CN108598397A - A kind of MoS2Nanometer sheet/carbon sponge composite material and preparation method and application - Google Patents
A kind of MoS2Nanometer sheet/carbon sponge composite material and preparation method and application Download PDFInfo
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- CN108598397A CN108598397A CN201810298859.3A CN201810298859A CN108598397A CN 108598397 A CN108598397 A CN 108598397A CN 201810298859 A CN201810298859 A CN 201810298859A CN 108598397 A CN108598397 A CN 108598397A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- 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
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H—ELECTRICITY
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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Abstract
The present invention relates to a kind of MoS2Nanometer sheet/carbon sponge composite material and preparation method and application, the MoS2Nanometer sheet/carbon sponge composite material is using carbon sponge as porous matrix, MoS2Nanometer sheet is at least partly coated on carbon sponge skeleton body structure surface.The preparation method is specially:In the mixed aqueous solution containing molybdenum source and sulphur source, be added carbon sponge, at a temperature of being placed in 160~200 DEG C, reaction 6~24 hours to get.Preparation process of the present invention is simple, with short production cycle, is easy to industrialization production, the MoS being prepared2/ carbon sponge composite material has the potentiality of large-scale promotion application, is particularly suitable for the negative material of kalium ion battery.
Description
Technical field
The invention belongs to function nano Material Fields, and in particular to a kind of MoS2Nanometer sheet/carbon sponge composite material and its
Preparation method and the application in kalium ion battery.
Background technology
In order to solve world energy sources crisis, the energy resource supply mode for seeking Cheap highly effective has become current research hotspot.It can
Rechargeable battery is to we provide a set of effective energy storage scheme, and wherein lithium ion battery is can to have realized that commercialization is answered now
Energy-storage system.However since lithium resource scarcity causes lithium ion battery is at high price can not large-scale application.Therefore, it explores
The rechargeable battery of novel alternative lithium ion battery is gradually by the extensive concern of researchers.Kalium ion battery is provided due to potassium mine
The abundant reserves in source and the interest for gradually causing researchers with the current potential close to lithium ion battery.Currently, potassium from
The research of sub- battery, which is concentrated mainly on, explores suitable positive and negative pole material.For kalium ion battery negative material, study at present
More is various carbonaceous materials.However carbonaceous material hinders potassium ion due to capacity ratio and the defects such as cycle life is low
Development of the battery towards high-efficiency energy-storage equipment.Therefore, the novel negative electrode material except exploration carbonaceous material is found for potassium
The development of ion battery has far reaching significance.
Transition metal selenides molybdenum disulfide due to can with alkali metal ion occur can inverse permutation react generation alloy and
It is studied to be applied in lithium ion battery and anode material of lithium-ion battery, and show good capacity ratio and cyclicity
Energy.The research that molybdenum disulfide nano sheet is used as kalium ion battery negative material is currently reported, but specific capacity is not still high.Two
Molybdenum sulfide nanometer sheet and the composite material of three-dimensional carbon sponge material are reported at present as potassium ion negative battery material.By two sulphur
Change molybdenum nanometer sheet and three-dimensional carbon sponge be combined with each other can not only improve active material and electrolyte contact area and also can
The conductivity of electrode material is improved to improve the performance of battery.Molybdenum disulfide nano sheet is used for three-dimensional carbon sponge composite material
Kalium ion battery negative material has the energy-storage property for expanding kalium ion battery negative material and improving kalium ion battery
Important guidance and reference.
Invention content
The purpose of the present invention is to provide a kind of MoS prepared by simple, efficient, low cost2Nanometer sheet/carbon sponge composite wood
Material.
The MoS2Nanometer sheet/carbon sponge composite material, using carbon sponge as porous matrix, MoS2Nanometer sheet is at least partly
It is coated on the surface of the skeleton structure of the carbon sponge.
Wherein, the carbon sponge is three-dimensional bridge crosslinking structure;The carbon sponge of this three-dimensional framework bridge crosslinking structure has specific surface
The big feature of product;It can repeat to contact with electrolyte, effectively improve specific capacity.It can directly carrying active substance MoS2Nanometer sheet conduct
Collector.
Preferably, the carbon sponge is the three-dimensional bridge crosslinking structure of N doping.It can be effectively improved using the carbon sponge of N doping
The electric conductivity of carbon.
