CN109888222A - A kind of N doping porous carbon and preparation method thereof of silver nano-grain package - Google Patents
A kind of N doping porous carbon and preparation method thereof of silver nano-grain package Download PDFInfo
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- CN109888222A CN109888222A CN201910141866.7A CN201910141866A CN109888222A CN 109888222 A CN109888222 A CN 109888222A CN 201910141866 A CN201910141866 A CN 201910141866A CN 109888222 A CN109888222 A CN 109888222A
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Abstract
The invention discloses a kind of N doping porous carbons and preparation method thereof of silver nano-grain package, and implementation steps include: first to synthesize the metal-organic framework material ZIF-8 presoma with tetrakaidecahedron pattern；High-temperature process obtains the porous carbon NPC of the N doping for the looks that hold its shape again；The cladding of silver nano-grain is finally carried out to it, the final nitrogen-doped porous carbon material for obtaining silver nano-grain package, general structure is Ag@NPC.The tetrakaidecahedron structure of its rule, can play the role of stabilizing material structure when as lithium ion battery negative material；The cladding of silver nano-grain helps to stablize the SEI film formed in electro-chemical test simultaneously, on the other hand can promote charge transfer process and lithium ion transfer speed, to achieve the purpose that improve material conductivity and chemical property.
Description
Technical field
The present invention relates to lithium ion battery negative material manufacturing technology fields, and in particular to a kind of silver nano-grain package
N doping porous carbon and preparation method thereof.
Background technique
Today's society, environmental pollution and energy shortage problem are increasingly severe, to promote the development of clean energy resource.Tool
The lithium ion battery of the advantages that standby high-energy density, high voltage and long circulation life, by the favor of numerous researchers, and gradually
It is applied in various electronic equipments.But there are still many problems for the application of lithium ion battery, therefore researches and develops with more
The new type lithium ion battery of excellent properties is extremely urgent.Lithium ion battery negative material as lithium ion battery core material it
One, there is vital effect for improving battery overall performance.During lithium ion battery applications, using lithium metal as
When negative electrode material, the Li dendrite ash of generation leads to the safety issues such as battery short circuit；And when using graphite material as negative electrode material,
The theoretical capacity and output power of battery are lower, this be also it is very formidable, therefore, for lithium metal and graphite material can be replaced
Negative electrode material research become a kind of challenge.
The porous structure of N doping porous carbon (NPC) based on ZIF-8, maintains metal-organic framework ZIF-8
Tetrakaidecahedron structure, have pattern, duct and carbon content it is controllable, large specific surface area, the high feature of structure thermal stability, from
And it can targetedly solve the problems, such as that the existing specific capacity of lithium ion battery is low, structural stability is poor.
Summary of the invention
The present invention provides a kind of preparation methods of the N doping porous carbon of silver nano-grain package, mainly have with metal
Machine frame structure ZIF-8 obtains the more of the N doping with large specific surface area, with tetrakaidecahedron structure as presoma, calcining
Then the silver nano-grain of preparation is coated on porous carbon by hole carbon, form the nitrogen-doped porous carbon of silver nano-grain package
Material, the negative electrode material as lithium ion battery.On the one hand the consistency matter of the SEI film of carbon material can be improved in silver nano-grain
Amount reduces electrolyte loss, slows down battery capacity decaying；On the other hand it can promote charge transfer process and lithium ion transfer speed
Degree, to achieve the purpose that improve material conductivity and chemical property.
