CN109360959A - A kind of carbon selenium material and preparation method thereof and the application in energy storage device - Google Patents
A kind of carbon selenium material and preparation method thereof and the application in energy storage device Download PDFInfo
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- CN109360959A CN109360959A CN201811188854.1A CN201811188854A CN109360959A CN 109360959 A CN109360959 A CN 109360959A CN 201811188854 A CN201811188854 A CN 201811188854A CN 109360959 A CN109360959 A CN 109360959A
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H01M10/00—Secondary cells; Manufacture thereof
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- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
Application the invention discloses a kind of carbon selenium material and preparation method thereof and in energy storage device; the preparation method of carbon selenium material is will to contain selenium organic matter and be placed under protective atmosphere to carry out carbonization treatment; carbon selenium material good up to stability, that selenium is uniformly dispersed, Se content is easily-controllable.Selenium in carbon selenium material mainly exists in the form of carbon selenium key and selenium selenium key, and stability is good, which is used as the electrode material of sodium-ion battery and sodium selenium cell, shows excellent chemical property.The carbon selenium material is efficiently synthesized under simple condition by a step high-temperature heat treatment, at low cost, low for equipment requirements, is conducive to industrialized production.
Description
Technical field
The present invention relates to a kind of carbon selenium material and its preparations and application, and in particular to using organic matter containing selenium as carbon source and selenium
The method that source generates carbon selenium material by a step pyroreaction, further relates to carbon selenium material as sodium-ion battery or sodium selenium cell etc.
The electrode material application of energy storage device, belongs to battery material technical field.
Background technique
Selenium resource distribution is extensive, and existence form diversification, furthermore selenium-containing compound has appearance structure controllable, and theory is held
It measures the advantages that high, the carbon that the composite material of especially selenium and cheap carbon mainly has selenium to adulterate, selenium/carbon composite.In recent years, these
Material has had a wide range of applications in fields such as lithium ion battery, sodium-ion battery, lithium selenium cell, sodium selenium cell and capacitors
Prospect.Although the Theoretical Mass specific capacity of selenium is lower than sulphur, relative to sulphur, selenium density with higher, therefore the theoretical body of selenium
Product energy density is suitable with the theoretical volumetric energy density of sulphur.Meanwhile compared with the sulphur almost to insulate, the selenium table of semiconductor property
Reveal preferable conductive capability, therefore, even if selenium can also be played higher in the battery system of high useful load and high areal density
Activity and utilization rate.Certainly, single selenium doped carbon or carbon selenium compound have some defects in practical applications: selenium contains
When measuring low, battery capacity is also low；It when Se content is high, is easy to be unevenly distributed, forms cluster, be that the performance of material is unstable；This
Main selenium simple substance to be used, is easy to appear shuttle effect during outer introducing selenium, so that the capacity of battery is decayed rapidly, circulation
Performance is unstable.Thus the preparation method to carbon selenium material is needed to improve, both makes to be evenly distributed, furthermore carbon selenium it
Between construct a certain amount of chemical bond, be conducive to alleviate shuttle effect of the material in stored energy application, and then obtain the performance of material
It is improved to great.Therefore the carbon material for finding suitable method preparation selenizing becomes the hot spot of a research.
Currently, prepare the method for carbon selenium material mainly using different carbon materials as carbon source, elemental selenium (CN105070892A,
CN104201349A, CN102078816A) it is used as selenium source, carbon selenium material is prepared by series reactions such as high temperature.These
Method first prepares carbon material, subsequent under a set of conditions to introduce selenium, and process is relative complex, and condition is harsh, and energy consumption is high.Selenium list
When matter introduces selenium, obtained product is easy unevenly, and is difficult to the shuttle effect for inhibiting energy storage device to occur in use,
The energy-storage property of material is promoted unobvious.
Summary of the invention
For existing carbon selenium material preparation process there are complex steps, condition are more demanding, carbon selenium is unevenly distributed, knot
Structure is unstable, lead to problems such as it is at high cost low with performance, the first purpose of this invention be to provide a kind of selenium be evenly distributed,
The easily-controllable carbon selenium material of stable structure, Se content.
Second object of the present invention is to be to provide a kind of mild condition, easy to operate, at low cost, low for equipment requirements
The method for preparing the carbon selenium material, this method is conducive to industrialized production.
