CN110247030A - Method for preparing three-dimensional porous microspheres surrounded by nitrogen/sulfur co-doped carbon nanosheets embedded with metal/carbon yolk shell structures - Google Patents
Method for preparing three-dimensional porous microspheres surrounded by nitrogen/sulfur co-doped carbon nanosheets embedded with metal/carbon yolk shell structures Download PDFInfo
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- CN110247030A CN110247030A CN201910435949.7A CN201910435949A CN110247030A CN 110247030 A CN110247030 A CN 110247030A CN 201910435949 A CN201910435949 A CN 201910435949A CN 110247030 A CN110247030 A CN 110247030A
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
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- H01M4/362—Composites
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- H—ELECTRICITY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H—ELECTRICITY
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention provides a method for preparing a three-dimensional porous microsphere surrounded by nitrogen/sulfur co-doped carbon nanosheets embedded with a metal/carbon yolk shell structure, which comprises the following steps: preparing a precursor: selecting antimony acetate, ammonium citrate and sodium chloride as raw materials, mixing and dissolving in deionized water, and spraying the obtained uniform mixed solution into balls by using a spray dryer to prepare a precursor; preparing a three-dimensional porous microsphere composite material formed by enclosing nitrogen/sulfur co-doped carbon nanosheets embedded with antimony/carbon yolk shell structures: and (3) placing the precursor prepared in the step (1) in the midstream of a tubular furnace, placing thiourea in the upstream, and obtaining the three-dimensional porous microsphere composite material formed by the nitrogen/sulfur co-doped carbon nanosheets embedded with the antimony/carbon yolk shell structure in a multi-step manner in one pot. The prepared three-dimensional porous microsphere composite material formed by surrounding nitrogen/sulfur co-doped carbon nanosheets embedded with antimony/carbon yolk shell structures is used as a negative electrode of a sodium ion battery.
Description
Technical field
Embedded metal/carbon yolk shell structure nitrogen/sulphur codope carbon is prepared using spray drying process the present invention relates to a kind of
The method for the three-dimensional porous microballoon that nanometer sheet surrounds, and very-high performance can be shown in the test of sodium-ion battery cathode, belong to
In nanocomposite technology of preparing and battery applications technical field.
Background technique
Highest attention with people to renewable energy utilization, the development and application of lithium/sodium-ion battery are extremely urgent.Mesh
Before, lithium/sodium-ion battery positive material preparation process is improved day by day, and performance has also substantially met industrialization demand.However it is negative
The development and application of pole material rest on phase of basic research more, since preparation process (hydro-thermal, solvent heat and electrostatic spinning etc.) produces
Measure low, process is complicated and valuableness causes to be difficult to industrialized production.Another critical issue is the production that many preparation methods obtain
It is difficult to possess cycle performance stable under high current when object is as lithium/sodium-ion battery cathode, this strongly limits industrialization to answer
Possibility.Therefore extensive efficiently preparation is in lithium/sodium-ion battery cathode with the electrode material of big multiplying power long circulating performance
Material is still a problem.
The three-dimensional porous carbosphere of nitrogen/sulphur codope has big specific surface area, high mechanical strength, excellent conduction
Property, thus it can be applied in the battery cathode such as lithium, sodium and potassium field, the nitrogen and sulphur atom of pore structure abundant and doping make
Obtaining the porous carbon microsphere can be by as the embedded other metal-based nano material of load matrix.Yolk shell structure has been found in electricity
Metal volume expansion can be effectively relieved in the charge and discharge process of pond, increase cyclical stability.Yolk shell structure combination nitrogen/sulphur is co-doped with
Miscellaneous three-dimensional porous carbosphere composite material can be used as high-performance sodium-ion battery and lithium ion battery plus-negative plate material, or even be expected to
Excellent properties are shown in fields such as electrochemical capacitance, lithium-sulfur cell, lithium metal battery and electrocatalytic hydrogen evolutions.
