CN115432692B - One-dimensional soft interface nanowire and super-assembly preparation method thereof - Google Patents
One-dimensional soft interface nanowire and super-assembly preparation method thereof Download PDFInfo
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- 239000002070 nanowire Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- CWLKGDAVCFYWJK-UHFFFAOYSA-N 3-aminophenol Chemical compound NC1=CC=CC(O)=C1 CWLKGDAVCFYWJK-UHFFFAOYSA-N 0.000 claims abstract description 52
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 48
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 37
- 229940018563 3-aminophenol Drugs 0.000 claims abstract description 25
- 239000004312 hexamethylene tetramine Substances 0.000 claims abstract description 24
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims abstract description 24
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 238000007865 diluting Methods 0.000 claims abstract description 5
- 238000010790 dilution Methods 0.000 claims description 17
- 239000012895 dilution Substances 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 15
- 230000035484 reaction time Effects 0.000 claims description 14
- 238000000034 method Methods 0.000 abstract description 8
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- 230000001105 regulatory effect Effects 0.000 abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 229960004011 methenamine Drugs 0.000 description 19
- 239000000463 material Substances 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000003917 TEM image Methods 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- 239000000693 micelle Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 102100028292 Aladin Human genes 0.000 description 3
- 101710065039 Aladin Proteins 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 238000013507 mapping Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- -1 phenolic aldehyde Chemical class 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002134 carbon nanofiber Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000001523 electrospinning Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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Abstract
The invention relates to a super-assembly preparation method of a one-dimensional soft interface nanowire, which comprises the following steps: adding m-aminophenol, cetyl trimethyl ammonium bromide CTAB and hexamethylenetetramine into an aqueous solution for hydrothermal reaction, then diluting, and continuing the reaction to obtain the one-dimensional soft interface nanowire. According to the method, m-aminophenol is used as a carbon source, hexamethylenetetramine is used as a raw material precursor, cetyltrimethylammonium bromide CTAB is used as a template agent, the ultra-fine soft nanowire is obtained through a hydrothermal method, and the size of the nanowire can be regulated and controlled between 10 nm and 160 nm. The method is simple and easy to operate, environment-friendly, strong in sustainability and capable of realizing large-scale production. The invention provides a novel idea for designing and preparing the superfine soft nanowire.
Description
Technical Field
The invention relates to the field of preparation of one-dimensional nanowires, in particular to a one-dimensional soft interface nanowire and a super-assembly preparation method thereof.
Background
In recent years, one-dimensional nanowire/nanofiber/nanotube structures having ultra-fine diameters and high aspect ratios have been widely studied for their unique physical and chemical properties, such as large surface area, superior mechanical properties and tunable surface properties.
In addition, the one-dimensional nanomaterial is an ideal material for constructing an assembled device with three-dimensional interconnected porosity, adjustable pore size, large pore volume and adjustable morphology. Therefore, the one-dimensional nano material and the derivative device thereof show a series of potential application prospects in the fields of drug delivery, energy storage and conversion, catalysis, sensors, separation, spinning, electronic devices, tissue engineering and the like. Carbon nanofibers, carbon nanotubes and organic nanowires are the most explored members of the one-dimensional nanomaterial family.
To date, various methods have been developed to prepare one-dimensional nanomaterials, such as electrospinning, chemical vapor deposition, physical vapor deposition, electrochemical deposition, laser ablation, hard template methods, hydrothermal synthesis, and the like. However, it is often desirable that the reaction conditions be harsh and/or that the reactions be multi-step, that the diameters and structures be difficult to adjust, and that it be difficult to incorporate pre-designed functions.
In addition, the method has few reports on the soft one-dimensional nanowire, so that the development of a simple and efficient synthesis strategy for preparing the soft one-dimensional nanowire has very important significance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the one-dimensional soft interface nanowire which is simple and easy to operate, environment-friendly, strong in sustainability and capable of realizing large-scale production and the super-assembly preparation method thereof.
