CN108565420A - Co is carried on the material, preparation method and application of MIL-101 - Google Patents
Co is carried on the material, preparation method and application of MIL-101 Download PDFInfo
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- CN108565420A CN108565420A CN201810308096.6A CN201810308096A CN108565420A CN 108565420 A CN108565420 A CN 108565420A CN 201810308096 A CN201810308096 A CN 201810308096A CN 108565420 A CN108565420 A CN 108565420A
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
A kind of Co is carried on the material, preparation method and application of MIL 101, is related to lithium battery material technical field.The Co is carried on the preparation method of the material of MIL 101 comprising following preparation process：After cobalt salt and MIL 101 are mixed plus water uses ultrasonication, is subsequently agitated for obtaining mixed liquor；Sodium borohydride solution is instilled into mixed liquor, is filtered, washed, is dried after stirring evenly.The preparation method has simple process and low cost, the advantages of being suitable for industrialized production, the material with bigger serface, high charge-discharge specific capacity can be prepared.In addition the invention further relates to above-mentioned Co to be carried on the material of MIL 101 and its application in preparing lithium cell cathode material.
Description
Technical field
The present invention relates to a kind of lithium battery material technical field, and more particularly to a kind of Co be carried on MIL-101 material,
Preparation method and application.
Background technology
Lithium ion battery (LIBs) has been widely used in every field as new generation of green high-power rechargeable battery,
Have many advantages, such as that voltage is high, energy density is big, good cycle, self discharge are small, memory-less effect.The lithium being widely used at present
Ion battery cathode material is carbon material, because its theoretical capacity relatively low (372mAh/g) cannot be satisfied the demand of the following application,
Therefore it is imperative to improve its performance to be used as electrode material for exploitation new material.Metal-organic framework is as molecule micropore
Material has that synthesis condition is mild, structure diversification, specific surface area are high and the advantages such as chemical property is controllable are in lithium electricity electricity
Huge potentiality are presented in the research of pole material.
Metal-organic framework materials (MOFs) are to pass through coordinate bond self assembly shape by organic ligand and metal ion or cluster
At the hybrid inorganic-organic materials with molecule inner pore, in metal-organic framework materials, due to organic ligand and gold
The arrangement for belonging to ion or cluster has apparent directionality to form different frame pore structures, so that it is shown different
Absorption property, optical property and electromagnetic property, this makes metal-organic framework materials in hydrogen storage, gas absorption and divides
From, sensor, medicament slow release, the obtained certain application in fields such as catalysis reaction, but the electric conductivity of MOFs is poor, this is tight
Weight limits its application in field of lithium.
Therefore, the application is intended to provide a kind of MOFs materials with excellent lithium cell cathode material performance and its preparation
Method.
Invention content
The purpose of the present invention is to provide the materials that a kind of Co is carried on MIL-101, with charging and discharging capacity height, follow
The advantage that ring stability is good and cyclical stability is strong.
Another object of the present invention is to provide the preparation methods that above-mentioned Co is carried on the material of MIL-101, with work
Skill is simple, it is at low cost, be suitable for the advantages of industrialized production.
Another object of the present invention is to provide above-mentioned Co to be carried on the material of MIL-101 in lithium cell cathode material
Using.
The present invention solves its technical problem using following technical scheme to realize.
A kind of Co is carried on the preparation method of the material of MIL-101 comprising following preparation process：
After cobalt salt and MIL-101 are mixed plus water uses ultrasonication, is subsequently agitated for obtaining mixed liquor；
Sodium borohydride solution is instilled into mixed liquor, is filtered, washed, is dried after stirring evenly.
Further, in a preferred embodiment of the present invention, the preparation method of MIL-101 is：By chromic salts, terephthalic acid (TPA),
Hydrofluoric acid and water are mixed evenly, and filter, wash after being reacted 6-8 hours at 180-220 DEG C, then stir in ethanol successively
Mix 18-24 hours, in NH4It is stirred 4-6 hours at 50-60 DEG C in F solution, washing, drying.
Further, in a preferred embodiment of the present invention, the molar ratio of chromic salts, terephthalic acid (TPA), hydrofluoric acid and water is 1：
1-2：1-2：280-300.