Summary of the invention
The object of the present invention is to provide one kind can preparation of industrialization embedded metal/carbon yolk shell structure nitrogen/sulphur codope
The method for the three-dimensional porous microballoon that carbon nanosheet surrounds；This method process is simple, efficient, low in cost, reproducible, obtains
The three-dimensional porous microballoon composite material pattern uniform one that nitrogen/sulphur codope carbon nanosheet of embedded antimony/carbon yolk shell structure surrounds
Cause, yield it is big, while when applying in sodium-ion battery cathode, even if can also show the overlength circulation longevity under high current
Life.Technical solution is as follows:
A kind of three-dimensional porous microballoon for preparing embedded metal/carbon yolk shell structure nitrogen/sulphur codope carbon nanosheet and surrounding
Method, including the following steps:
1) presoma is prepared
Select antimony acetate, ammonium citrate and sodium chloride be raw material mixed dissolution in deionized water, resulting uniform will mix
It closes solution and is sprayed balling-up using spray dryer, so that presoma be made.
2) the three-dimensional porous microballoon that nitrogen/sulphur codope carbon nanosheet of the embedded antimony/carbon yolk shell structure of preparation surrounds is compound
Material
Presoma made from step 1) is placed on tube furnace middle reaches, thiocarbamide is placed on upstream, the step 1 of one pot of multistep:
280 DEG C are warming up to 1 DEG C/min under high-purity argon gas atmosphere, 2h is kept the temperature, has obtained containing Sb this moment2S3Intermediate product, be denoted as
NaCl@N,S-carbon/Sb2S3；Step 2: being warming up to 450 DEG C under high-purity argon gas atmosphere, then switches to hydrogen-argon-mixed heat preservation
2h, currently available intermediate product are transformed into Sb, are denoted as NaCl@N, S-carbon/Sb；Step 3: it heats up under high-purity argon gas atmosphere
To 600 DEG C, it is cooled to room temperature after using argon gas to keep the temperature 2h as carrier gas, obtains calcined product, be denoted as NaCl@Sb@NS-
3DPCMSs-120 constructs egg using the physical property that the low-melting characteristic of Sb acutely distils at 500 DEG C or more in insulating process
Yellow shell structure；NaCl@Sb@NS-3DPCMSs-120 is removed into NaCl again, vacuum drying obtains Sb@NS-3DPCMSs-120, i.e.,
Obtain the three-dimensional porous microballoon composite material that nitrogen/sulphur codope carbon nanosheet of embedded antimony/carbon yolk shell structure surrounds.
1) in, according to Sb3+: C and C:Na+The ratio between amount of substance be 1:(12-18) and (25-30): 100 relationship selects original
Material.
The three-dimensional porous microballoon that prepared embedded antimony/carbon yolk shell structure nitrogen/sulphur codope carbon nanosheet surrounds is multiple
Condensation material is used as sodium-ion battery cathode.
Compared with the prior art, the method for the present invention has the advantage that (1) using NaCl (recyclable to recycle) as mould
Plate uses cheap (CH3COO)3Sb、C6H5O7(NH4)3And CH4N2Cost is greatly saved as raw material in S；(2) prepared
The process for the three-dimensional porous microballoon composite material that nitrogen/sulphur codope carbon nanosheet of embedded antimony/carbon yolk shell structure surrounds is continuous
Property it is high；(3) product purity is high, and yield is big, and controllability is good, is expected to that the following heavy industrialization is promoted to prepare the other of similar structures
The practical application of composite material.
Detailed description of the invention
Fig. 1 is the N, S-carbon/Sb prepared by the present invention after washing removes NaCl2S3、N,S-carbon/Sb、 Sb@
The XRD spectrum of NS-3DPCMSs-120；
Fig. 2 is presoma NaCl@(CH prepared by the present invention3COOH)3Sb-C6H5O7(NH4)3SEM image；
The SEM image that Fig. 3 is the Sb@NS-3DPCMSs-120 after washing removes NaCl prepared by the present invention；
The TEM image that Fig. 4 is the Sb@NS-3DPCMSs-120 after washing removes NaCl prepared by the present invention；
The HRTEM image that Fig. 5 is the Sb@NS-3DPCMSs-120 after washing removes NaCl prepared by the present invention；
Fig. 6 is Sb@NS-3DPCMSs-120 composite material prepared by the present invention and its carbon skeleton (note NS-3DPCMSs)
With the multiplying power and 100mAg of commercial Sb micron particles (Pure-Sb)-1Cycle performance under current density；
Fig. 7 is Sb@NS-3DPCMSs-120 composite material prepared by the present invention in 17Ag-1Following under current density for a long time
Ring performance
Fig. 8 is Sb@NS-3DPCMSs-120 composite material prepared by the present invention in 20Ag-1Following under current density for a long time
Ring performance
The present invention does not address place and is suitable for the prior art.