The aim of the invention can be achieved by the following technical scheme:
a super-assembly preparation method of a one-dimensional soft interface nanowire comprises the following steps: adding m-aminophenol, cetyl trimethyl ammonium bromide CTAB and hexamethylenetetramine into an aqueous solution for hydrothermal reaction, then diluting, and continuing the reaction to obtain the one-dimensional soft interface nanowire.
In the technical scheme, meta-aminophenol is used as a carbon source, hexamethylenetetramine is used as a raw material precursor, cetyltrimethylammonium bromide CTAB is used as a template agent, and the superfine soft nanowire is prepared.
Cetyl trimethylammonium bromide CTAB and m-aminophenol will self-assemble into columnar micelles in solution. As the reaction proceeds, the temperature begins to rise and hexamethylenetetramine will gradually decompose into formaldehyde and ammonia. The meta-aminophenol and limited formaldehyde are subjected to phenolic aldehyde condensation reaction to generate oligomer stable micelle, self-assembly of the micelle and slow phenolic aldehyde condensation reaction are synchronously carried out, and a pre-stable micelle solution is obtained after a certain time of reaction. And then diluting the solution, and continuing the reaction to obtain the superfine nanowire. The size of the nanowire and the like can be regulated and controlled through the content of m-aminophenol and hexamethylenetetramine, and can be regulated between 10 nanometers and 160 nanometers. The method is simple and easy to operate, environment-friendly, strong in sustainability, capable of realizing large-scale production and high in application value.
Further, the mass concentration of the m-aminophenol is 0.1-100mg/mL, preferably 2-20mg/mL, and more preferably 4-10mg/mL.
Further, the mass concentration of the hexamethylenetetramine is 0.2-200mg/mL, preferably 4-50mg/mL, and more preferably 10-30mg/mL.
Further, the mass concentration of the cetyl trimethyl ammonium bromide CTAB is 0.1-100mg/mL, preferably 2-20mg/mL, and more preferably 4-10mg/mL.
Further, the mass ratio of the m-aminophenol to the cetyl trimethyl ammonium bromide CTAB to the hexamethylenetetramine is (0.2-100): 0.2-200): 0.1-100.
Further, the mass ratio of the m-aminophenol to the cetyl trimethyl ammonium bromide CTAB to the hexamethylenetetramine is (2-20): 4-50): 2-20.
Preferably, the feeding ratio of the m-aminophenol to the aqueous solution is 1.0 g/100 g.
Further, the temperature of the hydrothermal reaction is 60-200 ℃. Before dilution, the hydrothermal reaction time is 0.5-3h; after dilution, the reaction time is 1-72h.
Preferably, the temperature of the hydrothermal reaction is 80-120 ℃, the reaction time before dilution is 1-3h, and the reaction time before dilution is 12-48h.
Further preferably, the temperature is 90-110 ℃, the reaction time before dilution is 1.5-2.5h, and the reaction time before dilution is 18-36h.
Further, the pre-stabilized solution volume is diluted 10-1000 times at the dilution. Preferably 50-500 times.
A one-dimensional soft interface nanowire prepared by the super-assembly preparation method. The obtained material has the appearance of one-dimensional nanowires.
Compared with the prior art, the invention has the following advantages:
(1) The invention provides a novel ultra-fine soft one-dimensional nanowire material;
(2) The method is simple and easy to operate, environment-friendly, strong in sustainability and capable of realizing large-scale production;
(3) The novel ultra-fine soft one-dimensional nanowire obtained by the preparation method is assembled based on micelles;
(4) The size of the nanowire material obtained by the invention can be effectively regulated and controlled through the contents of m-aminophenol and hexamethylenetetramine.