Further, in a preferred embodiment of the present invention, the mass ratio of cobalt salt and MIL-101 are 3-5：1.
Further, in a preferred embodiment of the present invention, cobalt salt is cobalt nitrate.
Further, in a preferred embodiment of the present invention, the time of ultrasonication is 20-60min.
Further, in a preferred embodiment of the present invention, the time of stirring is 3-6h.
Further, in a preferred embodiment of the present invention, the time stirred evenly is 3-6h.
The present invention also provides the material that a kind of Co is carried on MIL-101, obtained using above-mentioned preparation method.
The present invention also provides above-mentioned Co to be carried on application of the material of MIL-101 in lithium cell cathode material.
The Co of the embodiment of the present invention is carried on the material preparation method of MIL-101 and the advantageous effect of application：This hair
The preparation method for the material that the Co that bright embodiment provides is carried on MIL-101 includes following preparation process：By cobalt salt and MIL-101
After mixing plus water uses ultrasonication, is subsequently agitated for obtaining mixed liquor；Sodium borohydride solution is instilled into mixed liquor, stirring is equal
It is filtered, washed, dries after even.The preparation method has simple process and low cost, the advantages of being suitable for industrialized production, can
The material with bigger serface, high charge-discharge specific capacity is prepared.In addition the invention further relates to above-mentioned Co to be carried on MIL-
Application of 101 material in lithium cell cathode material.
Description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the TEM figures for the material that MIL-101 is prepared in the embodiment of the present invention 1；
Fig. 2 is the TEM figures that the embodiment of the present invention 1 is prepared that Co is carried on the material of MIL-101；
Fig. 3 is that the CV curves that Co is carried on the material of MIL-101 are prepared in the embodiment of the present invention 1；
Fig. 4 is that the charged/discharged voltage curve that Co is carried on the material of MIL-101 is prepared in the embodiment of the present invention 1；
Fig. 5 is that the embodiment of the present invention 1 is prepared in lower 100 cycles of 200mA/g for the material that Co is carried on MIL-101
Cycle performance and corresponding CE；
Fig. 6 is that the curve of double curvature that Co is carried on the material of MIL-101 is prepared in the embodiment of the present invention 1；
Fig. 7 is the electrochemical impedance spectroscopy of CoO@MIL-101 (Cr), CoO and MIL-101 (Cr) prepared by the embodiment of the present invention
Figure.
Specific implementation mode
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
The material preparation method of MIL-101 is carried on to the Co of the embodiment of the present invention below and application carries out specifically
It is bright.
A kind of Co is carried on the preparation method of the material of MIL-101 comprising following preparation process：
After cobalt salt and MIL-101 are mixed plus water uses ultrasonication, is subsequently agitated for obtaining mixed liquor；Preferably,
The preparation method of MIL-101 is：Chromic salts, terephthalic acid (TPA), hydrofluoric acid and water are mixed evenly, it is anti-at 180-220 DEG C
It filters, wash after answering 6-8 hours, then stir 18-24 hours in ethanol successively, in NH4It is stirred at 50-60 DEG C in F solution
It mixes 4-6 hours, washing, drying；Preferably, the molar ratio of chromic salts, terephthalic acid (TPA), hydrofluoric acid and water is 1：1-2：1-2：280-
300；Preferably, the mass ratio of cobalt salt and MIL-101 are 3-5：1；Preferably, cobalt salt is cobalt nitrate；Preferably, ultrasonication
Time be 20-60min；Preferably, the time of stirring is 3-6h；Preferably, the time stirred evenly is 3-6h.
Sodium borohydride solution is instilled into mixed liquor, is filtered, washed, is dried after stirring evenly.
The preparation method that Co provided in an embodiment of the present invention is carried on the material of MIL-101 uses chromic salts, to benzene two first
Formic acid, hydrofluoric acid and water reaction synthesis large specific surface area, the metal-organic framework materials MIL-101 for having porosity characteristic, then will
Metal-organic framework materials MIL-101 is uniformly mixed as after carrier and presoma cobalt salt high degree of dispersion, and uses reducing agent
NaBH4By Co2+Co nanometer particle loads are reduced on metal-organic framework materials MIL-101, to overcome the organic bone of metal
The problem of frame material poorly conductive, obtains the material that the Co with excellent cyclical stability and high rate performance is carried on MIL-101
The advantages of material, above-mentioned preparation method has simple process and low cost, is suitable for industrialized production.
