CN105047870A - Nitrogen-doped carbon-coated silicon composite material and preparation method thereof - Google Patents
Nitrogen-doped carbon-coated silicon composite material and preparation method thereof Download PDFInfo
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- H01M10/05—Accumulators with non-aqueous electrolyte
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Abstract
The invention discloses a nitrogen-doped carbon-coated silicon composite material and a preparation method thereof, and belongs to the field of lithium ion batteries. The nitrogen-doped carbon-coated silicon composite material comprises a silicon lithium-storage material which exists in the composite material as a main active substance, and organic pyrolytic nitrogen-doped carbon with certain lithium storage capacity and good electrical conductivity as a coating layer, wherein the content of silicon in the composite material is 30%-90%; and the preparation method comprises preparation and carbon-coating technologies of a composite material precursor. In addition, with cheap silicon dioxide as a silicon source, and the silicon dioxide is transformed into a silicon material with the lithium storage activity through a metal magnesiothermic reduction process. Compared with the prior art, the preparation method of the nitrogen-doped carbon-coated silicon composite material is short in flow, easy to operate and simple in synthetic process; large-scale production is easy to realize; and the prepared nitrogen-doped carbon-coated silicon composite material has excellent electrochemical property when taken as a lithium ion battery anode material, and has a potential application prospect in the fields of portable mobile devices and electric cars.
Description
Technical field:
The present invention relates to lithium ion battery negative material field, be specifically related to a kind of nitrating carbon coated Si composite material and preparation method thereof.
Background technology:
Current business-like lithium ion battery negative mainly uses graphite-like material with carbon element as active material, but its theoretical capacity is lower, only has 372mAh/g, is gradually difficult to meet people for the demand of lithium ion battery with high power capacity, high-energy-density.
In recent years, various lithium ion cell high-capacity negative material is developed gradually, this wherein silicium cathode material because of its very high theoretical capacity (4200mAh/g, Li
22si
5) become researcher pay close attention to focus.But, silicium cathode in charge and discharge cycles process with huge change in volume (about 300%), the mechanical stress that so huge bulk effect produces can make active material from collector peel off and silicon is active mutually self also can efflorescence, thus to lose and the electrical contact of collector and cause electrode cycle performance to decline rapidly.In addition, the intrinsic conductivity of silicon is very low by (6.7 × 10
-4s/cm), also limit its commercial applications.Current, the research for silicium cathode material mainly concentrates on its volumetric expansion of suppression, improves the aspects such as cycle performance.The major measure taked comprises silicon nanometer and silicon Composite two kinds.Nanometer mainly comprises methods such as preparing nano silica fume (as Chinese patent CN104332613A), silicon nanowires (as Chinese patent CN103515604A) and silicon thin film (as Chinese patent CN102637852A), although these methods effectively overcome the problem of silicon materials capacity attenuation in cyclic process, but the synthesis technique that it adopts is complicated, waste time and energy, be unfavorable for extensive preparation.Silicon Composite mainly prepares Si-C composite material, as Chinese patent (CN102623682A) and Chinese patent (CN103928662A), existing preparation method is by being simply difficult to obtain evenly coated Si-C composite material by solid material physical mixed, have impact on the cycle performance of composite material, simple pyrolytic carbon layer limited electrical conductivity also limit the charge-discharge performance of composite material under high current density simultaneously.
Therefore, developing the high power capacity silicon composite cathode material that a kind of preparation technology has good cyclical stability and good large current density electrical characteristics simply is simultaneously one of the technical barrier in affiliated field.
Summary of the invention:
For the deficiencies in the prior art, an object of the present invention is to provide a kind of nitrating carbon coated Si composite material and preparation method thereof, the method passes through a kind of nitrating carbon coated Si composite material of the nitrogenous organic carbon precursor power of pyrolysis, and described nitrating carbon coated Si composite material has good cyclical stability and good large current density electrical characteristics as lithium ion battery negative material.
The present invention adopts following technical scheme: a kind of nitrating carbon coated Si composite material, it comprise be present in composite inner and as the silicon materials of main storage lithium active material, and there is organic pyrolysis nitrating carbon coating layer of certain lithium storage content, the presoma of described nitrating carbon coating layer is ionic liquid.