Third object of the present invention is to be to provide a kind of application of carbon selenium material, and carbon selenium material can as electrode material
To obtain the high sodium-ion battery of good cycling stability, high rate performance or sodium selenium cell.
In order to achieve the above technical purposes, the present invention provides a kind of preparation method of carbon selenium material, this method is will to contain
Selenium organic matter be placed under protective atmosphere carry out carbonization treatment to get.
The present invention using organic matter containing selenium be and meanwhile as carbon source and selenium source, a series of complex occurs in high-temperature reaction process
Chemical reaction, the generation etc. including carburizing reagent and carbon selenium key, organic matter containing selenium is under protective gas atmosphere, partial
Deoxidation, carbonization form active centre, and active centre forms new carbon selenium key and carbon selenium long-chain in conjunction with the part selenium being broken simultaneously,
Be introduced into carbon structure to realize selenium stabilization, at the same in carbon selenium material selenium be selenium in-situ preparation in organic matter containing selenium and with
Carbon combines, and it is evenly dispersed in carbon selenium material to realize selenium.
Preferred scheme, the ratio between selenium atom and carbon atom >=1:6 in the organic compound containing selenium.It is preferably organic containing selenium
Compound includes benzo selenium phenol (C10H6Se2), polyselenophenes, and selenium phenol (C8H4Se3), 2,5- dicarboxyl selenium phenol, selenide
(C8H6Se3), at least one of tetramethyl tetraselenofulvalene.It is different according to the organic matter containing selenium of selection, under the conditions of identical carbonization
The carbon selenium material that different selenium contents can be obtained, may be implemented the Effective Regulation of selenium in carbon selenium material；It is preferred that selection selenium carbon
Atomic ratio is higher than 1:6 organic matter containing selenium, if selection selenium carbon atomic ratio is lower than the organic matter containing selenium of 1:6, after high temperature cabonization,
Se content is low or even cannot get carbon selenium material, it is difficult to meet sodium-ion battery or sodium selenium cell application requirement.
Preferred scheme, the condition of the carbonization treatment: under protective atmosphere, at a temperature of 400~800 DEG C, heat preservation 1~
8h.Protective atmosphere is generally the mixed gas of inert atmosphere or nitrogen or inert atmosphere and nitrogen.The temperature mistake of carbonization treatment
Low or excessively high or carbonization time is too long or the too short generation for being unfavorable for carbon selenium material, and temperature is excessively high or overlong time, is easy to lead
Carbon selenium key is caused to be broken and deselenization, and temperature is too low or the time is too short, is unfavorable for the generation of carbon selenium key, if not under protective atmosphere,
It cannot get carbon selenium material.Under suitable Carbonization Conditions, be conducive to the generation of carbon selenium material.Preferred carburizing temperature is 500~650
℃.Preferred carbonization time is 1~3h.
The carbon selenium material crude product that the present invention is prepared is washed to neutrality, then is centrifugated, and be dried in vacuo.From
The revolving speed of the heart is in 5000~10000r/min.Vacuum drying temperature is 50~100 DEG C, drying time 12h.
The present invention also provides a kind of carbon selenium materials, are obtained by the preparation method.
Preferred scheme, in the carbon selenium material selenium physics be coated on carbon material surface or and carbon with Covalent bonding together；Selenium
Mainly exist with selenium selenium key or selenium form of carbon bond.
Selenium mainly exists with carbon selenium bonding selenium selenium key-shaped formula in carbon selenium material of the invention, and selenium is incorporated in carbon by carbon selenium key
On material, the stability of material, and selenium in-situ preparation are substantially increased, stably dispersing solves in elemental selenium and carbon recombination process
The problems such as dispersion is uneven.
The present invention also provides the application of the carbon selenium material, as electrode material be applied to sodium-ion battery or
Sodium selenium cell.
Carbon selenium material of the invention is used to prepare sodium-ion battery: carbon selenium material, the carboxymethyl cellulose that will be prepared
Sodium (CMC), conductive carbon black 80:10:10 in mass ratio are uniformly mixed, and suitable deionized water are added, slurry is made and is applied to copper foil
On, being placed in a vacuum drying oven at 40-100 DEG C dry 4-12h after the solvent is volatilized can be obtained electrode used in sode cell.
Carbon selenium material of the invention is used to prepare sodium selenium cell: doing cathode, glass fibers with carbon selenium material for anode, metallic sodium
Dimension is diaphragm, the NaClO of 1M4As electrolyte, it is assembled into sodium selenium cell.