The present invention also provides the material that a kind of Co is carried on MIL-101, obtained using above-mentioned preparation method, tool
Have the advantages that high charging and discharging capacity, good cycling stability and cyclical stability are strong.
The present invention also provides above-mentioned Co to be carried on application of the material of MIL-101 in lithium cell cathode material.This
The method that the Co that invention provides is carried on the material use in-situ reducing Metal Supported of MIL-101, allows two kinds of materials of MIL-101 and Co
Material reaches uniform combination, functionally realizes that complementary and collaboration effect, Co nano-particles can improve the conduction of MIL-101
Property and the low problem of specific capacity, and the metal-organic framework materials MIL-101 as supporter can then greatly increase following for Co
Ring stability provides a 3D for Co nano-particles and supports protective shell, prevents Co nano-particles from having Li+Embedded and abjection mistake
Dusting and aggregation in journey, to obtain the height ratio capacity that high-energy density electrode material is brought, while the material also show it is excellent
Different cyclical stability and high rate performance.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
An embodiment of the present invention provides the materials that a kind of Co is carried on MIL-101, are prepared using following steps：
By Cr (NO3)3And terephthalic acid (TPA), hydrofluoric acid, deionized water press 1：1：1：300 molar ratio mixing, stirs evenly
Being added to 50mL afterwards has in the stainless steel cauldron of polytetrafluoroethyllining lining, reacts 8h at 200 DEG C, and obtained green is suspended
Liquid filters, washing obtains green solid object, by obtained green solid object in absolute ethyl alcohol magnetic agitation for 24 hours, then in NH4F
It washs after being stirred 6 hours at 60 DEG C in (30mM) solution, be dried in vacuo at 80 DEG C, obtain MIL-101 green powders；
It weighs the above-mentioned MIL-101 of 200mg to be added in 30mL deionized waters, ultrasonication 20min, 600mg is added
Co (NO3)2, magnetic agitation 5h obtains mixed liquor, then by the NaBH of 150.0mg4Solid be dissolved in 10mL deionized waters after by
It is added dropwise in above-mentioned mixed liquor, continues to stir 5h after being added dropwise, after product is filtered, washed under 80 DEG C and vacuum condition
It is dried overnight, obtains metal composite nano lithium cell cathode material Co@MIL-101.
Embodiment 2
An embodiment of the present invention provides the materials that a kind of Co is carried on MIL-101, are prepared using following steps：
By Cr (NO3)3And terephthalic acid (TPA), hydrofluoric acid, deionized water press 1：1.1：1.1：280 molar ratio mixing, stirring
It is added in the stainless steel cauldron of polytetrafluoroethyllining lining after uniformly, reacts 7h at 210 DEG C, obtained green is suspended
Liquid filters, washing obtains green solid object, by obtained green solid object in absolute ethyl alcohol magnetic agitation 22h, then in NH4F
It washs after being stirred 5 hours at 50 DEG C in (30mM) solution, be dried in vacuo at 70 DEG C, obtain MIL-101 green powders；
It weighs the above-mentioned MIL-101 of 200mg to be added in 30mL deionized waters, ultrasonication 30min, 650mg is added
Co (NO3)2, magnetic agitation 4h obtains mixed liquor, then by the NaBH of 140.0mg4Solid be dissolved in 10mL deionized waters after by
It is added dropwise in above-mentioned mixed liquor, continues to stir 4h after being added dropwise, after product is filtered, washed under 70 DEG C and vacuum condition
It is dried overnight, obtains metal composite nano lithium cell cathode material Co@MIL-101.