Preferably, the MoS2Nanometer sheet is uniformly coated on the table of the skeleton structure of the carbon sponge in the form of cluster
Face.
The surface of carbon sponge skeleton structure refers specifically to the total of carbon sponge, i.e. exposed part has all coated MoS2It receives
Rice piece, as shown in Figure 2.
Second object of the present invention is to provide a kind of MoS2The preparation method of nanometer sheet/carbon sponge composite material, tool
Body is:In the mixed aqueous solution containing molybdenum source and sulphur source, carbon sponge is added, at a temperature of being placed in 160~200 DEG C, reaction 6~
24 hours to get.
Wherein, the one kind of the molybdenum source in sodium molybdate, potassium molybdate, ammonium molybdate;
The one kind of the sulphur source in thiocarbamide, thioacetamide, vulcanized sodium;
Preferably, the molar ratio of the molybdenum source and sulphur source is 1:(1~3).
Wherein, further include activator in the mixed aqueous solution, the activator is polyethylene glycol;Selected from polyethylene glycol
1000, one or more in polyethylene glycol 2000, Macrogol 6000, polyethylene glycol 10000;
Preferably, the dosage of the activator accounts for the 20%~35% of molybdenum source and sulphur source gross mass.
Preferably, the temperature of the reaction is 170~230 DEG C, preferably 190~210 DEG C;
The time of the reaction is 6~30 hours, preferably 12~26 hours, most preferably 23~25 hours.
The present invention provides a kind of preferred embodiment, and the preparation method includes the following steps:
1) it is 1 by molar ratio:Sodium molybdate, the thiocarbamide of (1~3), and account for sodium molybdate, thiocarbamide gross mass 20%~35%
Polyethylene glycol is dissolved in deionized water, is stirred to the mixed aqueous solution of water white transparency;
2) carbon sponge is placed in the mixed aqueous solution, at a temperature of 90~210 DEG C, reaction 23~25 hours, i.e.,
.
It is of the present invention after reaction, still further comprise flushing and drying.
The flushing is specifically rinsed using ethyl alcohol.
The drying is specially:At a temperature of 50~80 DEG C, 8~15h is placed;It is preferred that at a temperature of 60 DEG C, place
12h。
Third object of the present invention is, provides above-mentioned MoS2Nanometer sheet/carbon sponge composite material is in kalium ion battery
In application.
Fourth object of the present invention is, a kind of potassium ion button cell is provided, with above-mentioned MoS2Nanometer sheet/carbon sponge
Composite material is negative material.
The MoS2 nanometer sheets/carbon sponge composite material can be specifically washed into a diameter of 8mm disks as active material electricity
Pole, electrolyte are the solution (volume of EC and DMC of the ethylene carbonate (EC) and carbonic acid dioctyl phthalate (DMC) of 1M Potassium Hexafluorophosphates
Than being 1:1), using metallic potassium as to electrode, microporous polypropylene membrane is battery diaphragm, is assembled into button cell.
Preparation method involved in the present invention is simple, raw material sources are extensive, it is at low cost, have large-scale application potentiality.And
MoS2The characteristic of semiconductor of itself and the satisfactory electrical conductivity of carbon material itself, can be conducive to electron-transport.MoS2Nanometer sheet is more
The carbon sponge structure and MoS of short ion transmission path and three-dimensional structure2Nanometer sheet high-specific surface area, it is effective to improve activity
Material and electrolyte come into full contact with to make battery specific capacity to improve.
Description of the drawings
Fig. 1 is MoS made from embodiment 12The SEM photograph of nanometer sheet cluster ball;
Fig. 2 is MoS made from embodiment 32The SEM photograph of/carbon sponge composite material;
Fig. 3 is MoS made from embodiment 42The SEM photograph of/carbon sponge composite material;
Fig. 4 is MoS made from embodiment 42The XRD spectrum of/carbon sponge composite material;
Fig. 5 is MoS made from embodiment 42Charge and discharge when/carbon sponge composite material is kalium ion battery negative material are bent
Line chart;
Fig. 6 is the specific discharge capacity cycle performance comparison diagram of three kinds of batteries in test example 1.
Specific implementation mode
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
The carbon sponge that following examples use is by taking 1cm*1cm*0.2cm as an example;It can be obtained by purchased in market or firing.It is following real
It applies example and fires acquisition with the following method.