The invention is realized by the following technical scheme:
A kind of preparation method of the nitrogen-doped porous carbon material of silver nano-grain package, comprising the following steps:
1) synthesis of presoma ZIF-8: by the concentration ratio of 1mol/L, zinc nitrate hexahydrate is taken to be completely dissolved in anhydrous methanol molten
Liquid, obtained solution A；By the concentration ratio of 4mol/L, 2-methylimidazole is taken to be completely dissolved in absolute methanol solution, then presses 2- first
Base imidazoles: the ratio of 1- methylimidazole molar ratio 10:1 takes the dispersion of 1- methylimidazole wherein, obtained solution B；Solution B is uniform,
It rapidly pours into solution A, is stirred at room temperature and stands after mixing, lower layer's milkiness shape liquid is centrifuged, then with anhydrous
Methanol repeatedly washs, and product is put into aeration cabinet, is dried to obtain ZIF-8 at 60 ~ 80 DEG C；
2) synthesis of N doping porous carbon: the ZIF-8 grind into powder that will be obtained is placed in silica crucible, in vacuum tube
In formula furnace, it is passed through high-purity argon gas, throughput is controlled in 50 ~ 60ml/min, risen temperature with the heating rate of 3 ~ 5 DEG C/min
To 800 ~ 900 DEG C, after heat preservation 5 ~ 6 hours, it is down to room temperature, fluffy black powder is obtained, is ground into powder, be scattered in
In hydrochloric acid solution, it is stirred at room temperature 12 ~ for 24 hours, it is centrifuged 15 ~ 20min, and be washed with distilled water removal HCl, product is put
Enter in air dry oven, dry 3 ~ 5h, obtains N doping porous carbon NPC at 60 ~ 80 DEG C；
3) it the preparation of silver nitrate solution: by the concentration ratio of 0.1mol/L, takes silver nitrate in distilled water, is stirred under the conditions of being protected from light
Mixing dissolves silver nitrate sufficiently；
4) it coats: N doping porous carbon NPC obtained by step 2 being poured into silver nitrate solution, heating is protected from light at 100 ~ 120 DEG C and stirs
5 ~ 10min is mixed, it is after being centrifuged and repeatedly washing removal unreacted silver nitrate, final product is dry in 60 ~ 80 DEG C of baking ovens, it obtains
The nitrogen-doped porous carbon material of silver nano-grain package.
The present invention is further preferred, after step 1) solution B is uniformly mixed with solution A, by mixed solution preservative film
Sealing and standing.Sealing and standing, particle growth stable structure.
The present invention is further preferred, and the concentration of hydrochloric acid solution used in step 2 is 20 ~ 40wt%.
Another object of the present invention is to the N doping porous carbon of the silver nano-grain package of open above method preparation, knots
Structure general formula is Ag@NPC, the nucleocapsid knot that the N doping porous carbon with tetrakaidecahedron structure is core, silver nano-grain is shell cladding
Structure, 2 μm of particle diameter size or so, 8 ~ 20 nm of silver nano-grain diameter.
Further preferably, the porous carbon surface of N doping has mesoporous, and silver nano-grain is embedded in aperture.
Compared with prior art, the present invention having following obvious advantage:
1, the nitrogen-doped porous carbon material of a kind of silver nano-grain package prepared by the present invention, with metal-organic framework ZIF-
8 are used as presoma, and stability is good, can still be maintained by processing, and product has the polyhedron pattern at well-regulated ten four sides,
It can play the role of stabilizing material structure when as lithium ion battery negative material；A large amount of micropores and mesoporous are existed simultaneously, it can
In Electolyte-absorptive dissociate fluorine ion, the side reaction between inhibitory activity material and electrolyte, regulatable cellular structure and
Excellent chemical property；And synthesis step is simple and efficient.
2, the present invention in the synthesis step of presoma ZIF-8, be added 1- methylimidazole, its object is to 2- methyl miaow
Azoles contention coordination, slows down 2-methylimidazole and Zn2+Complexation reaction can be with metal because the coordination site of two kinds of materials is different
The speed of coordination is just different, plays the role of a contention coordination in this way to slow down the speed of nucleation and increases ZIF-8 particle
Size dimension, because if fast nucleation just will form small volume.It factually tests and learns, simple 2-methylimidazole and Zn2+'s
Coordination, the particle diameter of formation is 200-500 nanometers general, and can be promoted to 2 microns after 1- methylimidazole contention is added, body
Product increases, so that N doping porous carbon specific surface area increases after calcining.