The present invention also adopts following technical scheme: a kind of preparation method of nitrating carbon coated Si composite material, it comprises the steps:
(1) magnesium metal is mixed with silicon dioxide, by magnesium metal thermal reduction, silicon dioxide is converted into the silicon materials with storage lithium activity;
(2) joined by ionic liquid in the silicon materials that step (1) obtains, mixing, obtains the presoma of composite material;
(3) composite material precursor that step (2) obtains is heat-treated under protective atmosphere, obtain nitrating carbon coated Si composite material.
Further, in described step (1), magnesium metal refer in magnesium grain, magnesium powder one or both.
Further, in described step (2), ionic liquid refers to ethyl-trimethyl imidazoles three cyanogen first salt (EMIM-TCCN).
Further, in described step (2), the mass ratio of silicon materials and ionic liquid is 2:9 ~ 4:1.
Further, in described step (2), the mass ratio of silicon materials and ionic liquid is 3:13 ~ 1:1.
Further, in the nitrating carbon coated Si composite material obtained in described step (3), the mass ratio of silicon materials and nitrating carbon coating layer is 3:7 ~ 9:1.
Further, in the nitrating carbon coated Si composite material obtained in described step (3), the mass ratio of silicon materials and nitrating carbon coating layer is 9:11 ~ 3:1.
Further, in described step (3), protective atmosphere is argon gas.
Further, in described step (3), Technology for Heating Processing is two-step thermal processing method, first step heat treatment is for being warmed up to 200 ~ 300 DEG C of insulations 2 ~ 5 hours with 2 DEG C/min, second step heat treatment, for being warmed up to 400 ~ 800 DEG C of insulations 2 ~ 5 hours with 2 DEG C/min, can obtain nitrating carbon coated Si composite material.
The present invention has following beneficial effect:
(1) the present invention uses method simply to prepare nitrating carbon coated Si composite material, and when using as lithium ion battery negative material, this composite material has good cyclical stability and good large current density electrical characteristics;
(2) flow process of the present invention is short; be easy to operation; synthesis technique is simple; be easy to accomplish scale production; when the nitrating carbon coated Si composite material of preparation is as lithium ion battery negative material; there is excellent chemical property, in portable mobile apparatus and electric automobile, there is potential application foreground.
Accompanying drawing illustrates:
Fig. 1 is the XRD figure of nitrating carbon coated Si composite material prepared by the embodiment of the present invention 1.
Fig. 2 is the stereoscan photograph of nano silica fume prepared by the embodiment of the present invention 1.
Fig. 3 is the stereoscan photograph of nitrating carbon coated Si composite material prepared by the embodiment of the present invention 1.
Fig. 4 is the lithium ion battery first charge-discharge curve resolution chart that the nitrating carbon coated Si composite material of the embodiment of the present invention 1 preparation is made.
Fig. 5 is the cycle life of lithium ion battery resolution chart that nano silica fume prepared by the nitrating carbon coated Si composite material prepared of embodiment of the present invention 1-6 and comparative example 1 is made.
Embodiment:
Nitrating carbon coated Si composite material of the present invention comprise be present in composite inner and as the silicon materials of main storage lithium active material, and organic pyrolysis nitrating carbon coating layer that the conductivity with certain lithium storage content is good, the composition of nitrating carbon coated Si composite material of the present invention is described as silicon nitrogen-carbon (SiN-C).Wherein the presoma of nitrating carbon coating layer is ionic liquid.
The preparation method of nitrating carbon coated Si composite material of the present invention, comprises the steps:
(1) magnesium metal is mixed with silicon dioxide, by magnesium metal thermal reduction, silicon dioxide is converted into the silicon materials with storage lithium activity;
(2) joined by ionic liquid in the silicon materials that step (1) obtains, mixing, obtains the presoma of composite material;
(3) composite material precursor that step (2) obtains is heat-treated under protective atmosphere, obtain nitrating carbon coated Si composite material.
In step (1), magnesium metal refer in magnesium grain, magnesium powder one or both.
In step (2), ionic liquid refers to ethyl-trimethyl imidazoles three cyanogen first salt (EMIM-TCCN).
In step (2), the mass ratio of silicon materials and ionic liquid is (2:9) ~ (4:1), can be defined as further (3:13) ~ (1:1).
In the nitrating carbon coated Si composite material obtained in step (3), the mass ratio of silicon materials and nitrating carbon coating layer is (3:7) ~ (9:1), can be defined as further (9:11) ~ (3:1).
