CN109817921A - A kind of sulfur doping MXene negative electrode material and its preparation method and application - Google Patents
A kind of sulfur doping MXene negative electrode material and its preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of sulfur doping MXene negative electrode materials and preparation method thereof, the following steps are included: sulphur persursor material and MXene are respectively placed in the two sides in quartz boat by (1), then quartz boat is transferred in tube furnace, wherein the mass ratio of the sulphur persursor material and MXene are 15-25:1, and the side that sulphur persursor material is placed in quartz boat is located at the upstream of tube furnace；(2) it is passed through protective gas; carry out heat treatment reaction; it washs, be dried in vacuo after being cooled to room temperature; obtain sulfur doping MXene negative electrode material; wherein the heat treatment reaction is first from room temperature to 170-600 DEG C; 1.5-2.5h is kept the temperature, then is cooled to 80-120 DEG C, then keeps the temperature 1.5-2.5h.The MXene negative electrode material large specific surface area of sulfur doping prepared by the present invention, shows good electric conductivity, improves specific capacity, the stable circulation performance of kalium ion battery, and element sulphur doping is controllable, is suitble to large-scale application.
Description
Technical field
The invention belongs to new energy materials fields, and in particular to a kind of preparation method of sulfur doping MXene negative electrode 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.
Lithium ion battery, which has the characteristics that voltage is high, specific energy is big, has extended cycle life, self discharge is small becomes the widest electricity of research at present
One of pond.But a large amount of consumption of lithium metal also start to cause the worry of people.Therefore, a kind of lithium ion battery generation is found
Become current research emphasis for product.
Since potassium element is resourceful, it is evenly distributed and advantage at low cost, kalium ion battery is likely to become big
Widely applied battery system in scale electrochemical energy storage field.But the chemical property of kalium ion battery does not still make us full
Meaning.The specific capacity of kalium ion battery how is improved, while having both excellent cycle performance, is current technology difficult point.
MXene material is a kind of novel two-dimensional layer material, is carved in a solution of hydrofluoric acid by lamellar compound MAX material
Erosion processing is made.Wherein, M is transition metal element, and A III, IV major element, X is C or N element.Because having and graphene
Similar two-dimensional structure and be named as MXene.During hf etching, M-X covalently bonded resultant force in lamellar compound MAX
Much stronger than M-A metallic bond, therefore A atomic layer is stripped, and is left M-X atomic layer and is formed two-dimensional layered-structure material.MXene material
Material has had been reported in supercapacitor and lithium ion battery, but MXene ontology is used as kalium ion battery negative electrode material, performance
It is still unsatisfactory.The present invention can increase interlamellar spacing and specific surface area by carrying out sulfur doping to MXene, and 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 cathode materials
Material.Another object of the present invention is to provide the preparation methods of above-mentioned sulfur doping MXene negative electrode material.Further, of the invention
A kind of application of sulfur doping MXene negative electrode material is provided, the sulfur doping MXene negative electrode material is born as kalium ion battery
Pole.
The invention adopts the following technical scheme:
A kind of preparation method of sulfur doping MXene negative electrode material, comprising the following steps:
(1) sulphur persursor material and MXene are respectively placed in the two sides in quartz boat, quartz boat is then transferred to pipe
In formula furnace, wherein the mass ratio of the sulphur persursor material and MXene be 15-25:1 (such as 16:1,17:1,18:1,19:1,
20:1,21:1,22:1,23:1,24:1), the side that sulphur persursor material is placed in quartz boat is located at the upstream of tube furnace；
(2) it is passed through protective gas (gas leads to downstream from the upstream of tube furnace), heat treatment reaction is carried out, is cooled to room temperature
Wash, be dried in vacuo to get sulfur doping MXene negative electrode material is arrived afterwards, wherein heat treatment reaction be it is first from room temperature to
170-600 DEG C (such as 170 DEG C, 180 DEG C, 190 DEG C, 200 DEG C, 210 DEG C, 220 DEG C, 230 DEG C, 240 DEG C, 250 DEG C, 260 DEG C, 270
℃、280℃、290℃、300℃、310℃、320℃、330℃、340℃、350℃、360℃、370℃、380℃、390℃、
400℃、410℃、420℃、430℃、440℃、450℃、460℃、470℃、480℃、490℃、500℃、510℃、520
DEG C, 530 DEG C, 540 DEG C, 550 DEG C, 560 DEG C, 570 DEG C, 580 DEG C, 590 DEG C, 600 DEG C), heat preservation 1.5-2.5h (such as 1.6,1.7,
1.8,1.9,2.0,2.1,2.2,2.3,2.4,2.5h), then be cooled to 80-120 DEG C (such as 80 DEG C, 90 DEG C, 100 DEG C, 110 DEG C,