With commercially available " wiping of nanometer cleaning sponge " of family's English brand for raw material, specifically it is made with the following method:By nanometer
Cleaning sponge wiping be placed in CVD tube furnaces center, under argon hydrogen mixed atmosphere, at 800 DEG C fire 6 hours after to get
Nitrogen-doped carbon sponge.
Embodiment 1
The present embodiment provides a kind of MoS2The preparation method of nanometer sheet cluster ball, includes the following steps:
1) 0.24g Na are weighed respectively2MoO4, 0.15g thiocarbamides and 0.12g polyethylene glycol 2000s, be dissolved in going for 32.5ml
In ionized water, 25~35min of magnetic agitation, until stirring evenly the mixed aqueous solution of water white transparency;
2) mixed aqueous solution described in step 1) is transferred in reaction kettle, at a temperature of 200 DEG C, is reacted 24 hours
Afterwards, ethyl alcohol rinses, and 12h is placed in 60 DEG C of baking oven, dries to get the MoS2Nanometer sheet cluster ball.
Fig. 1 is the MoS obtained by the present embodiment2The stereoscan photograph of nanometer sheet cluster ball.
Embodiment 2
The present embodiment provides a kind of MoS2Nanometer sheet/carbon sponge composite material, with the three-dimensional bridge crosslinking structure carbon sea of N doping
Silk floss is porous matrix, MoS2Nanometer sheet is uniformly coated on carbon sponge skeleton body structure surface in the form of cluster.
The MoS2The preparation method of nanometer sheet/carbon sponge composite material, includes the following steps:
1) 0.24g Na are weighed respectively2MoO4, 0.15g thiocarbamides and 0.12g polyethylene glycol 2000s, be dissolved in going for 32.5ml
In ionized water, 25~35min of magnetic agitation, until stirring evenly the mixed aqueous solution of water white transparency;
2) mixed aqueous solution described in step 1) is transferred in reaction kettle, and carbon sponge is placed in the mixed aqueous solution
In, at a temperature of 200 DEG C, after reacting 6 hours, ethyl alcohol rinses, and 12h is placed in 60 DEG C of baking oven, dries to get described
MoS2Nanometer sheet/carbon sponge composite material.
Embodiment 3
The present embodiment provides a kind of MoS2The preparation method of nanometer sheet/carbon sponge composite material, includes the following steps:
1) 0.24g Na are weighed respectively2MoO4, 0.15g thiocarbamides and 0.12g polyethylene glycol 2000s, be dissolved in going for 32.5ml
In ionized water, 25~35min of magnetic agitation, until stirring evenly the mixed aqueous solution of water white transparency;
2) mixed aqueous solution described in step 1) is transferred in reaction kettle, and carbon sponge is placed in the mixed aqueous solution
In, at a temperature of 200 DEG C, after reacting 12 hours, ethyl alcohol rinses, and 12h is placed in 60 DEG C of baking oven, dries to get described
MoS2Nanometer sheet/carbon sponge composite material.
If Fig. 2 is MoS obtained by the present embodiment2The SEM photograph of/carbon sponge composite material.As shown in SEM figures, reaction 12
Carbon skeleton after hour is not by MOS2Nanometer sheet is completely covered, also more white space.
Embodiment 4
The present embodiment provides a kind of MoS2The preparation method of nanometer sheet/carbon sponge composite material, includes the following steps:
1) 0.24g Na are weighed respectively2MoO4, 0.15g thiocarbamides and 0.12g polyethylene glycol 2000s, be dissolved in going for 32.5ml
In ionized water, 25~35min of magnetic agitation, until stirring evenly the mixed aqueous solution of water white transparency;
2) the step 1) mixed aqueous solution is transferred in reaction kettle, and carbon sponge is placed in the mixed aqueous solution
In, at a temperature of 200 DEG C, after reacting 24 hours, ethyl alcohol rinses, and 12h is placed in 60 DEG C of baking oven, dries to get described
MoS2Nanometer sheet/carbon sponge composite material.
Fig. 3 and Fig. 4 is MoS obtained by the present embodiment2The SEM photograph and XRD spectrum of/carbon sponge composite material.Such as
Shown in SEM figures, the carbon sponge skeleton after reacting 24 hours is by MoS2Nanometer sheet is completely covered, without white space.
