CN109817918A - Sulfur doping MXene composite material and preparation method and application - Google Patents
Sulfur doping MXene composite material and preparation method and application Download PDFInfo
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- CN109817918A CN109817918A CN201910057080.7A CN201910057080A CN109817918A CN 109817918 A CN109817918 A CN 109817918A CN 201910057080 A CN201910057080 A CN 201910057080A CN 109817918 A CN109817918 A CN 109817918A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a kind of sulfur doping MXene composite material and preparation methods, the following steps are included: MXene and sulphur source are that 1:1~20 is added in deionized water according to mass ratio by (1), it stirs and heats, be configured to the mixed liquor that concentration is 5-80mg/ml；(2) mixed liquor immigration reaction kettle is heated to 80-200 DEG C, reacts 4-36h, then cools to room temperature；(3) product that step (2) obtains is washed and is centrifuged with detergent, then be dried in vacuo, obtain the sulfur doping MXene composite material.The advantages that MXene composite material of sulfur doping prepared by the present invention has structural stability height, stable cycle performance, and charge and discharge coulombic efficiency is high, embedding/de- potassium current potential of the negative electrode material being prepared into is moderate, and cycle performance and high rate performance are good.
Description
Technical field
The invention belongs to new energy materials fields, and in particular to a kind of preparation method of sulfur doping MXene composite material and
Its application in kalium ion battery.
Background technique
With the high speed development of modern society, traditional energy is increasingly depleted, and finding new clean energy resource becomes more urgent.
For lithium ion battery because of its good chemical stability and chemical property, being exactly since be born can charge and discharge field of batteries core side
To, however the storage of lithium is limited, exploitation difficulty is larger, it is difficult to be widely applied.For find lithium ion battery substitute, chemically
Matter is close, and the bigger potassium of storage capacity starts the interest for causing researcher.Have for the research of high-performance kalium ion battery cathode
Important scientific meaning.
Potassium ion radius is greater than lithium ion radius, and traditional commercial graphite electrode interlamellar spacing is smaller without being able to satisfy potassium ion
Quick deintercalation, MXene material is similar to " page shape " as a kind of New Two Dimensional stratified material.The material has good lead
Electrically, higher specific surface area is suitable as kalium ion battery negative electrode material.But simple MXene material is used as potassium ion electricity
Pond negative electrode material, performance are still unsatisfactory.Interlamellar spacing can be increased by carrying out sulfur doping to MXene, optimization potassium ion expands
Channel is dissipated, to improve the chemical property of kalium ion battery.
Summary of the invention
In view of the problems of the existing technology, one of the objects of the present invention is to provide a kind of sulfur doping MXene composite woods
Material.Another object of the present invention is to provide the preparation methods of above-mentioned sulfur doping MXene composite material.Further, of the invention
A kind of application of sulfur doping MXene composite material is provided, the sulfur doping MXene composite material is born as kalium ion battery
Pole.
The invention adopts the following technical scheme:
A kind of preparation method of sulfur doping MXene composite material, comprising the following steps:
It (1) is that 1:1~20 (such as 1:2~15,1:5~10,1:6~8) addition is gone according to mass ratio by MXene and sulphur source
In ionized water, stir and heat, be configured to concentration be 5-80mg/ml (such as 10,15,20,25,30,35,40,45,50,55,
60,65,70,75mg/ml) mixed liquor；
(2) mixed liquor immigration reaction kettle is heated to 80-200 DEG C of (such as 80 DEG C, 90 DEG C, 100 DEG C, 110 DEG C, 120
DEG C, 130 DEG C, 140 DEG C, 150 DEG C, 160 DEG C, 170 DEG C, 180 DEG C, 190 DEG C, 200 DEG C), reaction 4-36h (such as 4,5,6,7,8,
9,10,12,14,16,18,20,22,24,26,28,30,32,34,36h), it then cools to room temperature；
(3) product that step (2) obtains is washed and is centrifuged with detergent, then be dried in vacuo, obtained described
Sulfur doping MXene composite material.
Further, the sulphur source is at least one of diphenyl sulfide, 2- benzene ethyl mercaptan, preferably diphenyl sulfide, preferred mass
Than for (2~5): 1 diphenyl sulfide and 2- benzene ethyl mercaptan.
Further, the MXene is Ti3C2Tx、Mo3C2Tx、V3C2Tx、Ti3N2Tx、Mo3N2Tx、V3N2TxOne of or
It is a variety of.
Further, sulfur doping amount is 1wt%-20wt%, preferably 2wt%- in the sulfur doping MXene composite material
12wt%.
Further, in the sulfur doping MXene composite material sulfur doping amount be 3wt%-15wt% (such as 3.5,4.5,
5.5,6.5,7.5,8.5,9.5,10.5,11.5,12.5,13.5,14.5wt%).
