CN106299367A - A kind of negative electrode of power lithium-ion battery porous carbon material and preparation method thereof - Google Patents
A kind of negative electrode of power lithium-ion battery porous carbon material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of negative electrode of power lithium-ion battery porous carbon material and preparation method thereof.First zinc salt is proportionally mixed with carbon source, obtain the metal-organic framework materials containing zinc；Then the metal-organic framework materials containing zinc is at high temperature carried out carbonization and except zinc processes the porous carbon material obtained based on micropore and mesopore.When the porous carbon material of gained is used for lithium ion battery cathode material, it is shown that outstanding specific discharge capacity, excellent cyclical stability and high rate performance.
Description
Technical field
The present invention relates to a kind of negative electrode of power lithium-ion battery porous carbon material and preparation method thereof, belong to electrochemical energy storage and clean energy resource field.
Background technology
Along with the continuous intensification of society's process of industrialization, for meeting the demand of sustainable economic development and protection of natural resources and environment, the research and development of clean energy resource and application have become as the key areas of Present S & T Development.Lithium ion battery is as a kind of electrochmical power source, there is specific capacity height, running voltage height, memory-less effect and advantages of environment protection, have been widely used at present on the miniaturized electronics such as mobile phone, portable computer, digital camera, and have market widely.And the research for the lithium ion battery of high power high-energy-density is rapidly heated also with the increase of the market demand, particularly in the field such as transportation and national defense industry, all stored energy capacitance, high rate performance and the security performance of lithium ion battery is had higher requirement.
At present, the widest lithium ion battery negative of commercial applications is mainly mesophase pitch microbeads, modified natural graphite and Delanium etc., the feature that these materials have good conductivity, cheap and safety is good.But the theoretical capacity of this kind of Carbon Materials is only 372mAh/g, and owing to having that scantling is big, specific surface area is little and the problem such as electrolyte wellability difference, causing lithium ion diffusion resistance wherein big, the high rate performance under big electric current is very poor, is difficult to meet the service behaviour demand of power lithium-ion battery.In order to substitute tradition carbon electrode material, it has been developed that the Carbon Materials of other form numerous, such as the composite etc. of CNT, hollow carbon sphere, carbon fiber, Graphene, porous carbon material and metal and oxide thereof with charcoal.In numerous new electrode materials, porous carbon material has the other pore passage structure of microscale-nanoscale, can be the diffusion transport more diffusion admittance of offer and the avtive spot of lithium ion, be conducive to improving lithium ion diffusion rate in the electrodes, thus substantially improve lithium storage content and the high rate performance of material.[R.Song, the et al. J. Mater. such as Song
Chem., 2012,22,12369] template is utilized, with linear phenol-aldehyde resin for presoma carbon source, with copper nitrate for templated metal source, by controlling the porous carbon material that condition of carbonization is prepared for having hierarchical pore structure, this porous carbon material presents the microscopic appearance of nanoscale twins and substantial amounts of middle aperture internal structure so that it is show high lithium storage content and big current ratio performance.[J.Yang, the et al. such as Yang
Electrochim. Acta, 2011,56,8576] with silicon dioxide gel as template, sucrose is carbon source, has synthesized the mesoporous porous carbon material that pore-size distribution is narrower, BET specific surface area is 420m2/ g, they can be with charge/discharge capacity up to 407 mAh/g.The template that the many uses of the above method are extra, needs to increase extra removing step after carbonization process, and will strictly control process conditions in presoma preparation process and carbonization process, to ensure that the shape of template reaches necessary requirement with distribution.
Recently, metal-organic framework materials (metal-organic frameworks, MOFs) prepare porous carbon materials field in template and obtain the biggest concern, this kind of material has designability and the controllability of modular structure, and the orderly pore structure that available pore-size distribution is single and specific surface area is big.Owing to having the above advantage, the metallic organic framework class material such as MOFs is considered as the excellent presoma preparing nanoporous Carbon Materials, and will be greatly expanded the structure of carbon nano-material and the kind of character.[Liu B, the et al. J. Am. such as Xu
Chem. Soc., 2008,130,5390] report at first with MOF-5 as template, utilize the method for vapour deposition to make furfuryl alcohol enter in the duct of MOF-5 and be polymerized, carbonization metallic zinc is volatilized under high temperature, obtain specific surface area and be up to 2872 m2The porous charcoal of/g.[Hu M, the et al. J. Am. Chem. such as Hu
Soc., 2012,134,2864] reporting a kind of with the MOFs containing aluminum as presoma, direct carbonization at 800 DEG C, they have obtained up to 5500 m2The specific surface area of/g.These methods all can need use extra carbon source or remove metal or its oxide etc. of remaining after charring process.