3, in N doping porous carbon of the present invention synthesis, temperature is risen to 800 with the heating rate of 3 ~ 5 DEG C/min ~
900 DEG C, heat preservation is heat-treated for 5 ~ 6 hours, and the control of temperature and time effectively makes NPC made of calcining have 8-20 nm
Mesoporous, if temperature is high, pore size is too big, and structure is easy for collapsing, but if temperature is low, organic principle is non-volatile, plugging hole,
Cause mesopore diameter too small, silver nano-grain is not easy to be embedded in again, and the application mesoporous pore size size is suitable, has both been easy to silver nanoparticle
Particle is embedded in aperture, again limits arbitrarily growing up for silver nano-grain, particle size is relatively uniform.
4, in circulating battery charging process, carbon material contacts poor quality easy to form, the biggish SEI of thickness with electrolyte
Film, SEI constantly increase, and consume electrolyte, will cause the acceleration decaying of battery capacity.The present invention is embedded in using silver nano-grain
N doping porous carbon is surface mesoporous middle to be coated comprehensively, it is possible to reduce contact of the electrolyte with porous carbon improves SEI film quality
Amount, is the excellence conductor of Li+, lithium ion can be allowed to be transmitted wherein；Silver nano-grain also has simultaneously leads well
Electrically, charge transfer process and lithium ion transfer speed can be promoted, improves material conductivity and chemical property to reach
Purpose.
Detailed description of the invention
Fig. 1 is the scanning electron microscope diagram of the nitrogen-doped porous carbon material of silver nano-grain package in embodiment 1.
Fig. 2 is the transmission electron microscope picture of the nitrogen-doped porous carbon material of silver nano-grain package in embodiment 1.
Fig. 3 is the Raman map of the nitrogen-doped porous carbon material of silver nano-grain package in embodiment 1.
Specific embodiment
A specific embodiment of the invention is described further below in conjunction with attached drawing.
Embodiment 1
1, the synthesis of presoma ZIF-8: 0.2 mol zinc nitrate hexahydrate is weighed in the beaker of 1000 ml, into beaker
200 ml absolute methanol solutions are added, 5 min, which are stirred at room temperature, dissolves zinc nitrate sufficiently, and solution A is prepared；Claim
It takes 0.8 mol 2-methylimidazole in the beaker of 500 ml, 200 ml absolute methanol solutions is added into beaker, in room
5 min of the lower stirring of temperature dissolve 2-methylimidazole sufficiently；Then the 1- methyl imidazole solution for measuring 6.28 ml, is poured into
In above-mentioned solution, and quickly stirring is allowed to be well-dispersed in solution, and solution B is prepared.Solution B uniformly, is rapidly fallen
Enter in solution A, 5 min, which are stirred at room temperature, makes the two after evenly mixing, and mixed solution is sealed with preservative film, quiet at room temperature
12 h are set, lower layer's milkiness shape liquid is centrifuged 5 min, is then repeatedly washed with anhydrous methanol, product is put into aeration-drying
In case, dry 3 h, obtain ZIF-8 at 60 DEG C.
2, the synthesis of the N doping porous carbon of silver nano-grain package: obtained ZIF-8 is ground into powder, is placed
In silica crucible.In vacuum tube furnace, it is passed through high-purity argon gas, throughput is controlled in 50 ml/min, with 3 DEG C/min's
Temperature is risen to 800 DEG C by heating rate, is kept the temperature 5 hours, is cooled to room temperature, obtains fluffy black powder, be ground into
It is powdered, hydrochloric acid solution (100 ml, 20wt%) are scattered in, 12 h are stirred at room temperature, are centrifuged 15 min, and use distilled water
Wash 3 ~ 5 removal HCl.Product is put into air dry oven, dry 3 h, it is porous to obtain N doping at 60 DEG C
Carbon (NPC).
3,2 mmol silver nitrates are weighed in beaker, 20 ml distilled water are added, 5 are stirred under the conditions of being protected from light
Min dissolves silver nitrate sufficiently.