Further, the detergent is at least one of deionized water and ethyl alcohol, such as with deionized water and ethyl alcohol
Alternately washing 2~6 times, such as 3 times.
Further, the revolving speed that centrifugation uses in step (3) is 3000-3500r/min, such as 3200r/min, is centrifuged 2-
4min。
Further, vacuum drying temperature is 50-70 DEG C in step (3), and preferably 60 DEG C, drying time is 8-24h (example
Such as 8,9,10,11,12,13,14,15,16,17,18,19,20,21,22,23, for 24 hours), vacuum degree is no more than 135Pa, such as not
More than 133Pa, such as no more than 125,115,105,95,85Pa.
A kind of sulfur doping MXene composite material that the preparation method of sulfur doping MXene composite material is prepared.
The sulfur doping MXene composite material is used for kalium ion battery by a kind of application of sulfur doping MXene composite material
Cathode.
Beneficial effects of the present invention:
(1) the MXene composite material of sulfur doping prepared by the present invention is high with structural stability, stable cycle performance, times
The advantages that rate performance is good, and charge and discharge coulombic efficiency is high, the negative electrode material being prepared into is embedding/de- potassium current potential is moderate, cycle performance and
High rate performance is good；
(2) preparation method of the invention is simple, and element sulphur doping is controllable, is suitble to large-scale application.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph in comparative example 1 undoped with MXene material；
Fig. 2 is the scanning electron microscope (SEM) photograph of sulfur doping MXene composite material in embodiment 1；
Fig. 3 is the cycle performance figure that sulfur doping MXene composite material does kalium ion battery cathode in embodiment 1；
Fig. 4 is the cycle performance figure for doing kalium ion battery cathode in comparative example 1 undoped with MXene material.
Specific embodiment
In order to preferably explain the present invention, it is described further now in conjunction with following specific embodiments, but the present invention is unlimited
In specific embodiment.
Embodiment 1
A kind of preparation method of sulfur doping MXene composite material, comprising the following steps:
(1) Ti of 0.1g is weighed3C2TxIt is add to deionized water with the diphenyl sulfide of 0.1g, is heated to 50 DEG C and magnetic force stirs
It mixes 1 hour, obtains mixed liquor.
(2) mixed liquor is moved into reaction kettle sealing, rear to place in baking oven, adjusting reaction temperature is 80 DEG C, and the reaction time is
4h。
(3) by alternately washing 3 times of obtained product deionized water and ethyl alcohol, and under the centrifugal speed of 3000r/min
It is centrifuged 2min, is finally putting into vacuum oven, dry 8h at 60 DEG C.
(4) prepared by kalium ion battery cathode: by resulting sulfur doping MXene and Kynoar binder, carbon black, by matter
Amount is mixed than the ratio for being 8:1:1, and suitable N-Methyl pyrrolidone is added, and is mixing uniformly to form slurry coated in collector
On, after vacuum dried, slice, sulfur doping MXene battery cathode is made.
(5) Fig. 1 shows that undoped with MXene be " accordion " pattern, and after doping, Fig. 2 is MXene after the present embodiment doping
Pattern.MXene specific surface area after doping is 172m2/ g, interlamellar spacing 0.71nm, sulphur atom content is 1%, much larger than not mixing
Specific surface area (the 40.8m of miscellaneous MXene2/ g), interlamellar spacing (0.64nm)；Fig. 3 shows the MXene of the present embodiment doping in 100mA/
Under the current density of g, it is Fig. 4 undoped with MXene kalium ion battery cathode that the reversible capacity after 100 circle of circulation, which is 251mAh/g,
2.6 times of reversible capacity (93.8mAh/g).
Embodiment 2
A kind of preparation method of sulfur doping MXene composite material, comprising the following steps:
(1) Ti of 0.2g is weighed3C2TxIt is add to deionized water with the diphenyl sulfide of 2g, is heated to 60 DEG C, magnetic agitation 3
Hour, obtain mixed liquor.
(2) mixed liquor is moved into reaction kettle sealing, rear to place in baking oven, adjusting reaction temperature is 160 DEG C, and the reaction time is
18h。
(3) by alternately washing 3 times of obtained product deionized water and ethyl alcohol, and under the centrifugal speed of 3250r/min
It is centrifuged 3min, is finally putting into vacuum oven, dry 16h at 60 DEG C.
(4) prepared by kalium ion battery cathode: by resulting sulfur doping MXene and Kynoar binder, carbon black, by matter
Amount is mixed than the ratio for being 8:1:1, and suitable N-Methyl pyrrolidone is added, and is mixing uniformly to form slurry coated in collector
On, after vacuum dried, slice, sulfur doping MXene battery cathode is made.