Specific embodiment
The specific embodiment of preparation method of the present invention is given below.Preparation that these embodiments are only used for that the present invention will be described in detail
Method is not intended to limit the protection scope of the claim of this application.
Technical proposal that the invention solves the above-mentioned problems be design it is a kind of by spray drying and subsequent " one pot of multistep " forge
The method for handling the three-dimensional porous microballoon that the nitrogen/sulphur codope carbon nanosheet for preparing embedded antimony/carbon yolk shell structure surrounds is burnt, it should
Preparation method uses following process route:
1) presoma is prepared
Select antimony acetate ((CH3COO)3Sb), ammonium citrate (C6H5O7(NH4)3) and sodium chloride (NaCl) be raw material mixing
Dissolution in deionized water, utilizes magnetic stirrer 9h at room temperature, and resulting uniform mixed solution is done using spraying
Dry machine spraying balling-up under 175 DEG C of inlet air temperature, so that presoma, which is made, (is denoted as NaCl@(CH3COOH)3Sb-C6H 5O7
(NH4)3).The white powder of acquisition is collected spare.
2) the three-dimensional porous microballoon that nitrogen/sulphur codope carbon nanosheet of the embedded antimony/carbon yolk shell structure of preparation surrounds is compound
The method of material
Presoma made from step 1 is placed on tube furnace middle reaches, thiocarbamide (CH4N2S provides the sulphur source of reaction and doping)
It is placed on upstream.The step 1 of one pot of multistep: being warming up to 280 DEG C under high-purity argon gas atmosphere with 1 DEG C/min, keeps the temperature 2h, obtains this moment
Contain Sb2S3Intermediate product (be denoted as NaCl@N, S-carbon/Sb2S3)；Step 2: 450 are warming up under high-purity argon gas atmosphere
DEG C, then hydrogen-argon-mixed heat preservation 2h is switched to, currently available intermediate product is transformed into Sb and (is denoted as NaCl@N, S-carbon/
Sb)；Step 3: being warming up to 600 DEG C under high-purity argon gas atmosphere, be cooled to room temperature, calcined after using argon gas to keep the temperature 2h as carrier gas
Product (is denoted as NaCl@Sb@NS-3DPCMSs-120), using Sb fusing point low (630 DEG C) at 500 DEG C or more in insulating process
The physical property acutely to distil constructs yolk shell structure.NaCl@Sb@NS-3DPCMSs-120 is washed 3 times through deionized water again
Above to remove NaCl, 60 DEG C of vacuum drying obtain Sb@NS-3DPCMSs-120 for 24 hours to get embedded antimony/carbon yolk shell structure is arrived
The three-dimensional porous microballoon composite material that surrounds of nitrogen/sulphur codope carbon nanosheet.
Embodiment 1
According to Sb3+: C and C:Na+The ratio between amount of substance be 1:15 and 28:100 relationship, by (the CH of 0.95g3COO)3Sb,
1.94g C6H5O7(NH4)3It is dissolved in 80mL deionized water with the NaCl of 10g, 9h is stirred at room temperature to guarantee C6H5O7(NH4)3
It is sufficiently complexed with metal salt.Gained uniform solution is spray-dried by spray dryer, spray dryer passes in and out wind-warm syndrome
Degree is respectively 175 DEG C and 90 DEG C.In the process, by (CH3COO)3Sb、C6H5O7(NH4)3It is self-assembly of with NaCl hollow
Ball, the size of ball is at normal distribution.Since at high temperature, the water of droplet surface volatilizees rapidly, the water of drop internal is carried
NaCl migrate to surface, cause it to be self-assembly of georama presoma NaCl@(CH in a very short period of time3COOH)3Sb-C6H5O7(NH4)3.Presoma is placed in tube furnace middle reaches, excessive thiocarbamide is placed in upstream and (is generated H by thermal decomposition2S), first
Lead to argon gas to exclude air, be then warming up to 280 DEG C with 1 DEG C/min, keeps the temperature 2h；450 DEG C are warming up to 8 DEG C/min again, then is changed
At 20% hydrogen-argon-mixed heat preservation 2h；It changes carrier gas into pure argon again, is then warming up to 600 DEG C with 8 DEG C/min, after keeping the temperature 2h
It is cooled to room temperature, obtains calcined product NaCl@[email protected] times by product deionized water and ethanol washing,
It is dried in vacuo at 60 DEG C and obtains sample Sb@NS-3DPCMSs-120 for 24 hours.