120 DEG C), then keep the temperature 1.5-2.5h (such as 1.6,1.7,1.8,1.9,2.0,2.1,2.2,2.3,2.4,2.5h).
Optionally, wherein heat treatment reaction is first to belong to Low Temperature Heat Treatment work from room temperature to 170-300 DEG C
Skill keeps the temperature 1.5-2.5h, then is cooled to 80-120 DEG C, then keeps the temperature 1.5-2.5h, belongs to continuous low temperature heat treatment process.
Room temperature can be 0-38 DEG C, such as 5-35 DEG C, 10-30 DEG C, 15-28 DEG C, 18-25 DEG C, be also possible to zubzero temperature.
Further, the sulphur persursor material is at least one of 2- benzene ethyl mercaptan, diphenyl sulfide, preferably 2- benzene second sulphur
Alcohol, preferred mass ratio are (2~5): 1 2- benzene ethyl mercaptan and diphenyl sulfide.
Further, the MXene is Ti2NTx、Mo2NTx、V2NTx、Ti2CTx、Mo2CTx、V2CTxOne of or it is more
Kind, optional V2CTx, optional Mo2NTx, optional V2NTx, optional mass ratio is the Ti of 4~6:12CTxAnd V2NTx, optional mass ratio is
The Ti of 4~6:12CTxAnd Mo2CTx, optional Ti2CTx、Mo2CTxAnd V2CTx(such as mass ratio is 5~8:2:1), TxFor surface official
It can group-O ,-F or-OH.
Further, in the sulfur doping MXene negative electrode material sulfur doping amount be 0.1wt%-25wt% (such as 0.3,
0.5、0.7、0.9、1.1、1.3、1.5、1.7、1.8、1.9、2.0、2.1、2.2、2.3、2.4、2.5、2.8、11、13、15、17、
19,21,23wt%).
Further, in the sulfur doping MXene negative electrode material sulfur doping amount be 3wt%-10wt% (such as 3.5,4.5,
5.5,6.5,7.5,8.5,9.5wt%).
Further, the flow velocity of the protective gas be 140-180ml/min, such as 140,145,150,155,160,
165,170,175,180ml/min；The protective gas is Ar.
Further, the rate of heating described in step (2) be 1.5-5 DEG C/min (such as 1.8,2,2.5,3,3.5,4,
4.5,5 DEG C/min), the rate of the cooling is 0.5-4 DEG C/min (such as 0.8,1,1.5,2,2.5,3,3.5,4 DEG C/min).
Further, the time that reaction is heat-treated described in step (2) is 2-5h (such as 2,3,4,5h).
Further, slurry and/or ethyl alcohol are washed in step (2)；Vacuum drying temperature is 50-70 DEG C,
It is preferred that 60 DEG C, vacuum degree is no more than 133Pa, such as no more than 125,115,105,95,85Pa.
A kind of sulfur doping MXene negative electrode material that the preparation method of sulfur doping MXene negative electrode material is prepared.
The sulfur doping MXene negative electrode material is used for kalium ion battery by a kind of application of sulfur doping MXene negative electrode material
Cathode.