(5) the MXene specific surface area after the present embodiment doping is 365m2/ g, interlamellar spacing 0.82nm, sulphur atom content are
10%, much larger than the specific surface area (40.8m undoped with MXene2/ g), interlamellar spacing (0.64nm)；The MXene of the present embodiment doping
Under the current density of 100mA/g, circulation 100 circle after reversible capacity be 363mAh/g, be undoped with MXene potassium ion electricity
3.8 times of pond cathode (93.8mAh/g).
Embodiment 3
A kind of preparation method of sulfur doping MXene composite material, comprising the following steps:
(1) Ti of 0.5g is weighed3C2TxIt is add to deionized water with the diphenyl sulfide of 10g, is heated to 70 DEG C, magnetic agitation 5
Hour, obtain mixed liquor.
(2) mixed liquor is moved into reaction kettle sealing, rear to place in baking oven, adjusting reaction temperature is 200 DEG C, and the reaction time is
36h。
(3) by alternately washing 3 times of obtained product deionized water and ethyl alcohol, and under the centrifugal speed of 3500r/min
It is centrifuged 4min, is finally putting into vacuum oven, is dried for 24 hours at 60 DEG C.
(4) prepared by kalium ion battery cathode: by resulting sulfur doping MXene and Kynoar binder, carbon black, by matter
Amount is mixed than the ratio for being 8:1:1, and suitable N-Methyl pyrrolidone is added, and is mixing uniformly to form slurry coated in collector
On, after vacuum dried, slice, sulfur doping MXene battery cathode is made.
(5) the MXene specific surface area after the present embodiment doping is 291m2/ g, interlamellar spacing 0.75nm, sulphur atom content are
20%, much larger than the specific surface area (40.8m undoped with MXene2/ g), interlamellar spacing (0.64nm)；The MXene of the present embodiment doping
Under the current density of 100mA/g, circulation 100 circle after reversible capacity be 301mAh/g, be undoped with MXene potassium ion electricity
3.2 times of pond cathode (93.8mAh/g).
Embodiment 4
A kind of preparation method of sulfur doping MXene composite material, comprising the following steps:
(1) Ti of 0.1g is weighed3C2Tx, the Mo of 0.1g3C2TxIt is add to deionized water with the diphenyl sulfide of 2g, is heated to 60
DEG C, magnetic agitation 3 hours, obtain mixed liquor.
(2) mixed liquor is moved into reaction kettle sealing, rear to place in baking oven, adjusting reaction temperature is 100 DEG C, and the reaction time is
6h。
(3) by alternately washing 3 times of obtained product deionized water and ethyl alcohol, and under the centrifugal speed of 3250r/min
It is centrifuged 3min, is finally putting into vacuum oven, dry 10h at 60 DEG C.
(4) prepared by kalium ion battery cathode: by resulting sulfur doping MXene and Kynoar binder, carbon black, by matter
Amount is mixed than the ratio for being 8:1:1, and suitable N-Methyl pyrrolidone is added, and is mixing uniformly to form slurry coated in collector
On, after vacuum dried, slice, sulfur doping MXene battery cathode is made.
(5) the present embodiment doping MXene under the current density of 100mA/g, circulation 100 circle after reversible capacity be
372mAh/g is 4.0 times undoped with MXene kalium ion battery cathode (93.8mAh/g).
Embodiment 5
A kind of preparation method of sulfur doping MXene composite material, comprising the following steps:
(1) V of 0.2g is weighed3C2TxIt is add to deionized water with the 2- benzene ethyl mercaptan of 2g, is heated to 60 DEG C, magnetic force stirs
It mixes 3 hours, obtains mixed liquor.
(2) mixed liquor is moved into reaction kettle sealing, rear to place in baking oven, adjusting reaction temperature is 120 DEG C, and the reaction time is
8h。
(3) by alternately washing 3 times of obtained product deionized water and ethyl alcohol, and under the centrifugal speed of 3250r/min
It is centrifuged 3min, is finally putting into vacuum oven, dry 8h at 60 DEG C.
(4) prepared by kalium ion battery cathode: by resulting sulfur doping MXene and Kynoar binder, carbon black, by matter
Amount is mixed than the ratio for being 8:1:1, and suitable N-Methyl pyrrolidone is added, and is mixing uniformly to form slurry coated in collector
On, after vacuum dried, slice, sulfur doping MXene battery cathode is made.
(5) the present embodiment doping MXene under the current density of 100mA/g, circulation 100 circle after reversible capacity be
368mAh/g is 3.9 times undoped with MXene kalium ion battery cathode (93.8mAh/g).
Comparative example 1: undoped with MXene kalium ion battery cathode, the process of kalium ion battery cathode is prepared with embodiment 2.
