CN107256811A - The synthetic method of nitrogen-doped carbon coating zinc oxide and its application - Google Patents
The synthetic method of nitrogen-doped carbon coating zinc oxide and its application Download PDFInfo
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- CN107256811A CN107256811A CN201710532673.5A CN201710532673A CN107256811A CN 107256811 A CN107256811 A CN 107256811A CN 201710532673 A CN201710532673 A CN 201710532673A CN 107256811 A CN107256811 A CN 107256811A
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- nitrogen
- zinc oxide
- doped carbon
- carbon coating
- coating zinc
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/04—Hybrid capacitors
- H01G11/06—Hybrid capacitors with one of the electrodes allowing ions to be reversibly doped thereinto, e.g. lithium ion capacitors [LIC]
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/50—Electrodes characterised by their material specially adapted for lithium-ion capacitors, e.g. for lithium-doping or for intercalation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of synthetic method of nitrogen-doped carbon coating zinc oxide, this method is using zinc nitrate, hexa as primary raw material, using hybrid reaction, then prepared by the mode of high temperature cabonization, and the weight/mass percentage composition of manganese oxide is 12 ~ 18% in the final nitrogen-doped carbon coating zinc oxide.The invention also discloses the electrode material that above-mentioned nitrogen-doped carbon coating zinc oxide is used as lithium-ion capacitor.The present invention can significantly improve the electric conductivity, charge-discharge performance and cycle performance of capacitor as electrode material.
Description
Technical field
The present invention relates to lithium-ion capacitance technical field, more particularly to a kind of synthesis side of nitrogen-doped carbon coating zinc oxide
Method and its application.
Background technology
Lithium-ion capacitor（LIC）It can be described as Li-Ion rechargeable battery（LIB）And double layer capacitor（EDLC）It is mixed
Capacitor is closed, positive pole typically uses activated carbon, and negative pole is typically using materials such as graphite.It is more stable than Li-Ion rechargeable battery, again
The electric property of double layer capacitor is surmounted, thermorunaway and aging are few, and self discharge is also seldom.The spy of lithium-ion capacitor
Point be have with double layer capacitor EDLC identical charging rates, and energy density be higher than EDLC.The cycle of charging and discharging
More preferably, charging and discharging is tens thousand of secondary repeatedly, and capacity only reduces a few percent for characteristic.Also it will not catch fire or explode even if temporary short circuit,
Security is very high.It can be said that the performance of lithium-ion capacitor has exceeded double layer capacitor comprehensively.
And electrode is the core of lithium-ion capacitor, the chemical property of electrode determines the performance of capacitor.With lithium
The development of ionistor technology, at present for lithium-ion capacitor requirement more and more higher, it is necessary to which it possesses quickly fills
Electricity.The performances such as high temperature resistant.And lithium-ion capacitor is typically using materials such as graphite as negative pole at present, its chemical property can not
Preferably meet the demand.
The content of the invention
There is provided a kind of nitrogen-doped carbon bag aiming at above-mentioned background technology not enough for the technical problems to be solved by the invention
Synthetic method and its application of zinc oxide are covered, the electric conductivity of capacitor can be significantly improved by employing the invention as electrode material
Energy, charge-discharge performance and cycle performance.
In order to solve the above technical problems, a kind of synthetic method for nitrogen-doped carbon coating zinc oxide that the present invention is provided, we
Method comprises the following steps using zinc nitrate, hexa as primary raw material：
1）, zinc nitrate solution and hexa solution are mixed, citric acid is added, is well mixed, gained mixed liquor is existed
Reacted under hydrothermal condition, it is fully reacted；
2）, by reaction solution centrifugal drying, solid product is obtained, by gained solid product high-temperature roasting, room temperature is then cooled to；
3）, in the conical flask that the solid product after cooling is poured into magnetic particle, add the stirring of TRIS-HCl buffer solutions, then plus
Enter the Dopamine hydrochloride of equivalent, stirring makes it fully react；
4）, reaction solution is centrifuged into washing drying, high-temperature calcination is obtained under nitrogen protection by gained solid product after drying
Nitrogen-doped carbon coating zinc oxide；
The weight/mass percentage composition of zinc oxide is 12 ~ 18% in the final nitrogen-doped carbon coating zinc oxide.