4, gained N doping porous carbon is poured into silver nitrate solution, 5 min of heating stirring is protected from light at 100 DEG C, centrifugation is simultaneously
It is repeatedly after washing removal unreacted silver nitrate, final product is dry in 60 DEG C of baking ovens, obtain the nitrogen of silver nano-grain package
Doped porous carbon material.
Embodiment 2
1, the synthesis of presoma ZIF-8: 0.3 mol zinc nitrate hexahydrate is weighed in the beaker of 1000 ml, into beaker
300 ml absolute methanol solutions are added, 8 min, which are stirred at room temperature, dissolves zinc nitrate sufficiently, and solution A is prepared；Claim
It takes 1.2 mol 2-methylimidazoles in the beaker of 500 ml, 300 ml absolute methanol solutions is added into beaker, in room
8 min of the lower stirring of temperature dissolve 2-methylimidazole sufficiently；Then the 1- methyl imidazole solution for measuring 9.42 ml, is poured into
In above-mentioned solution, and quickly stirring is allowed to be well-dispersed in solution, and solution B is prepared.Solution B uniformly, is rapidly fallen
Enter in solution A, 8 min, which are stirred at room temperature, makes the two after evenly mixing, and mixed solution is sealed with preservative film, quiet at room temperature
18 h are set, lower layer's milkiness shape liquid is centrifuged 8 min, is then repeatedly washed with anhydrous methanol, product is put into aeration-drying
In case, dry 4 h, obtain ZIF-8 at 70 DEG C.
2, the synthesis of the N doping porous carbon of silver nano-grain package: obtained ZIF-8 is ground into powder, is placed
In silica crucible.In vacuum tube furnace, it is passed through high-purity argon gas, throughput is controlled in 55 ml/min, with 4 DEG C/min's
Temperature is risen to 850 DEG C by heating rate, is kept the temperature 5.5 hours, is cooled to room temperature, obtains fluffy black powder, is ground
At powdered, hydrochloric acid solution (125 ml, 30wt%) are scattered in, 18 h are stirred at room temperature, are centrifuged 18 min, and with distilling
3 ~ 5 removal HCl of water washing.Product is put into air dry oven, dry 4 h, it is more to obtain N doping at 70 DEG C
Hole carbon (NPC).
3,2.5 mmol silver nitrates are weighed in beaker, 25 ml distilled water are added, 8 are stirred under the conditions of being protected from light
Min dissolves silver nitrate sufficiently.
4, gained N doping porous carbon is poured into silver nitrate solution, 8 min of heating stirring is protected from light at 110 DEG C, centrifugation is simultaneously
It is repeatedly after washing removal unreacted silver nitrate, final product is dry in 70 DEG C of baking ovens, obtain the nitrogen of silver nano-grain package
Doped porous carbon material.
Embodiment 3
1, the synthesis of presoma ZIF-8: 0.4 mol zinc nitrate hexahydrate is weighed in the beaker of 1000 ml, into beaker
400 ml absolute methanol solutions are added, 10 min, which are stirred at room temperature, dissolves zinc nitrate sufficiently, and solution A is prepared；
1.6 mol 2-methylimidazoles are weighed in the beaker of 500 ml, 400 ml absolute methanol solutions are added into beaker,
Stirring 10 min at room temperature dissolves 2-methylimidazole sufficiently；Then the 1- methyl imidazole solution of 12.56 ml is measured,
It pours into above-mentioned solution, and quickly stirring is allowed to be well-dispersed in solution, and solution B is prepared.Uniformly, quickly by solution B
Ground pours into solution A, and 10 min, which are stirred at room temperature, makes the two after evenly mixing, mixed solution is sealed with preservative film, room temperature
Lower layer's milkiness shape liquid is centrifuged 10 min, is then repeatedly washed with anhydrous methanol, product is put into ventilation by 24 h of lower standing
In drying box, dry 5 h, obtain ZIF-8 at 80 DEG C.