In sulfur doping MXene negative electrode material of the present invention, the part carbon atom of MXene is replaced by sulphur atom, generates a large amount of knots
Structure defect improves the specific capacity of MXene, and sulphur atom and MXene are with covalent bond to cause more electro-chemical activity sites
In conjunction with further improving the high rate performance and cyclical stability of MXene especially with Ti-S Covalent bonding together.Sulphur of the present invention
MXene after element doping is layer structure, and specific surface area with higher shows good electric conductivity.
Beneficial effects of the present invention:
(1) the MXene negative electrode material large specific surface area of sulfur doping prepared by the present invention, shows good electric conductivity, mentions
The high specific capacity of kalium ion battery, stable circulation performance；
(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 negative electrode material in embodiment 1；
Fig. 3 is the cycle performance figure that sulfur doping MXene negative electrode 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 negative electrode 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 negative electrode material, comprising the following steps:
(1) V of 0.2g is weighed2CTxWith the 2- benzene ethyl mercaptan of 4g, the both ends of quartz boat are respectively placed in, 2- benzene second will be placed with
One end of mercaptan is placed on the upstream of tube furnace；
It (2) is under 160ml/min high-purity argon gas (purity >=99.8%) protects atmosphere, from room temperature 20 in gas flow rate size
DEG C 170 DEG C are warming up to 1.5 DEG C/min, after keeping 2h, then with 0.5 DEG C/min be cooled to 100 DEG C, 2h is kept at 100 DEG C, then
Room temperature is dropped to, sample is washed with deionized water after cooling, vacuum drying obtains final sample.
(3) prepared by kalium ion battery cathode: by the resulting sulfur doping MXene of step (2) and Kynoar binder, carbon
It is black, it is mixed in mass ratio for the ratio of 8:1:1, suitable N-Methyl pyrrolidone is added, be mixing uniformly to form slurry coating
On a current collector, after vacuum dried, slice, sulfur doping MXene battery cathode is made.
(4) Fig. 1 shows that undoped with MXene be " accordion " pattern, and Fig. 2 is the pattern after the present embodiment doping.After doping
MXene negative electrode material specific surface area be 165m2/ g, interlamellar spacing 0.64nm, sulphur atom content is 0.1%, much larger than not mixing
Specific surface area (the 38.2m of miscellaneous MXene2/ g), interlamellar spacing (0.62nm)；Fig. 3 shows the MXene negative electrode material of the present embodiment doping
Under the current density of 100mA/g, it is Fig. 4 undoped with MXene potassium ion that the reversible capacity after 100 circle of circulation, which is 224mAh/g,
2.4 times of battery cathode (90.5mAh/g).
Embodiment 2
A kind of preparation method of sulfur doping MXene negative electrode material, comprising the following steps:
(1) V of 0.4g is weighed2CTxWith the 2- benzene ethyl mercaptan of 8g, the both ends of quartz boat are respectively placed in, 2- benzene second will be placed with
One end of mercaptan is placed on the upstream of tube furnace.
It (2) is under 160ml/min high-purity argon gas protects atmosphere, from 20 DEG C of room temperature with 2.5 DEG C/min in gas flow rate size
It is warming up to 320 DEG C, after keeping 2h, then with 2.5 DEG C/min is cooled to 100 DEG C, 2h is kept at 100 DEG C, then drop to room temperature, it is cooling
Sample is washed with deionized water afterwards, vacuum drying obtains final sample.
(3) prepared by kalium ion battery cathode: by the resulting sulfur doping MXene of step (2) and Kynoar binder, carbon
It is black, it is mixed in mass ratio for the ratio of 8:1:1, suitable N-Methyl pyrrolidone is added, be mixing uniformly to form slurry coating
On a current collector, after vacuum dried, slice, sulfur doping MXene negative electrode tab is made.
(4) the MXene specific surface area after the present embodiment doping is 312m2/ g, interlamellar spacing 0.75nm, sulphur atom content are
7%, much larger than the specific surface area (38.2m undoped with MXene2/ g), interlamellar spacing (0.62nm)；The MXene of the present embodiment doping
Negative electrode material under the current density of 100mA/g, it is undoped with MXene that the reversible capacity after 100 circle of circulation, which is 345mAh/g,
3.8 times of kalium ion battery cathode (90.5mAh/g).