In the above-mentioned technical solutions, the step 1）In, the reaction temperature of the hydro-thermal reaction is 80 ~ 95 DEG C, during reaction
Between in 10 ~ 12h.
In the above-mentioned technical solutions, the step 2）In, the drying temperature of mixed liquor is at 75 ~ 90 DEG C.
In the above-mentioned technical solutions, the step 2）In, high-temperature roasting is warming up to 800 using 5 DEG C/min heating rate
DEG C baked above, the roasting time of high-temperature roasting is in 0.5 ~ 1h.
In the above-mentioned technical solutions, the step 3）In, add TRIS-HCl buffer solutions and stir 0.5 ~ 1h, then add etc.
The Dopamine hydrochloride of amount, stirs more than 24h.
In the above-mentioned technical solutions, the step 4）In, high-temperature calcination is warming up to 600 using 5 DEG C/min heating rate
More than DEG C, the time of high-temperature calcination is in more than 3h.
Present invention also offers the application of above-mentioned nitrogen-doped carbon coating zinc oxide, the nitrogen-doped carbon coating zinc oxide is used as
The electrode material of lithium-ion capacitor, the nitrogen-doped carbon coating zinc oxide is preferably used as the negative material of lithium-ion capacitor.
Compared with prior art, the beneficial effects of the present invention are：Based on present invention use zinc nitrate, hexa
Raw material is wanted, nitrogen-doped carbon coating zinc oxide, whole preparation technology work are obtained by steps such as hybrid reaction, drying, high temperature cabonizations
Sequence is simple, easy to operate；Meanwhile, obtained nitrogen-doped carbon coating zinc oxide, its grain particles are uniform, and carbon coating is uniform, compact；
Traditional graphite or carbon electrode are used relative to prior art, the electrode energy prepared using nitrogen-doped carbon coating zinc oxide of the present invention
Enough significantly improve the electric conductivity, charge-discharge performance and cycle performance of lithium ion mixing electric capacity.
Brief description of the drawings
Fig. 1 is the outside drawing of nitrogen-doped carbon coating zinc oxide of the present invention；
The charging and discharging curve figure of capacitor prepared by Fig. 2 present invention under different electric currents.
Embodiment
The specific embodiment of the present invention is described in further detail below in conjunction with accompanying drawing：
The synthetic method of nitrogen-doped carbon coating zinc oxide, this method using zinc nitrate, hexa as primary raw material, including with
Lower step：
1）, zinc nitrate solution and hexa solution are mixed, citric acid is added, is well mixed, gained mixed liquor is existed
Reacted under hydrothermal condition, it is fully reacted；
2）, by reaction solution centrifugal drying, solid product is obtained, by gained solid product high-temperature roasting, room temperature is then cooled to；
3）, in the conical flask that the solid product after cooling is poured into magnetic particle, add the stirring of TRIS-HCl buffer solutions, then plus
Enter the Dopamine hydrochloride of equivalent, stirring makes it fully react；
4）, reaction solution is centrifuged into washing drying, high-temperature calcination is obtained under nitrogen protection by gained solid product after drying
Nitrogen-doped carbon coating zinc oxide；
The weight/mass percentage composition of zinc oxide is 12 ~ 18% in the final nitrogen-doped carbon coating zinc oxide.
The step 1）In, the reaction temperature of the hydro-thermal reaction is preferably 80 ~ 95 DEG C, and the reaction time is preferably controlled in 10
~12h。
The step 2）In, the drying temperature of mixed liquor is preferably controlled in 75 ~ 90 DEG C；High-temperature roasting be preferred to use 5 DEG C/
Min heating rate be warming up to 800 DEG C it is baked above, roasting time is preferably controlled in 0.5 ~ 1h.
The step 3）In, add TRIS-HCl buffer solutions and stir 0.5 ~ 1h, then add the Dopamine hydrochloride of equivalent, stir
Mix more than 24h.
The step 4）In, high-temperature calcination is preferred to use 5 DEG C/min heating rate and is warming up to more than 600 DEG C, during calcining
Between in more than 3h.
