CN117963881A - Preparation and application of PPy/ZIF-67 derived carbon interlayer material - Google Patents
Preparation and application of PPy/ZIF-67 derived carbon interlayer material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 26
- 239000011229 interlayer Substances 0.000 title claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000002131 composite material Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 claims abstract 4
- 239000008367 deionised water Substances 0.000 claims description 37
- 229910021641 deionized water Inorganic materials 0.000 claims description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- 239000011259 mixed solution Substances 0.000 claims description 26
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000004108 freeze drying Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims description 7
- 229940012189 methyl orange Drugs 0.000 claims description 7
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 7
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 2
- JDZCKJOXGCMJGS-UHFFFAOYSA-N [Li].[S] Chemical compound [Li].[S] JDZCKJOXGCMJGS-UHFFFAOYSA-N 0.000 abstract description 21
- 239000003575 carbonaceous material Substances 0.000 abstract description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 6
- 101100289192 Pseudomonas fragi lips gene Proteins 0.000 abstract description 5
- 210000000088 lip Anatomy 0.000 abstract description 5
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 230000005764 inhibitory process Effects 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 238000000137 annealing Methods 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 229920000128 polypyrrole Polymers 0.000 description 40
- 238000011056 performance test Methods 0.000 description 12
- 238000012360 testing method Methods 0.000 description 6
- 230000000630 rising effect Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 210000001787 dendrite Anatomy 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920000945 Amylopectin Polymers 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 238000004873 anchoring Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 229920001021 polysulfide Polymers 0.000 description 1
- 239000005077 polysulfide Substances 0.000 description 1
- 150000008117 polysulfides Polymers 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
Abstract
The invention relates to preparation and application of a PPy/ZIF-67 derived carbon material, and aims to provide a preparation method applied to a lithium-sulfur battery interlayer material, which is used for solving the technical problems of poor electrochemical performance, high manufacturing cost and the like of the existing interlayer material. The invention uses PPy as secondary carbon source and nitrogen source, which improves the overall conductivity of the material and generates more defects for adsorption LiPSs. The preparation method comprises the following steps: firstly, synthesizing PPy, and transferring the PPy to a synthesis process of ZIF-67 to obtain the PPy/ZIF-67 composite material. And then annealing the obtained product at high temperature under Ar protection to obtain a final sample. The preparation method has the advantages of low manufacturing cost, stable structure of the prepared PPy/ZIF-67 derived carbon material, excellent shuttle effect inhibition performance and the like, and is very suitable for being applied to the field of lithium-sulfur batteries as an interlayer material.
Description
Technical Field
The invention belongs to the technical field of new energy electronic materials, and relates to preparation and application of a PPy/ZIF-67 derived carbon interlayer material.
Background
With exhaustion of fossil fuels and increasing environmental problems, development of high-performance energy storage devices has led to extensive research by researchers. Lithium sulfur batteries are considered the most promising second generation energy storage devices in the 21 st century because of their higher theoretical specific capacity (1675 mAh g -1) and theoretical energy density (2600 Wh kg -1). Although the lithium-sulfur battery has the advantages of no toxicity, low cost, environmental friendliness and the like, the problems (W.Zhou,H.Chen,Y.Yu,D.Wang,Z.Cui,F.J.DiSalvo,H.D.Abruna,Amylopectin Wrapped Graphene Oxide/Sulfur for Improved Cyclability of Lithium-Sulfur Battery,ACS Nano 2013,7,8801-8808.). such as rapid capacity attenuation and irreversible structural change in the working process of the battery are caused by the serious shuttle phenomenon and volume expansion in the charging and discharging process and extremely low conductivity of active sulfur, and in addition, in the negative electrode of the battery, the positive electrode and the negative electrode are in direct contact due to the fact that lithium dendrites are generated to puncture a diaphragm, so that the risk of short circuit and explosion of the lithium-sulfur battery is caused. Researches show that the nano material with the porous structure is used as the lithium sulfur battery interlayer material, is favorable for inhibiting the shuttle effect of the nano material, guides lithium ions to be uniformly deposited on the surface of a negative electrode, and has the effect (Y.Xu,L.Gao,L.Shen,Q.Liu,Y.Zhu,Q.Liu,L.Li,X.Kong,Y.Lu,H.B.Wu,Ion-Transport-Rectifying Layer Enables Li-Metal Batteries with High Energy Density,Matter 2020,3,1685-1700.). reported to inhibit the growth of lithium dendrites, so that the lithium sulfur battery interlayer material generally has the problems (X.Huang,B.Sun,K.Li,S.Chen,G.Wang,Mesoporous Graphene Paper Immobilised Sulfur as a Flexible Electrode for Lithium-Sulfur Batteries,Journal of Materials Chemistry A2013,1,13484-13489.). that the shuttle effect inhibition mode is single, the catalysis effect on the conversion of lithium polysulfide (LiPSs) is weak, and the like, therefore, the lithium sulfur battery interlayer material with the chemical selectivity, the structure stability and the rapid anchoring and the catalysis of LiPSs conversion needs to be developed.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a PPy/ZIF-67 derived carbon interlayer material for improving the shuttle effect and specific capacity of a lithium-sulfur battery. Polypyrrole (PPy) is used as a secondary carbon source and a nitrogen source, so that the electrical property of the ZIF-67 derived carbon material is improved.