Summary of the invention
Present invention solves the technical problem that and be to provide a kind of negative electrode of power lithium-ion battery porous carbon material with very height ratio capacity and excellence big current ratio performance and preparation method thereof.
The present invention provide a kind of negative electrode of power lithium-ion battery porous carbon material, rich in micropore and mesopore, pore diameter range is between 0.2-50nm, and wherein micropore size is 0.2-2nm, mesopore pore size between 2-50nm, specific surface area 1100-3600m2/g。
The preparation method of a kind of negative electrode of power lithium-ion battery porous carbon material that the present invention provides, comprises the steps:
Step one: after being dissolved in solvent than the ratio for 4:1～1:5 with carbon source molecular number according to metal ion with carbon source by zinc salt, is processed by a step, obtains organometallic skeletal presoma.
Step 2: by organometallic skeletal presoma under inert atmosphere protection, carbonization 2～8 hours at 900～1200 DEG C, obtain target product.
Preferably, zinc salt described in step one selects zinc nitrate, zinc chloride, zinc sulfate and zinc acetate.
Preferably, described carbon source described in step one is selected from p-phthalic acid, to benzenetricarboxylic acid, 2-methylimidazole, fumaric acid and 4,4'-Bipyridine.
Preferably, described solvent described in step one is selected from DMF (DMF), N, N-diethylformamide (DEF) and methanol.
Preferably, a described step processing method described in step one stands selected from normal heating, hydro-thermal method and room temperature.
Carbonization process involved by step 2 is universal process prepared by Carbon Materials, i.e. under the protection of the noble gas such as nitrogen, argon, with certain heating rate, temperature rises to assigned temperature, and keeps certain time at this temperature.
Mainly there is several aspect in pore structure source in porous carbon material of the present invention, first it is the orderly pore passage structure that possessed of presoma MOFs itself, although these pore passage structures can cave in because of the pyrolysis of organic components in carbonization process, but also can be retained to a certain extent, thus serve the effect of template；Secondly, the effusion process at carbonization pyrolysis small molecular gas can cause certain micropore canals structure；Additionally, the boiling point of zinc is 907 DEG C, the carbonization temperature that we select is higher than this temperature, the zinc of gained of reducing in insulating process can constantly gasify and escape, footprint and the gas zinc of the mushy stage metallic zinc of the reduction gained under Can Liu escape the duct caused, and these all can cause the generation of substantial amounts of micropore and mesopore.The porous carbon material of gained of the present invention is suitable as lithium ion battery negative material.Owing to having the pore passage structure of higher specific surface area and different size and shape, thus the infiltration of beneficially electrolyte, and then improve diffuser efficiency and the storage volume of lithium ion.
The battery performance test of this negative material shows, under the electric current density of 50mA/g, it is shown that the reversible capacity of up to 1321～1610mAh/g, even if after circulation 50 times, its storage lithium specific capacity remains to be maintained at 1280～1595mAh/g.Under the conditions of big electric current impulse electricity, under the electric current density of 500 mA/g, reversible capacity has remained in that 860 mAh/g, and having circulated 300 after this, lithium storage content stills remain in 790 more than mAh/g.
Report [J.Yi et at according to Yi et al., J. Power Sources, 2011,196,6670], commercial natural graphite material reversible capacity under the electric current density of 18.6mA/g is 329.5mAh/g, and its reversible capacity is less than 50mAh/g under the electric current density of 167.4mA/g.And the silicon template reported at present to prepare the reversible capacity that the level porous carbon material of gained reached under the electric current density of 0.1C be 456.6mAh/g, being promoted to during 5C is 268mAh/g.[Yang J. et
al,Electrochim. Acta, 2011, 56, 8576].Compared to commercialization graphite material and the porous carbon material lithium ion battery negative of existing report, negative electrode of power lithium-ion battery porous carbon material provided by the present invention has more excellent reversible capacity and high rate performance.
The present invention has that controllability simple to operate is strong, preparation cost is low, excellent product performance and easily realize the advantage of large-scale production, has the biggest practice significance.
Accompanying drawing explanation
Accompanying drawing 1～3 is MOFs, the test figure of the porous carbon material of gained after 1000 DEG C of carbonizations synthesized by zinc nitrate that the embodiment of the present invention 1 mol ratio is 4:1 and p-phthalic acid.
Accompanying drawing 1 is the DFT pore size distribution figure of material；
Accompanying drawing 2 is the nitrogen adsorption isothermal curve of material；
Charge and discharge cycles figure when accompanying drawing 3 is as lithium ion battery negative, under 50 mA/g and 500mA/g electric current densities.
