing agent have each acted as function
Agent, a kind of substance have obtained multiple use, not only environmentally protective, but also step is simple.Obtained continuous carbon matrix is effective
Bulk effect of the silicon in cyclic process is inhibited, experiment is modified by technology, and extra small silver nanoparticle is introduced in silicon-carbon cathode
Particle, the presence of extra small Nano silver grain, which has, to be conducive to form more multi-emitting electric field in charge and discharge process, to construct high speed
Conductive channel, realizing silicon-based anode high rate performance significantly improves.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture of the silicon silver carbon nano-hybrid material prepared in embodiment 8；Wherein (a) is low power figure,
It (b) is high power figure；
Fig. 2 is the circulation and high rate performance data of the silicon silver carbon and silicon-carbon nano-hybrid material that prepare in embodiment 8；Wherein
Fig. 2 .a is the cycle performance datagram of silicon-carbon cathode material, and Fig. 2 .b is the cycle performance datagram of silicon silver carbon negative pole material, figure
2.c is silicon-carbon and silicon silver Carbon anode high rate performance datagram.
Specific embodiment
The present invention is further analyzed combined with specific embodiments below.
Silicon nano used in following embodiment is having a size of 10~700nm.
Embodiment 1
Step (1), first by 0.01g silver acetate by ultrasonic dissolution into 1g polyetheramine D400, obtain polyamine-silver from
Sub- composite material；
0.01g silicon nano is added in 1g epoxy resin DER331 by step (2), then with 0.147g step (1)
Obtained polyamine-silver ion composite material is mixed and stirred for 10 minutes, finally injects the mixture into Teflon mould
In, and move into baking oven and solidified, temperature uses 80 DEG C, and the reaction time is 60 minutes；
Obtained solid is placed in corundum crucible by step (3) by step (2), in 500 DEG C under an argon atmosphere in tube furnace
Calcining for 24 hours, obtains silicon silver carbon nano hybridization powder.
Embodiment 2
Step (1), first by 1g silver chlorate by ultrasonic dissolution into 1g polyetheramine D230, obtain polyamine-silver ion
Composite material；
0.2g silicon nano is added in 1g epoxy resin E40 by step (2), is then obtained with 0.147g step (1)
Polyamine-silver ion composite material be mixed and stirred for 10 minutes, finally inject the mixture into Teflon mould, and
It moves into 90 DEG C of baking oven and carries out solidification 30 minutes.
Obtained solid is placed in corundum crucible by step (3) by step (2), in tube furnace in a nitrogen atmosphere 1100
DEG C calcining 1h, obtain silicon silver carbon nano hybridization powder.
Embodiment 3
Step (1), first by 0.1g silver fluoride by ultrasonic dissolution into 1g ethylenediamine, obtain polyamine-silver ion it is multiple
Condensation material；
0.1g silicon nano is added in 1g epoxy resin E42 by step (2), is then obtained with 0.147g step (1)
Polyamine-silver ion composite material be mixed and stirred for 15 minutes, finally inject the mixture into Teflon mould, and
It moves into 85 DEG C of baking oven and carries out solidification 40 minutes.
Obtained solid is placed in corundum crucible by step (3) by step (2), in tube furnace under argon/hydrogen atmosphere
600 DEG C of calcining 18h obtain silicon silver carbon nano hybridization powder.
Embodiment 4
Step (1), first by 0.2g silver perchlorate by ultrasonic dissolution into 1g diethylenetriamine, obtain polyamine-silver
Ion composite material；
0.15g silicon nano is added in 1g epoxy resin E44 by step (2), is then obtained with 0.147g step (1)
To polyamine-silver ion composite material be mixed and stirred for 12 minutes, finally inject the mixture into Teflon mould,
And it moves into 82 DEG C of baking oven and carries out solidification 50 minutes.