Embodiment 2
According to Sb3+: C and C:Na+The ratio between amount of substance be 1:15 and 28:100 relationship, by (the CH of 4.3g3COO)3Sb,
8.74g C6H5O7(NH4)3It is dissolved in 355mL deionized water with the NaCl of 45g, 6h is stirred at room temperature to guarantee C6H5O7
(NH4)3It is sufficiently complexed with metal salt.Gained uniform solution is spray-dried by spray dryer, spray dryer disengaging
Air temperature is respectively 180 DEG C and 90 DEG C.Presoma is placed in tube furnace middle reaches, excessive thiocarbamide is placed in upstream, first lead to argon gas with
Air is excluded, is then warming up to 280 DEG C with 1 DEG C/min, keeps the temperature 100min；450 DEG C are warming up to 5 DEG C/min again, then is changed into
15% hydrogen-argon-mixed heat preservation 2h；It changes carrier gas into pure argon again, is then warming up to 600 DEG C with 5 DEG C/min, keep the temperature cold after 2h
But to room temperature, calcined product NaCl@Sb@NS-3DPCMSs-120 is obtained.Product is washed with deionized more than three times, 70
It is dried in vacuo 12h at DEG C and obtains sample Sb@NS-3DPCMSs-120.
Claims (3)
1. a kind of prepare three-dimensional porous microballoon that embedded metal/carbon yolk shell structure nitrogen/sulphur codope carbon nanosheet surrounds
Method, including the following steps:
1) presoma is prepared
Select antimony acetate, ammonium citrate and sodium chloride be raw material mixed dissolution in deionized water, will it is resulting it is uniform mix it is molten
Liquid is sprayed balling-up using spray dryer, so that presoma be made.
2) the three-dimensional porous microballoon composite material that nitrogen/sulphur codope carbon nanosheet of embedded antimony/carbon yolk shell structure surrounds is prepared
Presoma made from step 1) is placed on tube furnace middle reaches, thiocarbamide is placed on upstream, the step 1 of one pot of multistep: high-purity
280 DEG C are warming up to 1 DEG C/min under argon atmosphere, 2h is kept the temperature, has obtained containing Sb this moment2S3Intermediate product, be denoted as NaCl@
N,S-carbon/Sb2S3；Step 2: being warming up to 450 DEG C under high-purity argon gas atmosphere, then switches to hydrogen-argon-mixed heat preservation 2h, currently
Obtained intermediate product is transformed into Sb, is denoted as NaCl@N, S-carbon/Sb；Step 3: 600 are warming up under high-purity argon gas atmosphere
DEG C, it is cooled to room temperature after using argon gas to keep the temperature 2h as carrier gas, obtains calcined product, be denoted as NaCl@Sb@NS-3DPCMSs-120,
Yolk shell structure is constructed using the physical property that the low-melting characteristic of Sb acutely distils at 500 DEG C or more in insulating process；Again
NaCl@Sb@NS-3DPCMSs-120 is removed into NaCl, vacuum drying obtain Sb@NS-3DPCMSs-120 to get to embedded antimony/
The three-dimensional porous microballoon composite material that the nitrogen of carbon yolk shell structure/sulphur codope carbon nanosheet surrounds.
2. the method according to claim 1, wherein in 1), according to Sb3+: C and C:Na+The ratio between amount of substance be
1:(12-18) and (25-30): 100 relationship selects raw material.