Embodiment 3
An embodiment of the present invention provides the materials that a kind of Co is carried on MIL-101, are prepared using following steps：
By Cr (NO3)3And terephthalic acid (TPA), hydrofluoric acid, deionized water press 1：1.2：1.2：290 molar ratio mixing, stirring
It is added in the stainless steel cauldron of polytetrafluoroethyllining lining after uniformly, reacts 6h at 190 DEG C, the green suspension that will be obtained
Filter, washing obtains green solid object, by obtained green solid object in absolute ethyl alcohol magnetic agitation 18h, then in NH4F
It washs after being stirred 5 hours at 60 DEG C in (30mM) solution, be dried in vacuo at 70 DEG C, obtain MIL-101 green powders；
It weighs the above-mentioned MIL-101 of 200mg to be added in 30mL deionized waters, ultrasonication 40min, 700mg is added
Co (NO3)2, magnetic agitation 4.5h obtains mixed liquor, then by the NaBH of 200.0mg4After solid is dissolved in 20mL deionized waters
It is added dropwise in above-mentioned mixed liquor, continues to stir 6h after being added dropwise, in 80 DEG C and vacuum condition after product is filtered, washed
Under be dried overnight, obtain metal composite nano lithium cell cathode material Co@MIL-101.
Embodiment 4
An embodiment of the present invention provides the materials that a kind of Co is carried on MIL-101, are prepared using following steps：
By Cr (NO3)3And terephthalic acid (TPA), hydrofluoric acid, deionized water press 1：1.05：1.05：300 molar ratio mixing, is stirred
It is added in the stainless steel cauldron of polytetrafluoroethyllining lining after mixing uniformly, reacts 6h at 220 DEG C, obtained green is hanged
Turbid filter, washing obtain green solid object, by obtained green solid object in absolute ethyl alcohol magnetic agitation for 24 hours, then
NH4It washs after being stirred 6 hours at 50 DEG C in F (40mM) solution, be dried in vacuo at 80 DEG C, obtain MIL-101 green powders；
It weighs the above-mentioned MIL-101 of 200mg to be added in 30mL deionized waters, ultrasonication 20min, 800mg is added
Co (NO3)2, magnetic agitation 6h obtains mixed liquor, then by the NaBH of 300.0mg4Solid be dissolved in 20mL deionized waters after by
It is added dropwise in above-mentioned mixed liquor, continues to stir 6h after being added dropwise, after product is filtered, washed under 80 DEG C and vacuum condition
It is dried overnight, obtains metal composite nano lithium cell cathode material Co@MIL-101.
Embodiment 5
An embodiment of the present invention provides the materials that a kind of Co is carried on MIL-101, are prepared using following steps：
By Cr (NO3)3And terephthalic acid (TPA), hydrofluoric acid, deionized water press 1：1.3：1.3：300 molar ratio mixing, stirring
It is added in the stainless steel cauldron of polytetrafluoroethyllining lining after uniformly, reacts 5h at 210 DEG C, obtained green is suspended
Liquid filters, washing obtains green solid object, by obtained green solid object in absolute ethyl alcohol magnetic agitation 20h, then in NH4F
It washs after being stirred 5 hours at 55 DEG C in (30mM) solution, be dried in vacuo at 70 DEG C, obtain MIL-101 green powders；
It weighs the above-mentioned MIL-101 of 100mg to be added in 20mL deionized waters, ultrasonication 60min, 300mg is added
Co (NO3)2, magnetic agitation 5h obtains mixed liquor, then by the NaBH of 200.0mg4Solid be dissolved in 20mL deionized waters after by
It is added dropwise in above-mentioned mixed liquor, continues to stir 6h after being added dropwise, after product is filtered, washed under 70 DEG C and vacuum condition
It is dried overnight, obtains metal composite nano lithium cell cathode material Co@MIL-101.
The material that the MIL-101 materials and Co be prepared to the embodiment of the present invention 1 is carried on MIL-101 carries out TEM electricity
Microscopy is surveyed, and testing result is as depicted in figs. 1 and 2, shows that the Co is carried in the material of MIL-101 that there are Co, it was demonstrated that Co has become
It is carried on MIL-101 to work(；In addition the MIL-101 materials and Co CoO, embodiment 1 being prepared are carried on MIL-101's
Material carries out electro-chemical test, as a result as shown in Fig. 3, Fig. 4, Fig. 5, Fig. 6 and Fig. 7, the results showed that：The Co is carried on MIL-101
The charging and discharging capacity of material can reach 810mAh/g, significantly larger than use the charging and discharging capacity of pure MIL-101
(84mAh/g), while the material also shows excellent cyclical stability and high rate performance, has and is applied to lithium ion battery anode material
Foreground in material.