According to the invention, the preparation method of the PPy/ZIF-67 derived carbon interlayer material comprises the following steps:
(1) 0.098g of methyl orange is weighed and dissolved in 150mL of deionized water, and stirred for 30min;
(2) Adding 0.2g of polyvinylpyrrolidone into the mixed solution in the step (1), and stirring for 10min;
(3) Weighing 1mL of pyrrole, adding the pyrrole into the mixed solution in the step (2), and uniformly stirring;
(4) Transferring the solution obtained in the step (3) to a cold bath, and stirring for 30min at 0 ℃;
(5) 1.8g FeCl 3·6H2 O is weighed and dissolved in 50mL deionized water, and slowly added into the mixed solution in the step (4) in a dropwise manner for reaction for 24 hours;
(6) Centrifuging the product obtained in the step (5), washing with deionized water, and freeze-drying to obtain PPy;
(7) Weighing 0.1-0.3 g of the product obtained in the step (6), dispersing 0.6g of Co (NO 3)2·6H2 O and 1.2g of 2-methylimidazole in 60mL of deionized water, and stirring for 2h;
(8) Centrifuging the product obtained in the step (7), washing with deionized water, and drying to obtain a PPy/ZIF-67 composite material;
(9) And heating the PPy/ZIF-67 composite material to 700-1000 ℃ under the protection of Ar, and preserving heat for 0.5-3 h, wherein the heating rate is 5 ℃/min, so as to obtain a final sample.
According to the invention, it is preferred that the mass of PPy added in step (7) is 0.3g.
According to the invention, the drying in step (8) is preferably freeze-drying.
According to the invention, the reaction temperature in step (9) is preferably 800 ℃.
According to the invention, the incubation time in step (9) is preferably 2h.
The application of the PPy/ZIF-67 derived carbon material is used as an interlayer material of a lithium-sulfur battery.
Compared with the prior art, the invention has the following advantages:
(1) The invention adopts PPy as a secondary carbon source and a nitrogen source, and defects generated by nitrogen doping can be absorbed LiPSs more efficiently.
(2) The invention has simple process and is suitable for large-scale industrial production.
(3) The PPy/ZIF-67 derived carbon material prepared by the invention has stable structure, and can inhibit the shuttle of LiPSs through multiple angles such as physical limitation, chemical adsorption, catalytic conversion and the like, and the initial specific capacity of the lithium sulfur battery assembled by using the PPy/ZIF-67 derived carbon material as an interlayer material at 1C is up to 1072.82mAh g -1, which is superior to most of reported carbon-based interlayer materials.
Drawings
FIG. 1 is a scanning electron microscope image of a PPy/ZIF-67 derived carbon material prepared in example 1 of the present invention.
FIG. 2 is a transmission electron microscope image of the PPy/ZIF-67 derived carbon material prepared in example 1 of the present invention.
FIG. 3 is an XRD spectrum of the PPy/ZIF-67-derived carbon material prepared in example 1 of the present invention and the ZIF-67-derived carbon material prepared in comparative example.
FIG. 4 is an XPS spectrum of a PPy/ZIF-67 derived carbon material prepared in example 1 of the present invention.
FIG. 5 is a graph showing the rate performance of a lithium sulfur battery assembled from the PPy/ZIF-67-derived carbon interlayer material prepared in example 1 of the present invention and the ZIF-67-derived carbon interlayer material prepared in comparative example.
FIG. 6 is a graph showing the long cycle performance of a lithium sulfur battery assembled from the PPy/ZIF-67-derived carbon interlayer material prepared in example 1 of the present invention and the ZIF-67-derived carbon interlayer material prepared in comparative example.
Detailed Description
The invention is further described below with reference to specific examples and figures, but is not limited thereto.
Meanwhile, the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials, unless otherwise specified, are commercially available.