Compared with the prior art, technical solution of the present invention bring advantageous effects:
The present invention is used as carbon source and selenium source using organic matter containing selenium simultaneously, and organic carbon generates porous carbon materials skeleton, simultaneously
Selenium in-situ preparation, and be incorporated on carbon skeleton, carbon selenium material is obtained, organic matter containing selenium is common industrial chemicals, and raw material sources are wide,
It avoids and uses elemental selenium.
In carbon selenium material preparation process of the invention, carbon real-time formation synchronous with selenium, selenium element distribution in obtained material
Uniformly, and with carbon skeleton bonding action is formed.
Reaction condition is simple in carbon selenium material preparation process of the invention, and controllability is good, and material source is abundant, is conducive to work
Industry metaplasia produces；
In carbon selenium material preparation process of the present invention using organic selenides be used as direct material, to production equipment requirement it is low,
Preparation cost is cheap, economic value with higher；
The present invention can be by changing organic selenides, the type of polymer, reaction time, the conditional regulatories such as heating temperature
Se content in carbon selenium material help to obtain high performance carbon selenium material.
There are a large amount of carbon selenium keys in carbon selenium material structure of the invention, are conducive to the fixation of selenium element, while carbon selenium material
Material is porous material, improves the physics fixed function to selenium, and selenium can be firmly secured at very much between the hole of porous carbon materials, because
This, carbon selenium material be applied to sodium-ion battery or sodium selenium cell, can be well solved occur in electrode material use process fly
Shuttle effect, to show excellent chemical property.
Detailed description of the invention
[Fig. 1] is that the scanning electron microscope (SEM) photograph of carbon selenium material prepared by embodiment 1 and high-resolution project electron microscope；It can from Fig. 1
To see that carbon selenium material part is graphitized, and carbon selenium element is uniformly distributed.
[Fig. 2] is the XPS analysis figure of carbon selenium material prepared by embodiment 1；From can illustrate to generate in carbon selenium material in Fig. 2
Stable carbon selenium key.
[Fig. 3] is cycle performance figure of the carbon selenium material as the electrode material of sode cell in embodiment 5；It can be with from Fig. 3
Find out and circulate in 200 times or more, capacity is able to maintain in 300mAh g-1More than；
[Fig. 4] is CV curve of the carbon selenium material as sodium selenium cell in embodiment 6；As can be seen from Figure 4 there is obvious selenium
Redox peaks；
[Fig. 5] is high rate performance figure of the sodium selenium cell of carbon selenium material assembling in embodiment 6 under different current densities；Figure
5 illustrate carbon selenium material as sodium selenium cell electrode material, and the sodium selenium cell of preparation is under high current density, and high rate performance is still very
It is high.
Specific embodiment
The content of present invention is described further with reference to embodiments, without will form the limit to the scope of the present invention
System.
Embodiment 1
With benzo selenium phenol (C10H6Se2) raw material prepares carbon selenium material
By benzo selenium phenol, 0.5-2h is kept under atmosphere of inert gases, is gradually warming up to 500 DEG C, and protect at such a temperature
1h is held, after reaction, Temperature fall to room temperature.Then its product is washed to neutrality, the substance obtained after centrifugation exists
10h is dried at 70 DEG C of vacuum, carbon selenium material as shown in Figure 1 can be obtained.It can be seen that gained carbon selenium material is piece from Fig. 1 a
Shape structure projects electron microscope from the high-resolution of Fig. 1 b, it is further known that the carbon of the graphited selenizing in part has been prepared in we
Material, Fig. 1 c, element Surface scan are analyzed each element in the material and are uniformly distributed.
According to the operating procedure and condition of embodiment 1, different Organic Ingredients are selected, it is as a result as follows to prepare carbon selenium material
Shown in table 1:
The contrast table of the reaction result of the different starting materials of table 1
Embodiment 2
Carbon selenium material is prepared in the case where sealing environment by raw material of polyselenophenes
Polyselenophenes are placed under tube sealing environment, are gradually warming up to 650 DEG C, and keep 2h at such a temperature, after reaction,
Temperature fall is to room temperature.Then its product is washed to neutrality, the substance obtained after centrifugation is dried at 65 DEG C of vacuum
High-carbon selenium material can be obtained in 12h.Fig. 2, for the XPS map of the material.