Embodiment 5
The present embodiment provides a kind of MoS2The preparation method of nanometer sheet/carbon sponge composite material, includes the following steps:
1) 0.12g Na are weighed respectively2MoO4, 0.1g thiocarbamides and 0.05g polyethylene glycol 2000s, be dissolved in 32.5ml go from
In sub- water, 25~35min of magnetic agitation, until stirring evenly the mixed aqueous solution of water white transparency;
2) the step 1) mixed aqueous solution is transferred in reaction kettle, and carbon sponge is placed in the mixed aqueous solution
In, at a temperature of 200 DEG C, after reacting 24 hours, ethyl alcohol rinses, and 12h is placed in 60 DEG C of baking oven, dries to get described
MoS2Nanometer sheet/carbon sponge composite material.
Embodiment 6
The present embodiment provides a kind of MoS2The preparation method of nanometer sheet/carbon sponge composite material, includes the following steps:
1) 0.12g Na are weighed respectively2MoO4, 0.1g thiocarbamides and 0.05g Macrogol 6000s, be dissolved in 32.5ml go from
In sub- water, 25~35min of magnetic agitation, until stirring evenly the mixed aqueous solution of water white transparency;
2) 1) solution in is transferred in reaction kettle and carbon sponge is placed in the mixed aqueous solution, in 200 DEG C of temperature
Under degree, after reacting 24 hours, ethyl alcohol rinses, and 12h is placed in 60 DEG C of baking oven, dries to get the MoS2Nanometer sheet/carbon sea
Continuous composite material.
Embodiment 7
The present embodiment provides a kind of MoS2The preparation method of nanometer sheet/carbon sponge composite material, includes the following steps:
1) 0.12g Na are weighed respectively2MoO4, 0.1g thiocarbamides and 0.05g polyethylene glycol 10000, be dissolved in going for 32.5ml
In ionized water, 25~35min of magnetic agitation, until stirring evenly the mixed aqueous solution of water white transparency;
2) 1) solution in is transferred in reaction kettle and carbon sponge is placed in the mixed aqueous solution, in 200 DEG C of temperature
Under degree, after reacting 24 hours, ethyl alcohol rinses, and 12h is placed in 60 DEG C of baking oven, dries to get the MoS2Nanometer sheet/carbon sea
Continuous composite material.
Embodiment 8
The present embodiment provides a kind of potassium ion button cells, with MoS made from embodiment 42Nanometer sheet/carbon sponge composite wood
Material is negative material, and the MoS2 nanometer sheets/carbon sponge composite material is specifically washed into a diameter of 8mm disks as active material
Electrode, electrolyte are the solution (body of EC and DMC of the ethylene carbonate (EC) and carbonic acid dioctyl phthalate (DMC) of 1M Potassium Hexafluorophosphates
Product is than being 1:1), using metallic potassium as to electrode, microporous polypropylene membrane is battery diaphragm, is assembled into potassium ion button cell.
Test example 1
By MoS made from embodiment 12MoS is made in nanometer sheet cluster ball, individual carbon sponge, embodiment 42Nanometer sheet/carbon
Sponge composite material is tested for the property as negative material;
First group:Individual MoS2Nanometer sheet cluster ball assembles half-cell step:Using DMF as solvent, pole piece uses matter
Amount is than being MoS2 nanometer sheet cluster balls:PVDF:Acetylene black is 7:2:1 slurry, and coated in being placed in 80 DEG C true on copper foil
Dry 12h in empty drying box, after punching to obtain the final product;The potassium ion button cell is metallic potassium to electrode, and electrolyte is
The ethyl carbonate ester solution of 1.0mol/L KPF6, diaphragm is celgard2400 films, and assembling process is completed in argon gas atmosphere.
Second group:Using individual carbon sponge as negative material, potassium ion button is made using 8 identical method of embodiment
Battery.
Third group:Potassium ion button cell made from embodiment 8.
Above-mentioned three groups of batteries are subjected to specific discharge capacity cycle performance test, as shown in fig. 6, third group is in 200 circle cycles
Performance in charge and discharge process is substantially better than the performance of first group and second group;When charge and discharge cycles 200 are enclosed, third group, second
Group, first group of specific discharge capacity are respectively 220mAh/g, 139mAh/g, 95mAh/g.
Although above having used general explanation, specific implementation mode and experiment, the present invention is made to retouch in detail
It states, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art
's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed
Range.