Embodiment 1
1）Appropriate zinc nitrate solution and hexa solution are taken, is mixed, and citric acid is added dropwise simultaneously in backward mixed liquor
Stirring, by gained mixed liquor at a temperature of 80 DEG C hydro-thermal reaction 10h；
2）By reaction solution in 75 DEG C of centrifugal dryings, solid product is obtained, by gained solid product high-temperature roasting, high-temperature roasting is used
5 DEG C/min heating rate is warming up to 800 DEG C, is calcined 0.5h, then naturally cools to room temperature；
3）In the conical flask that solid product after cooling is poured into magnetic particle, TRIS-HCl buffer solutions stirring 0.5h is added, and
The Dopamine hydrochloride of equivalent is added afterwards, stirs 24h；
4）Reaction solution is centrifuged into washing drying, by gained solid product high-temperature calcination under nitrogen protection, high temperature after drying
Calcining is warming up to 600 DEG C using 5 DEG C/min heating rate, and calcination time 3h obtains nitrogen-doped carbon coating zinc oxide；
Zinc nitrate and hexa must ensure the weight/mass percentage composition of manganese oxide in final product 12%.
Through range estimation, the nitrogen-doped carbon coating zinc oxide homogeneous grain size of the present embodiment is evenly coated.
Embodiment 2
1）Appropriate zinc nitrate solution and hexa solution are taken, is mixed, and citric acid is added dropwise simultaneously in backward mixed liquor
Stirring, by gained mixed liquor at a temperature of 85 DEG C hydro-thermal reaction 11h；
2）By reaction solution in 80 DEG C of centrifugal dryings, solid product is obtained, by gained solid product high-temperature roasting, high-temperature roasting is used
5 DEG C/min heating rate is warming up to 800 DEG C, is calcined 0.5h, then naturally cools to room temperature；
3）In the conical flask that solid product after cooling is poured into magnetic particle, TRIS-HCl buffer solutions stirring 0.5h is added, and
The Dopamine hydrochloride of equivalent is added afterwards, stirs 24h；
4）Reaction solution is centrifuged into washing drying, by gained solid product high-temperature calcination under nitrogen protection, high temperature after drying
Calcining is warming up to 650 DEG C using 5 DEG C/min heating rate, and calcination time 3h obtains nitrogen-doped carbon coating zinc oxide；
Zinc nitrate and hexa must ensure the weight/mass percentage composition of manganese oxide in final product 13%.
Through range estimation, the nitrogen-doped carbon coating zinc oxide homogeneous grain size of the present embodiment is evenly coated.
Embodiment 3
1）Appropriate zinc nitrate solution and hexa solution are taken, is mixed, and citric acid is added dropwise simultaneously in backward mixed liquor
Stirring, by gained mixed liquor at a temperature of 85 DEG C hydro-thermal reaction 12h；
2）By reaction solution in 85 DEG C of centrifugal dryings, solid product is obtained, by gained solid product high-temperature roasting, high-temperature roasting is used
5 DEG C/min heating rate is warming up to 800 DEG C, is calcined 0.5h, then naturally cools to room temperature；
3）In the conical flask that solid product after cooling is poured into magnetic particle, TRIS-HCl buffer solutions stirring 0.5h is added, and
The Dopamine hydrochloride of equivalent is added afterwards, stirs 24h；
4）Reaction solution is centrifuged into washing drying, by gained solid product high-temperature calcination under nitrogen protection, high temperature after drying
Calcining is warming up to 650 DEG C using 5 DEG C/min heating rate, and calcination time 4h obtains nitrogen-doped carbon coating zinc oxide；
Zinc nitrate and hexa must ensure the weight/mass percentage composition of manganese oxide in final product 15%.
Through range estimation, the nitrogen-doped carbon coating zinc oxide homogeneous grain size of the present embodiment is evenly coated.
Embodiment 4
1）Appropriate zinc nitrate solution and hexa solution are taken, is mixed, and citric acid is added dropwise simultaneously in backward mixed liquor
Stirring, by gained mixed liquor at a temperature of 90 DEG C hydro-thermal reaction 11h；
2）By reaction solution in 85 DEG C of centrifugal dryings, solid product is obtained, by gained solid product high-temperature roasting, high-temperature roasting is used
5 DEG C/min heating rate is warming up to 850 DEG C, is calcined 1h, then naturally cools to room temperature；
3）In the conical flask that solid product after cooling is poured into magnetic particle, TRIS-HCl buffer solutions stirring 1h is added, then
The Dopamine hydrochloride of equivalent is added, 24h is stirred；
4）Reaction solution is centrifuged into washing drying, by gained solid product high-temperature calcination under nitrogen protection, high temperature after drying
Calcining is warming up to 700 DEG C using 5 DEG C/min heating rate, and calcination time 4h obtains nitrogen-doped carbon coating zinc oxide；
Zinc nitrate and hexa must ensure the weight/mass percentage composition of manganese oxide in final product 17%.