2, the synthesis of the N doping porous carbon of silver nano-grain package: obtained ZIF-8 is ground into powder, is placed
In silica crucible.In vacuum tube furnace, it is passed through high-purity argon gas, throughput is controlled in 60 ml/min, with 5 DEG C/min's
Temperature is risen to 900 DEG C by heating rate, is kept the temperature 6 hours, is cooled to room temperature, obtains fluffy black powder, be ground into
It is powdered, hydrochloric acid solution (150 ml, 40wt%) are scattered in, 24 h are stirred at room temperature, are centrifuged 20 min, and use distilled water
Wash 3 ~ 5 removal HCl.Product is put into air dry oven, dry 5 h, it is porous to obtain N doping at 80 DEG C
Carbon (NPC).
3,3 mmol silver nitrates are weighed in beaker, 30 ml distilled water are added, 10 are stirred under the conditions of being protected from light
Min dissolves silver nitrate sufficiently.
4, gained N doping porous carbon is poured into silver nitrate solution, 10 min of heating stirring is protected from light at 120 DEG C, be centrifuged
It is and repeatedly after washing removal unreacted silver nitrate, final product is dry in 80 DEG C of baking ovens, obtain silver nano-grain package
Nitrogen-doped porous carbon material.
The above description is only an embodiment of the present invention, is not intended to limit the present invention, all using equivalent replacement or equivalent exchange
Mode technical solution obtained, falls within the scope of protection of the present invention.
The result of embodiment 1
Using FEI Quanta 450FEG type field emission scanning electron microscope (SEM) to sample prepared in embodiment 1 into
Row morphology characterization, as shown in Figure 1.SEM result finds out, the nitrogen-doped porous carbon material of silver nano-grain package, and particle is uniform
Dispersion, without apparent agglomeration, tetrakaidecahedron structure is presented in granule-morphology, and granular size is about 2 μm.
Using the TECNAI F30 high-resolution-ration transmission electric-lens (TEM) of Dutch FEI company production to made in embodiment 1
Standby sample is characterized, as shown in Figure 2.Schemed by TEM, it is apparent that particle surface is uniform-distribution with many silver nanoparticles
Particle, the nanoparticle size is relatively uniform, and the diameter of particle is mainly distributed on 8 ~ 20 nm.
Using the TriVista CRS557 micro-Raman spectroscopy of Princeton company to prepared in embodiment 1
Sample characterized, as a result as shown in figure 3, peak in figure at the position D indicates the disordered portion of carbon, the peak at the position G
Indicate carbon has preamble section, and the peak D is apparently higher than the peak G, illustrates that the N doping of prepared silver nano-grain package is porous
Carbon in carbon material mainly exists with disordered state, and there are a large amount of defects in disordered state structure, these defects can promote lithium ion
Diffusion and insertion, increase active site.
Claims (5)
1. a kind of preparation method of the nitrogen-doped porous carbon material of silver nano-grain package, which comprises the following steps:
1) synthesis of presoma ZIF-8: by the concentration ratio of 1mol/L, zinc nitrate hexahydrate is taken to be completely dissolved in anhydrous methanol molten
Liquid, obtained solution A；By the concentration ratio of 4mol/L, 2-methylimidazole is taken to be completely dissolved in absolute methanol solution, then presses 2- first
Base imidazoles: the ratio of 1- methylimidazole molar ratio 10:1 takes the dispersion of 1- methylimidazole wherein, obtained solution B；Solution B is uniform,
It rapidly pours into solution A, is stirred at room temperature and stands after mixing, lower layer's milkiness shape liquid is centrifuged, then with anhydrous
Methanol repeatedly washs, and product is put into aeration cabinet, is dried to obtain ZIF-8 at 60 ~ 80 DEG C；
2) synthesis of N doping porous carbon: the ZIF-8 grind into powder that will be obtained is placed in silica crucible, in vacuum tube
In formula furnace, it is passed through high-purity argon gas, throughput is controlled in 50 ~ 60ml/min, risen temperature with the heating rate of 3 ~ 5 DEG C/min
To 800 ~ 900 DEG C, after heat preservation 5 ~ 6 hours, it is down to room temperature, fluffy black powder is obtained, is ground into powder, be scattered in
In hydrochloric acid solution, it is stirred at room temperature 12 ~ for 24 hours, it is centrifuged 15 ~ 20min, and be washed with distilled water removal HCl, product is put
Enter in air dry oven, dry 3 ~ 5h, obtains N doping porous carbon NPC at 60 ~ 80 DEG C；
3) it the preparation of silver nitrate solution: by the concentration ratio of 0.1mol/L, takes silver nitrate in distilled water, is stirred under the conditions of being protected from light
Mixing dissolves silver nitrate sufficiently；
4) it coats: N doping porous carbon NPC obtained by step 2 being poured into silver nitrate solution, heating is protected from light at 100 ~ 120 DEG C and stirs
5 ~ 10min is mixed, it is after being centrifuged and repeatedly washing removal unreacted silver nitrate, final product is dry in 60 ~ 80 DEG C of baking ovens, it obtains
The nitrogen-doped porous carbon material of silver nano-grain package.