Embodiment 3
With the scheme of embodiment 1, when reaction temperature is set as 400 DEG C, 600 DEG C and 700 DEG C by we, under the conditions of same
Se content gradually decreases in the carbon selenium material of preparation.
Embodiment 4
With the scheme of embodiment 1, when we are extending heating time to 3h, under the conditions of same, the carbon of obtained selenizing
Se content reduces 3/5ths in material.
Embodiment 5
Material obtained in embodiment 1 is assembled into sodium-ion battery, cathode is done for anode, metallic sodium with the material, is gathered
Propylene is diaphragm, the NaClO of 1M4Do electrolyte.It is preferable that electrochemical property test shows that the material has for sodium-ion battery
Chemical property, in 0.1A g-1Current density under, capacity is up to 400mAh g-1；In 0.1A g-1Current density under
After circulation 200 times, reversible specific capacity is still up to 320mAh g-1, which also shows good cycle performance.
Embodiment 6
Material obtained in embodiment 2 is assembled into sodium selenium cell, cathode, glass are done for anode, metallic sodium with the material
Fiber is diaphragm, the NaClO of 1M4Do electrolyte.It is preferable that electrochemical property test shows that the material has for sodium selenium cell
Chemical property has apparent redox peaks in CV curve, in 0.1A g-1Current density under, capacity is up to 450mAh
g-1；In 3.2A g-1Current density under, reversible specific capacity still be up to 260mAh g-1, which also shows good
High rate performance.
Claims (7)
1. a kind of preparation method of carbon selenium material, it is characterised in that: selenium organic matter will be contained be placed under protective atmosphere and carry out at carbonization
Reason to get.
2. a kind of preparation method of carbon selenium material according to claim 1, it is characterised in that: selenium in the organic matter containing selenium
The ratio between atom and carbon atom >=1:6.
3. a kind of preparation method of carbon selenium material according to claim 2, it is characterised in that: the organic compound containing selenium
Including benzo selenium phenol, polyselenophenes and at least one of selenium phenol, 2,5- dicarboxyl selenium phenol, selenide, tetramethyl tetraselenofulvalene.
4. the preparation method of described in any item a kind of carbon selenium materials according to claim 1~3, it is characterised in that: the carbonization
The condition of processing: under protective atmosphere, at a temperature of 400~800 DEG C, 1~8h is kept the temperature.
5. a kind of carbon selenium material, it is characterised in that: obtained by any one of Claims 1 to 4 preparation method.
6. a kind of carbon selenium material according to claim 5, it is characterised in that: selenium physics is coated on carbon in the carbon selenium material
Material surface or and carbon with Covalent bonding together；Selenium mainly exists with selenium selenium key or selenium form of carbon bond.
7. the application of carbon selenium material described in claim 5 or 6, it is characterised in that: be applied to sodium ion electricity as electrode material
Pond or sodium selenium cell.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109817920A (en) * | 2019-01-22 | 2019-05-28 | 陕西科技大学 | A kind of preparation method and application of selenium enveloped carbon nanometer tube/graphene |
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| CN104201349A (en) * | 2014-08-13 | 2014-12-10 | 东南大学 | Preparation method of selenium-carbon electrode material with porous structure and application of selenium-carbon electrode material |
| CN105070892A (en) * | 2015-09-22 | 2015-11-18 | 中国科学院化学研究所 | Preparation method and application of selenium-carbon compound |
| CN108183224A (en) * | 2017-12-30 | 2018-06-19 | 武汉理工大学 | Porous nucleocapsid carbon/selenium composite material of a kind of original position nitrating and its preparation method and application |
| CN108502844A (en) * | 2018-04-12 | 2018-09-07 | 武汉理工大学 | A kind of carbon selenium composite material, lithium selenium cell anode and application |
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| CN104201349A (en) * | 2014-08-13 | 2014-12-10 | 东南大学 | Preparation method of selenium-carbon electrode material with porous structure and application of selenium-carbon electrode material |
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| CN108183224A (en) * | 2017-12-30 | 2018-06-19 | 武汉理工大学 | Porous nucleocapsid carbon/selenium composite material of a kind of original position nitrating and its preparation method and application |
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| CN109817920A (en) * | 2019-01-22 | 2019-05-28 | 陕西科技大学 | A kind of preparation method and application of selenium enveloped carbon nanometer tube/graphene |
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