Through range estimation, the nitrogen-doped carbon coating zinc oxide homogeneous grain size of the present embodiment is evenly coated.
Embodiment 5
1）Appropriate zinc nitrate solution and hexa solution are taken, is mixed, and citric acid is added dropwise simultaneously in backward mixed liquor
Stirring, by gained mixed liquor at a temperature of 95 DEG C hydro-thermal reaction 12h；
2）By reaction solution in 90 DEG C of centrifugal dryings, solid product is obtained, by gained solid product high-temperature roasting, high-temperature roasting is used
5 DEG C/min heating rate is warming up to 850 DEG C, is calcined 1h, then naturally cools to room temperature；
3）In the conical flask that solid product after cooling is poured into magnetic particle, TRIS-HCl buffer solutions stirring 1h is added, then
The Dopamine hydrochloride of equivalent is added, 24h is stirred；
4）Reaction solution is centrifuged into washing drying, by gained solid product high-temperature calcination under nitrogen protection, high temperature after drying
Calcining is warming up to 700 DEG C using 5 DEG C/min heating rate, and calcination time 4h obtains nitrogen-doped carbon coating zinc oxide；
Zinc nitrate and hexa must ensure the weight/mass percentage composition of manganese oxide in final product 18%.
Through range estimation, the nitrogen-doped carbon coating zinc oxide homogeneous grain size of the present embodiment is evenly coated.
As shown in figure 1, the nitrogen-doped carbon coating zinc oxide of the present invention is crystalline powder.The nitrogen-doped carbon cladding of the present invention
Zinc oxide may be used as the electrode material of lithium-ion capacitor, be preferably used as the negative material of lithium-ion capacitor.
As shown in Fig. 2 after testing, using traditional graphite or carbon electrode relative to prior art, being mixed using nitrogen of the present invention
Electrode prepared by miscellaneous carbon coating zinc oxide can significantly improve the electric conductivity and cycle performance of lithium ion mixing electric capacity.
The core of the present invention is to utilize zinc nitrate, hexa to be primary raw material, passes through hybrid reaction, drying, height
The steps such as temperature carbonization obtain nitrogen-doped carbon coating zinc oxide, for the electrode material of lithium-ion capacitor, improve the electrification of electrode
Performance is learned, therefore, protection scope of the present invention is not limited only to above-described embodiment, on the basis of the principle of the invention, it is any to utilize
The change or deformation of above-mentioned mechanism, belong to protection scope of the present invention.
Claims (10)
1. a kind of synthetic method of nitrogen-doped carbon coating zinc oxide, it is characterised in that：This method is with zinc nitrate, hexa
For primary raw material, comprise the following steps：
1）, zinc nitrate solution and hexa solution are mixed, citric acid is added, is well mixed, gained mixed liquor is existed
Reacted under hydrothermal condition, it is fully reacted；
2）, by reaction solution centrifugal drying, solid product is obtained, by gained solid product high-temperature roasting, room temperature is then cooled to；
3）, in the conical flask that the solid product after cooling is poured into magnetic particle, add the stirring of TRIS-HCl buffer solutions, then plus
Enter the Dopamine hydrochloride of equivalent, stirring makes it fully react；
4）, reaction solution is centrifuged into washing drying, high-temperature calcination is obtained under nitrogen protection by gained solid product after drying
Nitrogen-doped carbon coating zinc oxide；
The weight/mass percentage composition of zinc oxide is 12 ~ 18% in the final nitrogen-doped carbon coating zinc oxide.
2. the synthetic method of nitrogen-doped carbon coating zinc oxide according to claim 1, it is characterised in that：The step 1）
In, the reaction temperature of the hydro-thermal reaction is 80 ~ 95 DEG C, and the reaction time is in 10 ~ 12h.