Example 1:
First, 0.098g of methyl orange was weighed into 150mL of deionized water, stirred for 30min, 0.2g of polyvinylpyrrolidone was added to the mixed solution, and stirred for 10min. 1mL of pyrrole is measured and added into the mixed solution, the mixed solution is stirred uniformly, transferred into a cold bath, stirred at 0 ℃ for 30min, 1.8g of FeCl 3·6H2 O is weighed and dissolved in 50mL of deionized water, and slowly added into the mixed solution in a dropwise manner, and the reaction is carried out for 24h. Centrifuging the obtained product, washing with deionized water, and freeze-drying to obtain PPy;
Then 0.3g of the obtained PPy and 0.6g of Co (NO 3)2·6H2 O and 1.2g of 2-methylimidazole) are weighed and dissolved in 60mL of deionized water, stirred for 2 hours, the obtained product is centrifuged, washed with deionized water, and freeze-dried to obtain the PPy/ZIF-67 composite material.
Finally, the PPy/ZIF-67 composite material is heated to 800 ℃ under the protection of Ar, the temperature is kept for 2 hours, and the temperature rising rate is 5 ℃/min, so that a final sample is obtained.
And (3) completing lithium-sulfur battery assembly in a glove box, performing room-temperature multiplying power performance test by a blue-electricity battery test system under different multiplying powers, and performing room-temperature cycle performance test under the condition of 1C.
Example 2:
First, 0.098g of methyl orange was weighed into 150mL of deionized water, stirred for 30min, 0.2g of polyvinylpyrrolidone was added to the mixed solution, and stirred for 10min. 1mL of pyrrole is measured and added into the mixed solution, the mixed solution is stirred uniformly, transferred into a cold bath, stirred at 0 ℃ for 30min, 1.8g of FeCl 3·6H2 O is weighed and dissolved in 50mL of deionized water, and slowly added into the mixed solution in a dropwise manner, and the reaction is carried out for 24h. Centrifuging the obtained product, washing with deionized water, and freeze-drying to obtain PPy;
Then 0.1g of the obtained PPy and 0.6g of Co (NO 3)2·6H2 O and 1.2g of 2-methylimidazole) are weighed and dissolved in 60mL of deionized water, stirred for 2 hours, the obtained product is centrifuged, washed with deionized water, and freeze-dried to obtain the PPy/ZIF-67 composite material.
Finally, the PPy/ZIF-67 composite material is heated to 800 ℃ under the protection of Ar, the temperature is kept for 2 hours, and the temperature rising rate is 5 ℃/min, so that a final sample is obtained.
And (3) completing lithium-sulfur battery assembly in a glove box, performing room-temperature multiplying power performance test by a blue-electricity battery test system under different multiplying powers, and performing room-temperature cycle performance test under the condition of 1C.
Example 3:
First, 0.098g of methyl orange was weighed into 150mL of deionized water, stirred for 30min, 0.2g of polyvinylpyrrolidone was added to the mixed solution, and stirred for 10min. 1mL of pyrrole is measured and added into the mixed solution, the mixed solution is stirred uniformly, transferred into a cold bath, stirred at 0 ℃ for 30min, 1.8g of FeCl 3·6H2 O is weighed and dissolved in 50mL of deionized water, and slowly added into the mixed solution in a dropwise manner, and the reaction is carried out for 24h. Centrifuging the obtained product, washing with deionized water, and freeze-drying to obtain PPy;
Then 0.3g of the obtained PPy and 0.6g of Co (NO 3)2·6H2 O and 1.2g of 2-methylimidazole) are weighed and dissolved in 60mL of deionized water, stirred for 2 hours, the obtained product is centrifuged, washed with deionized water, and freeze-dried to obtain the PPy/ZIF-67 composite material.
Finally, the PPy/ZIF-67 composite material is heated to 700 ℃ under the protection of Ar, the temperature is kept for 1h, and the temperature rising rate is 5 ℃/min, so that a final sample is obtained.
And (3) completing lithium-sulfur battery assembly in a glove box, performing room-temperature multiplying power performance test by a blue-electricity battery test system under different multiplying powers, and performing room-temperature cycle performance test under the condition of 1C.
Example 4:
First, 0.098g of methyl orange was weighed into 150mL of deionized water, stirred for 30min, 0.2g of polyvinylpyrrolidone was added to the mixed solution, and stirred for 10min. 1mL of pyrrole is measured and added into the mixed solution, the mixed solution is stirred uniformly, transferred into a cold bath, stirred at 0 ℃ for 30min, 1.8g of FeCl 3·6H2 O is weighed and dissolved in 50mL of deionized water, and slowly added into the mixed solution in a dropwise manner, and the reaction is carried out for 24h. Centrifuging the obtained product, washing with deionized water, and freeze-drying to obtain PPy;
Then 0.3g of the obtained PPy and 0.6g of Co (NO 3)2·6H2 O and 1.2g of 2-methylimidazole) are weighed and dissolved in 60mL of deionized water, stirred for 2 hours, the obtained product is centrifuged, washed with deionized water, and freeze-dried to obtain the PPy/ZIF-67 composite material.