Detailed description of the invention
In order to be further appreciated by the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but it is to be understood that these describe simply as further illustrating the features and advantages of the present invention rather than limiting to the claimed invention.
Embodiment 1
Weigh 6g zinc nitrate and 0.8g p-phthalic acid, be dissolved in 100mlDMF, at 120 DEG C, then react 24h, obtain MOFs presoma.By MOFs presoma in nitrogen is protected, it is incubated 4h at 1000 DEG C, then naturally cools to room temperature, obtain target carbonizing production.
As shown in Figure 1 and Figure 2, products therefrom specific surface area is 2565m2/ g, pore volume is 2.76cm3/ g, micropore size 1.3nm, mesopore pore size 6.4nm.
Test electrode uses coating method to make.Detailed process is as follows: according to the quality of 8:1:1, the porous carbon material of gained, acetylene black and binding agent PVDF are compared mix homogeneously, it is fully ground dispersion with N-Methyl pyrrolidone, it is coated in after being modulated into homogeneous paste thing in the nickel foam of circle, after the most again vacuum tank being dried 12h at 120 DEG C, is pressed into thin slice.Battery testing uses button-shaped CR2032 type system simulated battery, is wherein metal lithium sheet to electrode.Battery is carried out constant current charge-discharge test, to investigate the reversible lithium storage capacity of this material, cycle performance and big current ratio performance.Charging/discharging voltage scope is 0.01～3.0V, circulates 50 times under the electric current density of 50mA/g, circulates 300 times under the electric current density of 500mA/g.
As it is shown on figure 3, during as lithium ion battery negative material, discharge capacity has reached 3710mAh/g first, and reversible capacity is up to 1600mAh/g.Under the electric current density of 50 mA/g, after circulating 50 times, still remain in 1590 more than mAh/g, almost without decay；Under the electric current density of 500mA/g, even if after circulating 300 times, reversible discharge capacity still possesses 790mAh/g, quite excellent.
Embodiment 2
Weigh 4.5g zinc nitrate and 0.8g p-phthalic acid, be dissolved in 150mlDEF, at 105 DEG C, then react 24h, obtain MOFs presoma.By MOFs presoma in nitrogen is protected, it is incubated 4h at 1000 DEG C, then naturally cools to room temperature, obtain target carbonizing production.
Products therefrom specific surface area is 2328m2/ g, pore volume is 2.16cm3/ g, micropore size 1.2nm, mesopore pore size 6.1nm.Using method same as in Example 1 to carry out electro-chemical test, result shows, electric current density is that to circulate the reversible capacity of 50 times under 50mA/g be 1451mAh/g.Electric current density is that after circulating 300 times under 500mA/g, reversible capacity is 745mAh/g.
Embodiment 3
Weigh 6g zinc nitrate and 0.8g p-phthalic acid, be dissolved in 100mlDMF, at 120 DEG C, then react 24h, obtain MOFs presoma.By MOFs presoma in nitrogen is protected, it is incubated 4h at 1100 DEG C, then naturally cools to room temperature, obtain target carbonizing production.
Products therefrom specific surface area is 2574m2/ g, pore volume is 2.65cm3/ g, micropore size 1.3nm, mesopore pore size 5.8nm.Using method same as in Example 1 to carry out electro-chemical test, result shows, electric current density is that to circulate the reversible capacity of 50 times under 50mA/g be 1522mAh/g.Electric current density is that after circulating 300 times under 500mA/g, reversible capacity is 782mAh/g.
Embodiment 4
Weigh the 2-methylimidazole of 3g zinc nitrate and 4.1g, be dissolved in 120ml methanol, at room temperature stand 12h after stirring and dissolving, obtain MOFs presoma.By MOFs presoma in nitrogen is protected, it is incubated 4h at 1000 DEG C, then naturally cools to room temperature, obtain target carbonizing production.
Products therefrom specific surface area is 1134m2/ g, pore volume is 1.34cm3/ g, micropore size 0.59nm, mesopore pore size 2.6nm.Using method same as in Example 1 to carry out electro-chemical test, result shows, electric current density is that to circulate the reversible capacity of 50 times under 50mA/g be 1243mAh/g.Electric current density is that after circulating 300 times under 500mA/g, reversible capacity is 692mAh/g.
Embodiment 5
Weigh 3.9g zinc nitrate and 1.6g fumaric acid, be dissolved in 150mlDMF, at 100 DEG C, then react 24h, obtain MOFs presoma.By MOFs presoma in nitrogen is protected, it is incubated 8h at 910 DEG C, then naturally cools to room temperature, obtain target carbonizing production.