In conclusion the material that the Co of the embodiment of the present invention is carried on MIL-101 has bigger serface, high charge-discharge ratio
Capacity, excellent cyclical stability and high rate performance；The preparation method that the Co is carried on the material of MIL-101 has technique letter
It is single, at low cost, the advantages of being suitable for industrialized production.The material that the Co is carried on MIL-101 has in lithium cell cathode material
The foreground of middle application.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of Co is carried on the preparation method of the material of MIL-101, which is characterized in that it includes following preparation process：
After cobalt salt and MIL-101 are mixed plus water uses ultrasonication, is subsequently agitated for obtaining mixed liquor；
Sodium borohydride solution is instilled into the mixed liquor, is filtered, washed, dries after stirring evenly.
2. Co according to claim 1 is carried on the preparation method of the material of MIL-101, which is characterized in that the MIL-
101 preparation method is：Chromic salts, terephthalic acid (TPA), hydrofluoric acid and water are mixed evenly, react 6-8 at 180-220 DEG C
It is filtered after hour, washing, then stirs 18-24 hours in ethanol successively, in NH4In F solution 4-6 is stirred at 50-60 DEG C
Hour, washing, drying.
3. Co according to claim 2 is carried on the preparation method of the material of MIL-101, which is characterized in that the chromic salts,
The molar ratio of the terephthalic acid (TPA), the hydrofluoric acid and the water is 1：1-2：1-2：280-300.
4. Co according to claim 1 is carried on the preparation method of the material of MIL-101, which is characterized in that the cobalt salt
Mass ratio with the MIL-101 is 3-5：1.
5. Co according to claim 1 is carried on the preparation method of the material of MIL-101, which is characterized in that the cobalt salt
For cobalt nitrate.
6. Co according to claim 1 is carried on the preparation method of the material of MIL-101, which is characterized in that the ultrasound
The time of wave processing is 20-60min.
7. Co according to claim 1 is carried on the preparation method of the material of MIL-101, which is characterized in that the stirring
Time be 3-6h.
8. Co according to claim 1 is carried on the preparation method of the material of MIL-101, which is characterized in that the stirring
The uniform time is 3-6h.
9. a kind of Co is carried on the material of MIL-101, which is characterized in that use as described in any one of claim 1-8 in fact
Preparation method obtain.
10. Co according to claim 9 is carried on application of the material of MIL-101 in lithium cell cathode material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810308096.6A CN108565420A (en) | 2018-04-08 | 2018-04-08 | Co is carried on the material, preparation method and application of MIL-101 |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810308096.6A CN108565420A (en) | 2018-04-08 | 2018-04-08 | Co is carried on the material, preparation method and application of MIL-101 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113451556A (en) * | 2021-05-18 | 2021-09-28 | 天津空间电源科技有限公司 | Low-temperature lithium ion battery |
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|---|---|---|---|---|
| CN105233878A (en) * | 2015-11-11 | 2016-01-13 | 北京林业大学 | Synthesis method for metal-loaded-type MIL-101 bio-oil hydrogenation catalyst |
| CN106883419A (en) * | 2017-01-19 | 2017-06-23 | 湖北大学 | A kind of fast synthesis method of cobalt-based metal-organic framework materials and its application |
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2018
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|---|---|---|---|---|
| CN105233878A (en) * | 2015-11-11 | 2016-01-13 | 北京林业大学 | Synthesis method for metal-loaded-type MIL-101 bio-oil hydrogenation catalyst |
| CN106883419A (en) * | 2017-01-19 | 2017-06-23 | 湖北大学 | A kind of fast synthesis method of cobalt-based metal-organic framework materials and its application |
| CN107732248A (en) * | 2017-11-21 | 2018-02-23 | 盐城工学院 | The MOF materials of negative electrode of lithium ion battery and its application |
Non-Patent Citations (1)
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| 陈玉贞: "基于金属-有机骨架纳米复合材料的设计、合成与催化性能研究", 《中国博士学位论文全文数据库-工程科技Ⅰ辑》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113451556A (en) * | 2021-05-18 | 2021-09-28 | 天津空间电源科技有限公司 | Low-temperature lithium ion battery |
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