Table 1: performance test
Above is only a specific embodiment of the present invention, it is not intended to limit the scope of the invention, all utilizations
The equivalent transformation that the present invention makees, is applied directly or indirectly in other relevant technical fields, similarly includes of the invention
Among scope of patent protection.
Claims (10)
1. a kind of preparation method of sulfur doping MXene composite material, which comprises the following steps:
(1) it is that 1:1~20 is added in deionized water according to mass ratio by MXene and sulphur source, stirs and heat, being configured to concentration is
The mixed liquor of 5-80mg/ml；
(2) mixed liquor immigration reaction kettle is heated to 80-200 DEG C, reacts 4-36h, then cools to room temperature；
(3) product that step (2) obtains is washed and is centrifuged with detergent, then be dried in vacuo, obtained the sulphur and mix
Miscellaneous MXene composite material.
2. the preparation method of sulfur doping MXene composite material according to claim 1, which is characterized in that the sulphur source is
At least one of diphenyl sulfide, 2- benzene ethyl mercaptan.
3. the preparation method of sulfur doping MXene composite material according to claim 1, which is characterized in that the MXene is
Ti3C2Tx、Mo3C2Tx、V3C2Tx、Ti3N2Tx、Mo3N2Tx、V3N2TxOne of or it is a variety of.
4. the preparation method of sulfur doping MXene composite material according to claim 1, which is characterized in that the sulfur doping
Sulfur doping amount is 1wt%-20wt% in MXene composite material.
5. the preparation method of sulfur doping MXene composite material according to claim 1, which is characterized in that the sulfur doping
Sulfur doping amount is 3wt%-15wt% in MXene composite material.
6. the preparation method of sulfur doping MXene composite material according to claim 1, which is characterized in that the detergent
For at least one of deionized water and ethyl alcohol.
7. the preparation method of sulfur doping MXene composite material according to claim 1, which is characterized in that in step (3) from
The revolving speed that the heart uses is 3000-3500r/min, is centrifuged 2-4min.
8. the preparation method of sulfur doping MXene composite material according to claim 1, which is characterized in that true in step (3)
The dry temperature of sky is 50-70 DEG C, drying time 8-24h, and vacuum degree is no more than 135Pa.
9. a kind of sulfur doping MXene composite material that preparation method according to claim 1 to 8 is prepared.
10. a kind of application of sulfur doping MXene composite material according to claim 9, which is characterized in that mix the sulphur
Miscellaneous MXene composite material is used for kalium ion battery cathode.
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| WO2020147294A1 (en) * | 2019-01-15 | 2020-07-23 | 五邑大学 | Selenium-doped mxene material, preparation method therefor and use thereof |
| CN112072101A (en) * | 2020-08-14 | 2020-12-11 | 五邑大学 | Boron-doped MXene material and preparation method thereof |
| CN112191244A (en) * | 2020-08-31 | 2021-01-08 | 浙江工业大学 | Activated carbon-supported gold-based catalyst, preparation method thereof and application thereof in acetylene hydrogenation |
| CN113969171A (en) * | 2020-07-24 | 2022-01-25 | Tcl科技集团股份有限公司 | Preparation method of doped MXene quantum dots, optical film and QLED |
| WO2022032743A1 (en) * | 2020-08-12 | 2022-02-17 | 五邑大学 | Cote2/mxene composite material and preparation method therefor |
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| WO2022032744A1 (en) * | 2020-08-10 | 2022-02-17 | 五邑大学 | Nbs2/mxene composite material and preparation method therefor |
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Cited By (8)
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| WO2020147294A1 (en) * | 2019-01-15 | 2020-07-23 | 五邑大学 | Selenium-doped mxene material, preparation method therefor and use thereof |
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| WO2022032747A1 (en) * | 2020-08-10 | 2022-02-17 | 五邑大学 | Method for preparing sulfur-doped rese2/mxene composite material |
| WO2022032744A1 (en) * | 2020-08-10 | 2022-02-17 | 五邑大学 | Nbs2/mxene composite material and preparation method therefor |
| WO2022032743A1 (en) * | 2020-08-12 | 2022-02-17 | 五邑大学 | Cote2/mxene composite material and preparation method therefor |
| CN112072101A (en) * | 2020-08-14 | 2020-12-11 | 五邑大学 | Boron-doped MXene material and preparation method thereof |
| CN112191244A (en) * | 2020-08-31 | 2021-01-08 | 浙江工业大学 | Activated carbon-supported gold-based catalyst, preparation method thereof and application thereof in acetylene hydrogenation |
| CN112191244B (en) * | 2020-08-31 | 2023-03-31 | 浙江工业大学 | Activated carbon-supported gold-based catalyst, preparation method thereof and application thereof in acetylene hydrogenation |
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