In step (3); protective atmosphere is argon gas; Technology for Heating Processing is two-step thermal processing method; first step heat treatment is for being warmed up to 200 ~ 300 DEG C of insulations 2 ~ 5 hours with 2 DEG C/min; second step heat treatment, for being warmed up to 400 ~ 800 DEG C of insulations 2 ~ 5 hours with 2 DEG C/min, can obtain nitrating carbon coated Si composite material.
Below by six specific embodiments, nitrating carbon coated Si composite material of the present invention and preparation method thereof is described.
Embodiment 1
Take 1g silicon oxide pellets powder to mix with 1g magnesium powder, be laid in aluminium oxide porcelain boat, be positioned over the position, the thermal treatment zone of tube furnace, under argon gas atmosphere protection, with the ramp of 2 DEG C/min to 680 DEG C, be incubated 6 hours, cool to room temperature with the furnace, then magnesium hot is placed in the hydrochloric acid that 50mL concentration is 1mol/L, stir 5 hours, centrifugation, distilled water washs three times, the solid obtained is placed in the hydrochloric acid that 50mL concentration is 1mol/L again, stir 5 hours, centrifugation, distilled water washs three times, absolute ethanol washing twice, last vacuumize 24 hours under 60 DEG C of conditions, nano silica fume can be obtained.
Mixed with the ionic liquid of 150mg by nano silica fume above-mentioned for 150mg, grinding evenly, can obtain the presoma of composite material.
The presoma of above-mentioned composite material is transferred in tube furnace and heat-treats, under an argon atmosphere, with the ramp of 2 DEG C/min to 300 DEG C, be incubated 5 hours, then with the ramp of 2 DEG C/min to 700 DEG C, be incubated 4 hours, with stove cooling, nitrating carbon coated Si composite material can be obtained.In this composite material, the content of silicon is 75.8%wt.
By prepared nitrating carbon coated Si composite material and commercially available sodium alginate and acetylene black in mass ratio 6:2:2 mix, prepare slurry with deionized water as solvent, be evenly coated on Copper Foil, put into vacuum drying chamber, vacuumize 12 hours under condition at 110 DEG C, takes out and is washed into pole piece.Using lithium sheet as to electrode, electrolyte is EC+DMC (volume ratio the is 1:1) solution of the LiPF6 of 1mol/L, adopts Celgard2400 barrier film, assembles CR2016 type button cell being full of in argon gas atmosphere glove box.Adopt blue electric tester to carry out electrochemical property test, discharge and recharge cut-ff voltage scope is 0.01V ~ 1.5V (vsLi
+/ Li), test under room temperature, charge-discharge performance is tested: measuring current density selects first 10 weeks to be 100mA/g, and 11 to 100 weeks were 500mA/g.
The charge-discharge performance test of the button cell that nitrating carbon coated Si composite material prepared by the present embodiment is made: reversible capacity is 1343.8mAh/g first, coulombic efficiency is 74.2% first, within 100th week, reversible capacity is 1180.7mAh/g, and reversible capacity conservation rate is 87.9%.
Embodiment 2
According to the method preparing nano silica fume in embodiment 1, prepare nano silica fume.
Mixed with the ionic liquid of 150mg by nano silica fume above-mentioned for 100mg, grinding evenly, can obtain the presoma of composite material.
The presoma of above-mentioned composite material is transferred in tube furnace and heat-treats, under an argon atmosphere, with the ramp of 2 DEG C/min to 200 DEG C, be incubated 2 hours, then with the ramp of 2 DEG C/min to 650 DEG C, be incubated 5 hours, with stove cooling, nitrating carbon coated Si composite material can be obtained.In this composite material, the content of silicon is 65.6%wt.
According to the method preparing button cell in embodiment 1, button cell made by the nitrating carbon coated Si composite material using the present embodiment to prepare, and according to electrochemical property test condition in embodiment 1, charge-discharge performance test carrying out to battery: reversible capacity is 1005.7mAh/g first, coulombic efficiency is 66.2% first, within 100th week, reversible capacity is 875.6mAh/g, and reversible capacity conservation rate is 87.1%.
Embodiment 3
According to the method preparing nano silica fume in embodiment 1, prepare nano silica fume.
Mixed with the ionic liquid of 650mg by nano silica fume above-mentioned for 150mg, grinding evenly, can obtain the presoma of composite material.