Embodiment 3
A kind of preparation method of sulfur doping MXene negative electrode material, comprising the following steps:
(1) V of 0.5g is weighed2CTxWith the 2- benzene ethyl mercaptan of 10g, the both ends of quartz boat are respectively placed in, 2- benzene will be placed with
One end of ethyl mercaptan is placed on the upstream of tube furnace.
It (2) is under 160ml/min high-purity argon gas protects atmosphere, from 20 DEG C of room temperature with 5 DEG C/min liter in gas flow rate size
Temperature after keeping 2h, then with 4 DEG C/min is cooled to 100 DEG C, 2h is kept at 100 DEG C, then drop to room temperature to 600 DEG C, uses after cooling
Deionized water washs sample, and vacuum drying obtains final sample.
(3) prepared by kalium ion battery cathode: by the resulting sulfur doping MXene of step (2) and Kynoar binder, carbon
It is black, it is mixed in mass ratio for the ratio of 8:1:1, suitable N-Methyl pyrrolidone is added, be mixing uniformly to form slurry coating
On a current collector, after vacuum dried, slice, sulfur doping MXene material cell cathode is made.
(4) the MXene specific surface area after the present embodiment doping is 233m2/ g, interlamellar spacing 0.81nm, sulphur atom content are
25%, much larger than the specific surface area (38.2m undoped with MXene2/ g), interlamellar spacing (0.62nm)；The MXene of the present embodiment doping
Under the current density of 100mA/g, circulation 100 circle after reversible capacity be 289mAh/g, be undoped with MXene potassium ion electricity
3.1 times of pond cathode (90.5mAh/g).
Embodiment 4
A kind of preparation method of sulfur doping MXene negative electrode material, comprising the following steps:
(1) MXene (Ti of 0.3g is weighed2CTxWith the Mo of 0.05g2CTxBe uniformly mixed) with the 2- benzene ethyl mercaptan of 7g, respectively
The both ends of quartz boat are placed in, the one end for being placed with 2- benzene ethyl mercaptan is placed on to the upstream of tube furnace.
It (2) is under 180ml/min high-purity argon gas (purity >=99.8%) protects atmosphere, from room temperature 20 in gas flow rate size
DEG C 180 DEG C are warming up to 1.5 DEG C/min, after keeping 2h, then with 0.5 DEG C/min be cooled to 100 DEG C, 2h is kept at 100 DEG C, then
Room temperature is dropped to, sample is washed with deionized water after cooling, vacuum drying obtains final sample.
(3) prepared by kalium ion battery cathode: by the resulting sulfur doping MXene of step (2) and Kynoar binder, carbon
It is black, it is mixed in mass ratio for the ratio of 8:1:1, suitable N-Methyl pyrrolidone is added, be mixing uniformly to form slurry coating
On a current collector, after vacuum dried, slice, sulfur doping MXene battery cathode is made.
The present embodiment doping MXene negative electrode material under the current density of 100mA/g, circulation 100 circle after it is reversible
Capacity is 387mAh/g, is 4.3 times undoped with MXene kalium ion battery cathode (90.5mAh/g).
Embodiment 5
A kind of preparation method of sulfur doping MXene negative electrode material, comprising the following steps:
(1) V of 0.4g is weighed2CTxWith the diphenyl sulfide of 6g, the both ends of quartz boat are respectively placed in, the one of diphenyl sulfide will be placed with
End is placed on the upstream of tube furnace.
(2) gas flow rate size be 180ml/min high-purity argon gas (purity >=99.8%) protect atmosphere under, from room temperature with
1.5 DEG C/min is warming up to 190 DEG C, after keeping 2h, then with 0.6 DEG C/min is cooled to 120 DEG C, 2h is kept at 120 DEG C, then drop to
Room temperature washs sample with deionized water after cooling, and vacuum drying obtains final sample.