Products therefrom specific surface area is 3532m2/ g, pore volume is 3.81cm3/ g, micropore size 1.12nm, mesopore pore size 2.82nm.Using method same as in Example 1 to carry out electro-chemical test, result shows, electric current density is that to circulate the reversible capacity of 50 times under 50mA/g be 1439mAh/g.Electric current density is that after circulating 300 times under 500mA/g, reversible capacity is 678mAh/g.
Embodiment 6
Weigh the 4,4'-Bipyridine of 3g zinc nitrate and 1.56g, be dissolved in 100ml ethanol, at 100 DEG C, then react 12h, obtain MOFs presoma.By MOFs presoma in nitrogen is protected, it is incubated 2h at 1200 DEG C, then naturally cools to room temperature, obtain target carbonizing production.
Products therefrom specific surface area is 1938m2/ g, pore volume is 2.09cm3/ g, micropore size 0.89nm, mesopore pore size 3.2nm.Using method same as in Example 1 to carry out electro-chemical test, result shows, electric current density is that to circulate the reversible capacity of 50 times under 50mA/g be 1103mAh/g.Electric current density is that after circulating 300 times under 500mA/g, reversible capacity is 672mAh/g.
Embodiment 7
Weigh 2.2g zinc nitrate and 0.8g p-phthalic acid, be dissolved in 150mlDEF, at 105 DEG C, then react 24h, obtain MOFs presoma.By MOFs presoma in nitrogen is protected, it is incubated 4h at 1000 DEG C, then naturally cools to room temperature, obtain target carbonizing production.
Products therefrom specific surface area is 2128m2/ g, pore volume is 1.91cm3/ g, micropore size 0.8nm, mesopore pore size 3.1nm.Using method same as in Example 1 to carry out electro-chemical test, result shows, electric current density is that to circulate the reversible capacity of 50 times under 50mA/g be 1381mAh/g.Electric current density is that after circulating 300 times under 500mA/g, reversible capacity is 725mAh/g.
The explanation of above example is only intended to help to understand method and the core concept thereof of the present invention.It should be pointed out that, for those skilled in the art, under the premise without departing from the principles of the invention, it is also possible to the present invention is carried out some improvement and modification, these improve and modify in the protection domain also falling into the claims in the present invention.
Described above to the disclosed embodiments, makes professional and technical personnel in the field be capable of or uses the present invention.Multiple amendment to these embodiments will be apparent from for those skilled in the art, and generic principles defined herein can realize without departing from the spirit or scope of the present invention in other embodiments.Therefore, the present invention is not intended to be limited to the embodiments shown herein, and is to fit to the widest scope consistent with principles disclosed herein and features of novelty.
Claims (7)
1. a negative electrode of power lithium-ion battery porous carbon material, rich in micropore and mesopore, pore diameter range is between 0.2-50nm, and wherein micropore size is 0.2-2nm, mesopore pore size between 2-50nm, specific surface area 1100-3600m2/g。
2. a preparation method for the porous carbon material described in claim 1, comprises following step:
(1), after zinc salt being dissolved in solvent than the ratio for 4:1～1:5 with carbon source molecular number according to metal ion with carbon source, processed by a step, obtain organometallic skeletal presoma;
(2) by organometallic skeletal presoma under inert atmosphere protection, carbonization 2～8 hours at 900～1200 DEG C, obtain target product.
The preparation method of porous charcoal the most according to claim 2, it is characterised in that: described zinc salt is the one in zinc nitrate, zinc chloride, zinc sulfate and zinc acetate.
The preparation method of porous charcoal the most according to claim 2, it is characterised in that: described carbon source is selected from p-phthalic acid, to benzenetricarboxylic acid, 2-methylimidazole, fumaric acid and 4,4'-Bipyridine.
The preparation method of porous charcoal the most according to claim 2, it is characterised in that: described solvent is selected from DMF, N, N-diethylformamide and methanol.
The preparation method of porous charcoal the most according to claim 2, it is characterised in that: a described step processing method stands selected from normal heating, hydro-thermal method and room temperature.
7., when using as lithium ion battery negative material, there is reversible specific capacity and the good circulation stability of 1590 mAh/g.
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| CN108832110A (en) * | 2018-06-26 | 2018-11-16 | 华南师范大学 | A kind of compound ZIF-8 negative electrode material of height ratio capacity bismuth nanoparticle and its preparation method and application |
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Application publication date: 20170104 |