The presoma of above-mentioned composite material is transferred in tube furnace and heat-treats, under an argon atmosphere, with the ramp of 2 DEG C/min to 230 DEG C, be incubated 2 hours, then with the ramp of 2 DEG C/min to 800 DEG C, be incubated 3 hours, with stove cooling, nitrating carbon coated Si composite material can be obtained.In this composite material, the content of silicon is 45.7%wt.
According to the method preparing button cell in embodiment 1, button cell made by the nitrating carbon coated Si composite material using the present embodiment to prepare, and according to electrochemical property test condition in embodiment 1, charge-discharge performance test carrying out to battery: reversible capacity is 1005.4mAh/g first, coulombic efficiency is 72.5% first, within 100th week, reversible capacity is 661.6mAh/g, and reversible capacity conservation rate is 65.9%.
Embodiment 4
According to the method preparing nano silica fume in embodiment 1, prepare nano silica fume.
Mixed with the ionic liquid of 450mg by nano silica fume above-mentioned for 100mg, grinding evenly, can obtain the presoma of composite material.
The presoma of above-mentioned composite material is transferred in tube furnace and heat-treats, under an argon atmosphere, with the ramp of 2 DEG C/min to 250 DEG C, be incubated 4 hours, then with the ramp of 2 DEG C/min to 400 DEG C, be incubated 5 hours, with stove cooling, nitrating carbon coated Si composite material can be obtained.In this composite material, the content of silicon is 33.1%wt.
According to the method preparing button cell in embodiment 1, button cell made by the nitrating carbon coated Si composite material using the present embodiment to prepare, and according to electrochemical property test condition in embodiment 1, charge-discharge performance test carrying out to battery: reversible capacity is 587.1mAh/g first, coulombic efficiency is 48.6% first, within 100th week, reversible capacity is 563.9mAh/g, and reversible capacity conservation rate is 96%.
Embodiment 5
According to the method preparing nano silica fume in embodiment 1, prepare nano silica fume.
Mixed with the ionic liquid of 200mg by nano silica fume above-mentioned for 100mg, grinding evenly, can obtain the presoma of composite material.
The presoma of above-mentioned composite material is transferred in tube furnace and heat-treats, under an argon atmosphere, with the ramp of 2 DEG C/min to 280 DEG C, be incubated 3 hours, then with the ramp of 2 DEG C/min to 550 DEG C, be incubated 2 hours, with stove cooling, nitrating carbon coated Si composite material can be obtained.In this composite material, the content of silicon is 56.8%wt.
According to the method preparing button cell in embodiment 1, button cell made by the nitrating carbon coated Si composite material using the present embodiment to prepare, and according to electrochemical property test condition in embodiment 1, charge-discharge performance test carrying out to battery: reversible capacity is 1214mAh/g first, coulombic efficiency is 78.1% first, within 100th week, reversible capacity is 1009.8mAh/g, and reversible capacity conservation rate is 83.2%.
Embodiment 6
According to the method preparing nano silica fume in embodiment 1, prepare nano silica fume.
Mixed with the ionic liquid of 100mg by nano silica fume above-mentioned for 400mg, grinding evenly, can obtain the presoma of composite material.
The presoma of above-mentioned composite material is transferred in tube furnace and heat-treats, under an argon atmosphere, with the ramp of 2 DEG C/min to 300 DEG C, be incubated 4 hours, then with the ramp of 2 DEG C/min to 450 DEG C, be incubated 4 hours, with stove cooling, nitrating carbon coated Si composite material can be obtained.In this composite material, the content of silicon is 88.9%wt.
According to the method preparing button cell in embodiment 1, button cell made by the nitrating carbon coated Si composite material using the present embodiment to prepare, and according to electrochemical property test condition in embodiment 1, charge-discharge performance test carrying out to battery: reversible capacity is 1235.5mAh/g first, coulombic efficiency is 58.6% first, within 100th week, reversible capacity is 390.5mAh/g, and reversible capacity conservation rate is 31.6%.
Comparative example 1
According to the method preparing nano silica fume in embodiment 1, prepare nano silica fume.
According to the method preparing button cell in embodiment 1, the nano silica fume using the present embodiment to prepare makes button cell, and according to electrochemical property test condition in embodiment 1, charge-discharge performance test carrying out to battery: reversible capacity is 1252.5mAh/g first, coulombic efficiency is 43.6% first, within 100th week, reversible capacity is 455.5mAh/g, and reversible capacity conservation rate is 36.4%.