(3) prepared by kalium ion battery cathode: by the resulting sulfur doping MXene of step (2) and Kynoar binder, carbon
It is black, it is mixed in mass ratio for the ratio of 8:1:1, suitable N-Methyl pyrrolidone is added, be mixing uniformly to form slurry coating
On a current collector, after vacuum dried, slice, sulfur doping MXene battery cathode is made.
The present embodiment doping MXene negative electrode material under the current density of 100mA/g, circulation 100 circle after it is reversible
Capacity is 370mAh/g, is 4.1 times undoped with MXene kalium ion battery cathode (90.5mAh/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 negative electrode material, which comprises the following steps:
(1) sulphur persursor material and MXene are respectively placed in the two sides in quartz boat, quartz boat is then transferred to tube furnace
In, wherein the mass ratio of the sulphur persursor material and MXene are 15-25:1, the one of sulphur persursor material is placed in quartz boat
Side is located at the upstream of tube furnace；
(2) it is passed through protective gas, carries out heat treatment reaction, washs, be dried in vacuo to get sulfur doping is arrived after being cooled to room temperature
MXene negative electrode material, wherein heat treatment reaction is first to keep the temperature 1.5-2.5h, then cool down from room temperature to 170-600 DEG C
To 80-120 DEG C, 1.5-2.5h is then kept the temperature.
2. the preparation method of sulfur doping MXene negative electrode material according to claim 1, which is characterized in that the sulphur forerunner
Body material is at least one of 2- benzene ethyl mercaptan, diphenyl sulfide.
3. the preparation method of sulfur doping MXene negative electrode material according to claim 1, which is characterized in that the MXene is
Ti2NTx、Mo2NTx、V2NTx、Ti2CTx、Mo2CTx、V2CTxOne of or it is a variety of.
4. the preparation method of sulfur doping MXene negative electrode material according to claim 1, which is characterized in that the sulfur doping
Sulfur doping amount is 0.1wt%-25wt% in MXene negative electrode material.
5. the preparation method of sulfur doping MXene negative electrode material according to claim 1, which is characterized in that the sulfur doping
Sulfur doping amount is 3wt%-10wt% in MXene negative electrode material.
6. the preparation method of sulfur doping MXene negative electrode material according to claim 1, which is characterized in that the protection gas
The flow velocity of body is 140-180ml/min；The protective gas is Ar.
7. the preparation method of sulfur doping MXene negative electrode material according to claim 1, which is characterized in that institute in step (2)
The rate for stating heating is 1.5-5 DEG C/min, and the rate of the cooling is 0.5-4 DEG C/min.
8. the preparation method of sulfur doping MXene negative electrode material according to claim 1, which is characterized in that institute in step (2)
The time for stating heat treatment reaction is 2-5h.
9. a kind of sulfur doping MXene negative electrode material that preparation method according to claim 1 to 8 is prepared.
10. a kind of application of sulfur doping MXene negative electrode material according to claim 9, which is characterized in that mix the sulphur
Miscellaneous MXene negative electrode material is used for kalium ion battery cathode.
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| CN111180694A (en) * | 2019-12-31 | 2020-05-19 | 广东工业大学 | MXene/metal sulfide composite material, negative electrode material, preparation and application |
| WO2020147295A1 (en) * | 2019-01-15 | 2020-07-23 | 五邑大学 | Se-doped mxene battery cathode material and preparation method and use thereof |
| CN111943149A (en) * | 2020-08-25 | 2020-11-17 | 合肥工业大学 | General preparation method of transition metal nitride |
| 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 |
| 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 |
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| CN111180694A (en) * | 2019-12-31 | 2020-05-19 | 广东工业大学 | MXene/metal sulfide composite material, negative electrode material, preparation and application |
| 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 |
| 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 |
| CN111943149A (en) * | 2020-08-25 | 2020-11-17 | 合肥工业大学 | General preparation method of transition metal nitride |
| 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 |
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