Obtained solid is placed in corundum crucible by step (3) by step (2), in tube furnace under nitrogen/hydrogen atmosphere
1000 DEG C of calcining 2h obtain silicon silver carbon nano hybridization powder.
Embodiment 5
Step (1), first by 0.5g silver acetate, 0.3g silver chlorate by ultrasonic dissolution into isophorone diamine, obtain
Polyamine-silver ion composite material；
0.05g silicon nano is added in 1g epoxy resin E51 by step (2), is then obtained with 0.147g step (1)
To polyamine-silver ion composite material be mixed and stirred for 14 minutes, finally inject the mixture into Teflon mould,
And it moves into 90 DEG C of baking oven and carries out solidification 60 minutes.
Obtained solid is placed in corundum crucible by step (3) by step (2), in 700 DEG C in a nitrogen atmosphere in tube furnace
15h is calcined, silicon silver carbon nano hybridization powder is obtained.
Embodiment 6
Step (1), first by 0.2g silver fluoride, 0.2g silver perchlorate by ultrasonic dissolution to 0.5g polyetheramine D230,
In 0.5g ethylenediamine, polyamine-silver ion composite material is obtained；
0.1g silicon nano is added in 0.5g epoxy resin E44,0.5g epoxy resin E51 by step (2), then
The polyamine obtained with 0.0735g step (1)-silver ion composite material is mixed and stirred for 10 minutes, is finally injected the mixture into
Into Teflon mould, and moves into 85 DEG C of baking oven and carry out solidification 50 minutes.
Obtained solid is placed in corundum crucible by step (3) by step (2), in tube furnace under argon/hydrogen atmosphere
900 DEG C of calcining 5h obtain silicon silver carbon nano hybridization powder.
Embodiment 7
Step (1), first by 0.03g silver fluoride by ultrasonic dissolution into 0.6g ethylenediamine, 0.4g diethylenetriamine, obtain
Obtain polyamine-silver ion composite material；
0.1g silicon nano is added in 0.3g epoxy resin DER331,0.7g epoxy resin E40 by step (2), so
The polyamine obtained afterwards with 0.1029g step (1)-silver ion composite material is mixed and stirred for 15 minutes, finally infuses mixture
Enter into Teflon mould, and moves into 85 DEG C of baking oven and carry out solidification 50 minutes.
Obtained solid is placed in corundum crucible by step (3) by step (2), in tube furnace under an argon atmosphere 1100
DEG C calcining 1h, obtain silicon silver carbon nano hybridization powder.
In the silicon silver carbon nano hybridization powder that above-described embodiment 1-7 is prepared Nano silver grain size range 1nm~
5nm。
Embodiment 8
Step (1), first by 0.3g silver nitrate by ultrasonic dissolution into 1.47g diethylenetriamine, obtain polyamine-silver
Ion composite material；
1g silicon nano is added in 10g epoxy resin DER331 by step (2), is then obtained with 1.77g step (1)
To polyamine-silver ion composite material be mixed and stirred for 15 minutes, finally inject the mixture into Teflon mould,
And it moves into 85 DEG C of baking oven and carries out solidification 30 minutes.
Obtained solid is placed in corundum crucible by step (3) by step (2), in 800 DEG C under an argon atmosphere in tube furnace
4h is calcined, silicon silver carbon nano hybridization powder is obtained.
From being clear that size about 3nm in silicon silver carbon nano hybridization powder that embodiment 8 is prepared in Fig. 1
Nano silver grain.
Fig. 2 .a is the cycle performance datagram of silicon-carbon.Fig. 2 .b is the silicon silver carbon nano hybridization material that embodiment 8 is prepared
The cycle performance datagram of material.Silicon-carbon and silicon silver carbon nano-hybrid material show good follow as ion cathode material lithium
Ring stability.By 100 charge and discharge cycles, the charging capacity of silicon silver carbon is 699mAhg-1, capacity retention ratio 71%；Silicon-carbon
Charging capacity is 674mAhg-1, capacity retention ratio 69%.Capacity retention ratio calculates according to the following formula:
Charging capacity maximum value in charging capacity/cyclic process of capacity retention ratio=100th time.