Claims (10)
1. a kind of MoS2Nanometer sheet/carbon sponge composite material, which is characterized in that using carbon sponge as porous matrix, MoS2Nanometer sheet
At least partly it is coated on the skeleton structure surface of the carbon sponge.
2. MoS according to claim 12Nanometer sheet/carbon sponge composite material, which is characterized in that the carbon sponge is three-dimensional
Bridge crosslinking structure;
Preferably, the carbon sponge is the three-dimensional bridge crosslinking structure of N doping.
3. MoS according to claim 1 or 22Nanometer sheet/carbon sponge composite material, which is characterized in that the MoS2Nanometer
Piece is uniformly coated in the form of cluster.
4. a kind of MoS2The preparation method of nanometer sheet/carbon sponge composite material, which is characterized in that mixed containing molybdenum source and sulphur source
In Heshui solution, be added carbon sponge, at a temperature of being placed in 160~200 DEG C, reaction 6~24 hours to get;
Preferably, the temperature of the reaction is 170~230 DEG C, the time is 6~30 hours;
It is highly preferred that the temperature of the reaction is 190~210 DEG C, the time is 23~25 hours.
5. preparation method according to claim 4, which is characterized in that the molybdenum source is selected from sodium molybdate, potassium molybdate, ammonium molybdate
In one kind;
And/or the one kind of the sulphur source in thiocarbamide, thioacetamide, vulcanized sodium;
Preferably, the molar ratio of the molybdenum source and sulphur source is 1:(1-3).
6. preparation method according to claim 4 or 5, which is characterized in that further include activator in the mixed aqueous solution,
The activator is polyethylene glycol;
Preferably, the dosage of the activator accounts for the 20%~35% of molybdenum source and sulphur source gross mass.
7. preparation method according to claim 4, which is characterized in that include the following steps:
1) it is 1 by molar ratio:Sodium molybdate, the thiocarbamide of (1~3), and account for sodium molybdate, thiocarbamide gross mass 20%~35% poly- second
Glycol is dissolved in deionized water, is stirred to the mixed aqueous solution of water white transparency;
2) carbon sponge is placed in the mixed aqueous solution, at a temperature of 90~210 DEG C, reaction 23~25 hours to get.
8. MoS made from a kind of any one of claim 4~7 preparation method2Nanometer sheet/carbon sponge composite material.
9. claims 1 to 3,8 any one of them MoS2Nanometer sheet/application of the carbon sponge composite material in kalium ion battery.
10. a kind of potassium ion button cell, which is characterized in that with claims 1 to 3,4 any one of them MoS2Nanometer sheet/carbon
Sponge composite material is negative material.
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CN110380019A (en) * | 2019-06-18 | 2019-10-25 | 华南农业大学 | A kind of metal chalcogenide compound for kalium ion battery/three-dimensional network level hole carbon composite and its preparation method and application |
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CN111276694A (en) * | 2020-01-30 | 2020-06-12 | 吉林师范大学 | Preparation method of polyimide derived carbon/molybdenum disulfide negative electrode material and application of polyimide derived carbon/molybdenum disulfide negative electrode material in potassium ion battery |
CN113697832A (en) * | 2021-09-16 | 2021-11-26 | 安徽建筑大学 | Preparation method of basic magnesium carbonate nanosheet loaded activated carbon sponge |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110380019A (en) * | 2019-06-18 | 2019-10-25 | 华南农业大学 | A kind of metal chalcogenide compound for kalium ion battery/three-dimensional network level hole carbon composite and its preparation method and application |
CN110459752A (en) * | 2019-08-29 | 2019-11-15 | 浙江大学山东工业技术研究院 | A kind of anode material of lithium-ion battery and its preparation method and application |
CN111276694A (en) * | 2020-01-30 | 2020-06-12 | 吉林师范大学 | Preparation method of polyimide derived carbon/molybdenum disulfide negative electrode material and application of polyimide derived carbon/molybdenum disulfide negative electrode material in potassium ion battery |
CN113697832A (en) * | 2021-09-16 | 2021-11-26 | 安徽建筑大学 | Preparation method of basic magnesium carbonate nanosheet loaded activated carbon sponge |
CN113697832B (en) * | 2021-09-16 | 2023-07-14 | 安徽建筑大学 | Preparation method of basic magnesium carbonate nanosheet-loaded activated carbon sponge |
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