3. the synthetic method of nitrogen-doped carbon coating zinc oxide according to claim 1, it is characterised in that：The step 2）
In, the drying temperature of mixed liquor is at 75 ~ 90 DEG C.
4. the synthetic method of nitrogen-doped carbon coating zinc oxide according to claim 1, it is characterised in that：The step 2）
In, high-temperature roasting using 5 DEG C/min heating rate be warming up to 800 DEG C it is baked above.
5. the synthetic method of nitrogen-doped carbon coating zinc oxide according to claim 1, it is characterised in that：The step 2）
In, the roasting time of high-temperature roasting is in 0.5 ~ 1h.
6. the synthetic method of nitrogen-doped carbon coating zinc oxide according to claim 1, it is characterised in that：The step 3）
In, add TRIS-HCl buffer solutions and stir 0.5 ~ 1h, then add the Dopamine hydrochloride of equivalent, stir more than 24h.
7. the synthetic method of the nitrogen-doped carbon coating zinc oxide according to claim 1 ~ 6 any one, it is characterised in that：Institute
State step 4）In, high-temperature calcination is warming up to more than 600 DEG C using 5 DEG C/min heating rate.
8. the synthetic method of nitrogen-doped carbon coating zinc oxide according to claim 7, it is characterised in that：The step 4）
In, the time of high-temperature calcination is in more than 3h.
9. a kind of application of nitrogen-doped carbon coating zinc oxide as described in claim 1 ~ 8, it is characterised in that：The nitrogen-doped carbon
Coating zinc oxide is used as the electrode material of lithium-ion capacitor.
10. the application of nitrogen-doped carbon coating zinc oxide according to claim 9, it is characterised in that：The nitrogen-doped carbon bag
Cover the negative material that zinc oxide is used as lithium-ion capacitor.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107867713A (en) * | 2017-11-09 | 2018-04-03 | 扬州大学 | A kind of ZnO sensing electrode material preparation methods of porous nano pie structure |
| CN108365211A (en) * | 2018-04-20 | 2018-08-03 | 合肥工业大学 | A kind of preparation method of nitrogen-doped carbon cladding zinc telluridse nano wire and its application as anode material of lithium-ion battery |
| CN109786666A (en) * | 2019-03-21 | 2019-05-21 | 福建蓝海黑石新材料科技有限公司 | A kind of nitrogen-doped carbon coated Si nano particle composite material, preparation method and application |
| CN112745559A (en) * | 2020-12-23 | 2021-05-04 | 河南工业大学 | Polymer dielectric elastomer and preparation method and application thereof |
| CN113101962A (en) * | 2021-04-25 | 2021-07-13 | 山西中科国蕴环保科技有限公司 | Porous carbon layer protection catalyst for activating persulfate, preparation method and application |
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| CN103991896A (en) * | 2014-04-08 | 2014-08-20 | 西北大学 | Spherical zinc oxide nanometer material preparation method |
Non-Patent Citations (1)
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107867713A (en) * | 2017-11-09 | 2018-04-03 | 扬州大学 | A kind of ZnO sensing electrode material preparation methods of porous nano pie structure |
| CN107867713B (en) * | 2017-11-09 | 2019-07-05 | 扬州大学 | A kind of ZnO sensing electrode material preparation method of porous nano pie structure |
| CN108365211A (en) * | 2018-04-20 | 2018-08-03 | 合肥工业大学 | A kind of preparation method of nitrogen-doped carbon cladding zinc telluridse nano wire and its application as anode material of lithium-ion battery |
| CN109786666A (en) * | 2019-03-21 | 2019-05-21 | 福建蓝海黑石新材料科技有限公司 | A kind of nitrogen-doped carbon coated Si nano particle composite material, preparation method and application |
| CN112745559A (en) * | 2020-12-23 | 2021-05-04 | 河南工业大学 | Polymer dielectric elastomer and preparation method and application thereof |
| CN112745559B (en) * | 2020-12-23 | 2023-02-17 | 河南工业大学 | Polymer dielectric elastomer and preparation method and application thereof |
| CN113101962A (en) * | 2021-04-25 | 2021-07-13 | 山西中科国蕴环保科技有限公司 | Porous carbon layer protection catalyst for activating persulfate, preparation method and application |
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