The high rate performance datagram for the silicon silver carbon nano-hybrid material that Fig. 2 .c is silicon-carbon and embodiment 8 is prepared.Silicon silver
Carbon nano-hybrid material shows superior high rate performance than silicon-carbon nano-hybrid material:
Under the current density of 1C, 2C and 5C when charge and discharge, silicon silver carbon discharge capacity average value is respectively 795mAhg-1,
530mAhg-1And 299mAhg-1；Under the current density of 1C, 2C and 5C when charge and discharge, discharge capacity average value divides silicon-carbon cathode
It Wei not 572mAhg-1,342mAhg-1And 128mAhg-1。
Above-described embodiment is not for limitation of the invention, and the present invention is not limited only to above-described embodiment, as long as meeting
The present invention claims all belong to the scope of protection of the present invention.
Claims (8)
1. a kind of preparation method of silicon silver carbon nano-hybrid material, it is characterised in that method includes the following steps:
Step (1), first by silver salt by ultrasonic dissolution into polyamine, obtain polyamine-silver ion composite material；
Silicon nano is added in epoxy resin by step (2), and the polyamine-silver ion then obtained with step (1) is compound
Material is mixed and stirred for 10-15 minutes, is finally injected the mixture into Teflon mould, and is moved into baking oven and consolidated
Change；
Obtained solid is placed in corundum crucible by step (3) by step (2), in being calcined under inert gas atmosphere in tube furnace,
Obtain silicon silver carbon nano hybridization powder；
Above-mentioned silicon silver carbon nano-hybrid material is distributed in continuous carbon Medium Culture, Yin Na by silicon nano, extra small Nano silver grain
Rice corpuscles size is in 1nm~5nm.
2. the method as described in claim 1, it is characterised in that the mass ratio of step (1) silver salt and polyamine is 0.01~1:1.
3. the method as described in claim 1, it is characterised in that silver salt described in step (1) is silver acetate, silver chlorate, fluorination
Silver, one of silver perchlorate or several, polyamine is polyetheramine D400, polyetheramine D230, ethylenediamine, diethylenetriamine,
One of isophorone diamine is several.
4. the method as described in claim 1, it is characterised in that epoxy resin described in step (2) be DER331, E40, E42,
One or more of E44, E51 resin.
5. the method as described in claim 1, it is characterised in that step (2) silicon nano is 0.01 with epoxy resin mass ratio
~0.2:1；Epoxy resin and polyamine-silver ion composite material mass ratio are 5~50:1.
6. the method as described in claim 1, it is characterised in that step (2) condition of cure are as follows: temperature uses 80~90 DEG C, reaction
Time is 30~60 minutes.
7. the method as described in claim 1, it is characterised in that step (2) described silicon nano is having a size of 10~700nm.
8. the method as described in claim 1, it is characterised in that calcination temperature described in step (3) is 500~1100 DEG C, calcining
Time be 1~for 24 hours.
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| CN103151504A (en) * | 2013-04-08 | 2013-06-12 | 廖小玉 | Preparation method of silver doped carbon-silicon composite negative electrode material |
| CN103545488A (en) * | 2013-10-18 | 2014-01-29 | 中国第一汽车股份有限公司 | Method for preparing Si/Ag/C composite negative material based on silver mirror reaction principle |
| CN104332594A (en) * | 2014-10-10 | 2015-02-04 | 奇瑞汽车股份有限公司 | Silicon-based negative electrode material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103151504A (en) * | 2013-04-08 | 2013-06-12 | 廖小玉 | Preparation method of silver doped carbon-silicon composite negative electrode material |
| CN103545488A (en) * | 2013-10-18 | 2014-01-29 | 中国第一汽车股份有限公司 | Method for preparing Si/Ag/C composite negative material based on silver mirror reaction principle |
| CN104332594A (en) * | 2014-10-10 | 2015-02-04 | 奇瑞汽车股份有限公司 | Silicon-based negative electrode material and preparation method and application thereof |
Non-Patent Citations (1)
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| Preparation and Study on Si/Ag/C Composite as Anode Material for Lithium Ion Batteries;Tao Cui等;《Advanced Materials Research》;20131031;第834-836卷;第281-284页 * |
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