3. embedded antimony prepared by claim 1/carbon yolk shell structure nitrogen/sulphur codope carbon nanosheet surrounds three-dimensional porous
Microballoon composite material is used as sodium-ion battery cathode.
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| CN110739449A (en) * | 2019-09-26 | 2020-01-31 | 天津大学 | Preparation of Embedded FeS2Method for preparing three-dimensional microspheres surrounded by nitrogen/sulfur co-doped carbon nanosheets of nanoparticles |
| CN111600032A (en) * | 2020-05-27 | 2020-08-28 | 新昌县品宏科技有限公司 | SnSb alloy-carbon nanofiber sodium ion battery negative electrode material and preparation method thereof |
| CN112479258A (en) * | 2020-12-17 | 2021-03-12 | 陕西科技大学 | Molybdenum disulfide-carbon hollow sphere and preparation method and application thereof |
| CN113130864A (en) * | 2021-03-23 | 2021-07-16 | 华南理工大学 | Chemical bond enhanced silver ear-shaped porous carbon sphere embedded with monodisperse nano alloy particles and preparation and application thereof |
| CN113130924A (en) * | 2021-04-20 | 2021-07-16 | 中国科学技术大学 | Metal-air battery catalyst, preparation method and application thereof |
| CN114464872A (en) * | 2022-01-24 | 2022-05-10 | 西安交通大学 | Application of antimony nanosheet with surface doped with halogen in lithium ion battery |
| CN114530598A (en) * | 2022-01-10 | 2022-05-24 | 广东工业大学 | Nitrogen-oxygen-sulfur doped carbon negative electrode material and preparation method and application thereof |
| CN114843459A (en) * | 2022-04-14 | 2022-08-02 | 中国科学院长春应用化学研究所 | Antimony pentasulfide-based material and preparation method and application thereof |
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Cited By (12)
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| CN110739449A (en) * | 2019-09-26 | 2020-01-31 | 天津大学 | Preparation of Embedded FeS2Method for preparing three-dimensional microspheres surrounded by nitrogen/sulfur co-doped carbon nanosheets of nanoparticles |
| CN111600032A (en) * | 2020-05-27 | 2020-08-28 | 新昌县品宏科技有限公司 | SnSb alloy-carbon nanofiber sodium ion battery negative electrode material and preparation method thereof |
| CN112479258A (en) * | 2020-12-17 | 2021-03-12 | 陕西科技大学 | Molybdenum disulfide-carbon hollow sphere and preparation method and application thereof |
| CN113130864A (en) * | 2021-03-23 | 2021-07-16 | 华南理工大学 | Chemical bond enhanced silver ear-shaped porous carbon sphere embedded with monodisperse nano alloy particles and preparation and application thereof |
| CN113130864B (en) * | 2021-03-23 | 2022-08-16 | 华南理工大学 | Chemical bond enhanced silver ear-shaped porous carbon sphere embedded with monodisperse nano alloy particles and preparation and application thereof |
| CN113130924A (en) * | 2021-04-20 | 2021-07-16 | 中国科学技术大学 | Metal-air battery catalyst, preparation method and application thereof |
| CN113130924B (en) * | 2021-04-20 | 2022-09-06 | 中国科学技术大学 | Metal-air battery catalyst, preparation method and application thereof |
| CN114530598A (en) * | 2022-01-10 | 2022-05-24 | 广东工业大学 | Nitrogen-oxygen-sulfur doped carbon negative electrode material and preparation method and application thereof |
| CN114464872A (en) * | 2022-01-24 | 2022-05-10 | 西安交通大学 | Application of antimony nanosheet with surface doped with halogen in lithium ion battery |
| CN114464872B (en) * | 2022-01-24 | 2023-08-29 | 西安交通大学 | Application of antimony nanosheets doped with halogen on surface in lithium ion battery |
| CN114843459A (en) * | 2022-04-14 | 2022-08-02 | 中国科学院长春应用化学研究所 | Antimony pentasulfide-based material and preparation method and application thereof |
| CN114843459B (en) * | 2022-04-14 | 2023-12-15 | 中国科学院长春应用化学研究所 | Antimony pentasulfide-based material and preparation method and application thereof |
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