Finally, the PPy/ZIF-67 composite material is heated to 900 ℃ under the protection of Ar, the temperature is kept for 3 hours, and the temperature rising rate is 5 ℃/min, so that a final sample is obtained.
And (3) completing lithium-sulfur battery assembly in a glove box, performing room-temperature multiplying power performance test by a blue-electricity battery test system under different multiplying powers, and performing room-temperature cycle performance test under the condition of 1C.
Example 5:
First, 0.098g of methyl orange was weighed into 150mL of deionized water, stirred for 30min, 0.2g of polyvinylpyrrolidone was added to the mixed solution, and stirred for 10min. 1mL of pyrrole is measured and added into the mixed solution, the mixed solution is stirred uniformly, transferred into a cold bath, stirred at 0 ℃ for 30min, 1.8g of FeCl 3·6H2 O is weighed and dissolved in 50mL of deionized water, and slowly added into the mixed solution in a dropwise manner, and the reaction is carried out for 24h. Centrifuging the obtained product, washing with deionized water, and freeze-drying to obtain PPy;
Then 0.3g of the obtained PPy and 0.6g of Co (NO 3)2·6H2 O and 1.2g of 2-methylimidazole) are weighed and dissolved in 60mL of deionized water, stirred for 2 hours, the obtained product is centrifuged, washed with deionized water and dried to obtain the PPy/ZIF-67 composite material.
Finally, the PPy/ZIF-67 composite material is heated to 800 ℃ under the protection of Ar, the temperature is kept for 2 hours, and the temperature rising rate is 5 ℃/min, so that a final sample is obtained.
And (3) completing lithium-sulfur battery assembly in a glove box, performing room-temperature multiplying power performance test by a blue-electricity battery test system under different multiplying powers, and performing room-temperature cycle performance test under the condition of 1C.
Comparative example:
0.6g Co (NO 3)2·6H2 O and 1.2g 2-methylimidazole were dissolved in 60mL deionized water and stirred for 2 h), the resulting product was centrifuged, washed with deionized water and dried at 80℃to give ZIF-67.
And heating ZIF-67 to 900 ℃ under the protection of Ar, and preserving heat for 1h, wherein the heating rate is 5 ℃/min, so as to obtain a final sample.
And (3) completing lithium-sulfur battery assembly in a glove box, performing room-temperature multiplying power performance test by a blue-electricity battery test system under different multiplying powers, and performing room-temperature cycle performance test under the condition of 1C.
Claims (5)
1. The preparation method of the PPy/ZIF-67 derived carbon interlayer material is characterized by comprising the following steps:
(1) 0.098g of methyl orange is weighed and dissolved in 150mL of deionized water, and stirred for 30min;
(2) Adding 0.2g of polyvinylpyrrolidone into the mixed solution in the step (1), and stirring for 10min;
(3) Weighing 1mL of pyrrole, adding the pyrrole into the mixed solution in the step (2), and uniformly stirring;
(4) Transferring the solution obtained in the step (3) to a cold bath, and stirring for 30min at 0 ℃;
(5) 1.8g FeCl 3·6H2 O is weighed and dissolved in 50mL deionized water, and slowly added into the mixed solution in the step (4) in a dropwise manner for reaction for 24 hours;
(6) Centrifuging the product obtained in the step (5), washing with deionized water, and freeze-drying to obtain PPy;
(7) Weighing 0.1-0.3 g of the product obtained in the step (6), dispersing 0.6g of Co (NO 3)2·6H2 O and 1.2g of 2-methylimidazole in 60mL of deionized water, and stirring for 2h;
(8) Centrifuging the product obtained in the step (7), washing with deionized water, and drying to obtain a PPy/ZIF-67 composite material;
(9) And heating the PPy/ZIF-67 composite material to 700-1000 ℃ under the protection of Ar, and preserving heat for 0.5-3 h, wherein the heating rate is 5 ℃/min, so as to obtain a final sample.
2. The method for producing a PPy/ZIF-67-derived carbon interlayer material according to claim 1, wherein the mass of PPy added in step (7) is 0.3g.
3. The method for preparing a PPy/ZIF-67-derived carbon interlayer material according to claim 1, wherein the drying in step (8) is freeze drying.
4. The method for producing PPy/ZIF-67-derived carbon interlayer material according to claim 1, wherein the reaction temperature in step (9) is 800 ℃.
5. The method for preparing a PPy/ZIF-67-derived carbon interlayer material according to claim 1, wherein the holding time in step (9) is 2h.
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