2. a kind of preparation method of the N doping porous carbon of silver nano-grain package according to claim 1, it is characterised in that:
After step 1) solution B and solution A are uniformly mixed, by mixed solution preservative film sealing and standing.
3. a kind of preparation method of the N doping porous carbon of silver nano-grain package according to claim 1, it is characterised in that:
The concentration of hydrochloric acid solution used in step 2 is 20 ~ 40wt%.
4. according to claim 1, the N doping porous carbon of the silver nano-grain package of 2 or 3 the methods preparation, feature exist
In: general structure is Ag@NPC, the core that the N doping porous carbon with tetrakaidecahedron structure is core, silver nano-grain is shell cladding
Shell structure, 2 μm of particle diameter size or so, 8 ~ 20 nm of silver nano-grain diameter.
5. the N doping porous carbon of silver nano-grain package according to claim 4, it is characterised in that: N doping porous carbon
Surface have it is mesoporous, silver nano-grain be embedded in aperture in.
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| CN111268673A (en) * | 2020-02-11 | 2020-06-12 | 西安理工大学 | Preparation method of supercapacitor electrode material taking foamed nickel as template |
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| CN111842923A (en) * | 2020-07-14 | 2020-10-30 | 西安工程大学 | Preparation method of silver nanowire/biomass porous carbon electromagnetic wave absorption material |
| CN112421062A (en) * | 2020-11-11 | 2021-02-26 | 北京化工大学 | Preparation method of monoatomic iron dispersion/silver nanoparticle composite structure catalyst |
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| CN111268673A (en) * | 2020-02-11 | 2020-06-12 | 西安理工大学 | Preparation method of supercapacitor electrode material taking foamed nickel as template |
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| CN111842923A (en) * | 2020-07-14 | 2020-10-30 | 西安工程大学 | Preparation method of silver nanowire/biomass porous carbon electromagnetic wave absorption material |
| CN112421062A (en) * | 2020-11-11 | 2021-02-26 | 北京化工大学 | Preparation method of monoatomic iron dispersion/silver nanoparticle composite structure catalyst |
| CN114497580B (en) * | 2020-11-12 | 2023-09-19 | 中国科学院大连化学物理研究所 | Electrode and application of electrode serving as negative electrode in all-vanadium redox flow battery |
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| KR102631886B1 (en) * | 2021-04-09 | 2024-02-01 | 재단법인대구경북과학기술원 | Negative electrode active material for battery and manufacturing method thereof |
| CN113069940B (en) * | 2021-04-20 | 2023-03-07 | 江苏理工学院 | Preparation method of anti-pollution membrane |
| CN113069940A (en) * | 2021-04-20 | 2021-07-06 | 江苏理工学院 | Preparation method of anti-pollution membrane |
| CN113871599A (en) * | 2021-09-28 | 2021-12-31 | 广西超威鑫锋能源有限公司 | Lead-coated nitrogen-doped carbon composite material, preparation thereof and application thereof in lead-carbon battery |
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Application publication date: 20190614 |