The above is only the preferred embodiment of the present invention, it should be pointed out that for those skilled in the art, can also make some improvement under the premise without departing from the principles of the invention, and these improvement also should be considered as protection scope of the present invention.
Claims (10)
1. a nitrating carbon coated Si composite material, it is characterized in that: comprise be present in composite inner and as the silicon materials of main storage lithium active material, and there is organic pyrolysis nitrating carbon coating layer of certain lithium storage content, the presoma of described nitrating carbon coating layer is ionic liquid.
2. a preparation method for nitrating carbon coated Si composite material, is characterized in that: comprise the steps
(1) magnesium metal is mixed with silicon dioxide, by magnesium metal thermal reduction, silicon dioxide is converted into the silicon materials with storage lithium activity;
(2) joined by ionic liquid in the silicon materials that step (1) obtains, mixing, obtains the presoma of composite material;
(3) composite material precursor that step (2) obtains is heat-treated under protective atmosphere, obtain nitrating carbon coated Si composite material.
3. the preparation method of nitrating carbon coated Si composite material as claimed in claim 2, is characterized in that: in described step (1), magnesium metal refer in magnesium grain, magnesium powder one or both.
4. the preparation method of nitrating carbon coated Si composite material as claimed in claim 2, it is characterized in that: in described step (2), ionic liquid refers to ethyl-trimethyl imidazoles three cyanogen first salt (EMIM-TCCN).
5. the preparation method of nitrating carbon coated Si composite material as claimed in claim 2, it is characterized in that: in described step (2), the mass ratio of silicon materials and ionic liquid is 2:9 ~ 4:1.
6. the preparation method of nitrating carbon coated Si composite material as claimed in claim 5, is characterized in that: in described step (2), the mass ratio of silicon materials and ionic liquid is 3:13 ~ 1:1.
7. the preparation method of nitrating carbon coated Si composite material as claimed in claim 2, is characterized in that: in the nitrating carbon coated Si composite material obtained in described step (3), the mass ratio of silicon materials and nitrating carbon coating layer is 3:7 ~ 9:1.
8. the preparation method of nitrating carbon coated Si composite material as claimed in claim 7, is characterized in that: in the nitrating carbon coated Si composite material obtained in described step (3), the mass ratio of silicon materials and nitrating carbon coating layer is 9:11 ~ 3:1.
9. the preparation method of nitrating carbon coated Si composite material as claimed in claim 2, it is characterized in that: in described step (3), protective atmosphere is argon gas.
10. the preparation method of nitrating carbon coated Si composite material as claimed in claim 2, it is characterized in that: in described step (3), Technology for Heating Processing is two-step thermal processing method, first step heat treatment is for being warmed up to 200 ~ 300 DEG C of insulations 2 ~ 5 hours with 2 DEG C/min, second step heat treatment, for being warmed up to 400 ~ 800 DEG C of insulations 2 ~ 5 hours with 2 DEG C/min, can obtain nitrating carbon coated Si composite material.
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| CN107195890A (en) * | 2017-06-28 | 2017-09-22 | 山东大学 | A kind of high performance lithium ionic cell cathode Si@N C composites and preparation method thereof |
| CN107749474A (en) * | 2017-10-30 | 2018-03-02 | 北京万源工业有限公司 | A kind of preparation method of silicon-carbon cathode material and the silicon-carbon cathode material |
| CN108149343A (en) * | 2017-12-12 | 2018-06-12 | 东华大学 | The composite nano fiber of N doping porous carbon cladding nano silicon particles and preparation |
| CN109103440A (en) * | 2018-04-08 | 2018-12-28 | 毛强平 | A kind of lithium ion battery negative material, preparation method and lithium ion battery |
| CN110582876A (en) * | 2017-05-12 | 2019-12-17 | 株式会社Lg化学 | Negative electrode active material, negative electrode comprising the same, and secondary battery comprising the same |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110582876A (en) * | 2017-05-12 | 2019-12-17 | 株式会社Lg化学 | Negative electrode active material, negative electrode comprising the same, and secondary battery comprising the same |
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| CN109103440A (en) * | 2018-04-08 | 2018-12-28 | 毛强平 | A kind of lithium ion battery negative material, preparation method and lithium ion battery |
| CN109103440B (en) * | 2018-04-08 | 2021-06-01 | 山东天安华力新材料科技有限公司 | Lithium ion battery cathode material, preparation method and lithium ion battery |
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Application publication date: 20151111 |