Drawings
FIG. 1 is a Transmission Electron Microscope (TEM) image of the soft nanowires prepared in example 1;
FIG. 2 is a high magnification TEM image of the soft nanowires prepared in example 1;
FIG. 3 is a Scanning Electron Microscope (SEM) image of the soft nanowires prepared in example 1;
FIG. 4 is a high magnification SEM image of the soft nanowire prepared in example 1;
FIG. 5 is a mapping graph of the element distribution of the soft nanowire prepared in example 1;
FIG. 6 is a TEM image of the soft nanowires prepared in example 2;
FIG. 7 is a TEM image of the soft nanowires prepared in example 3;
FIG. 8 is a TEM image of the soft nanowires prepared in example 4;
fig. 9 is a Scanning Electron Microscope (SEM) image of the soft nanowire prepared in example 1.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples. The present embodiment is implemented on the premise of the technical scheme of the present invention, and a detailed implementation manner and a specific operation process are provided, but the protection scope of the present invention is not limited to the following embodiments.
A super-assembly preparation method of a one-dimensional soft interface nanowire comprises the following steps: adding m-aminophenol, cetyl trimethyl ammonium bromide CTAB and hexamethylenetetramine into an aqueous solution for hydrothermal reaction, then diluting, and continuing the reaction to obtain the one-dimensional soft interface nanowire. The obtained material has the appearance of one-dimensional nanowires.
The cetyl trimethyl ammonium bromide CTAB used in the examples is purchased from Aladin company under the trade designation H108983-100g, hereinafter referred to as CTAB; m-aminophenol is purchased from Aladin under the trade designation A301746-500g. Hexamethylene tetramine is purchased from Aladin under the trade designation H116380-100g.
The mass concentration of m-aminophenol is 0.1-100mg/mL, preferably 2-20mg/mL, more preferably 4-10mg/mL. The mass concentration of hexamethylenetetramine is 0.2-200mg/mL, preferably 4-50mg/mL, and more preferably 10-30mg/mL. The mass concentration of cetyl trimethyl ammonium bromide CTAB is 0.1-100mg/mL, preferably 2-20mg/mL, more preferably 4-10mg/mL.
The mass ratio of the m-aminophenol to the cetyl trimethyl ammonium bromide CTAB to the hexamethylenetetramine is (0.2-100): 0.2-200): 0.1-100. The mass ratio of the m-aminophenol to the cetyl trimethyl ammonium bromide CTAB to the hexamethylenetetramine is (2-20): 4-50): 2-20. Preferably, the feeding ratio of the m-aminophenol to the aqueous solution is 1.0 g/100 g.
The temperature of the hydrothermal reaction is 60-200 ℃. Before dilution, the hydrothermal reaction time is 0.5-3h; after dilution, the reaction time is 1-72h. Preferably, the temperature of the hydrothermal reaction is 80-120 ℃, the reaction time before dilution is 1-3h, and the reaction time before dilution is 12-48h. Further preferably, the temperature is 90-110 ℃, the reaction time before dilution is 1.5-2.5h, and the reaction time before dilution is 18-36h. The pre-stabilized solution volume is diluted 10-1000 times during dilution. Preferably 50-500 times.
Example 1
Super-assembly preparation method of one-dimensional soft interface nanowire
100mL of deionized water was removed and added to a 250mL Erlenmeyer flask, then 1.0g of m-aminophenol (10 mg/mL) and 1.0g of CTAB (10 mg/mL) and 1.5g of hexamethylenetetramine (15 mg/mL) were added to the solution and stirred for 2 hours. The Erlenmeyer flask was then placed in an oven at 100deg.C and allowed to react for 2 hours. 1mL of the solution was taken out and added to 199mL of deionized water, stirred for 2 hours, and then reacted in an oven at 100℃for 36 hours. Cooling to room temperature, suction filtering, washing with water and ethanol respectively, and drying to obtain the one-dimensional nanowire material.
The Transmission Electron Microscope (TEM) of the nanowire prepared in this embodiment is shown in fig. 1-2, and it can be seen from fig. 1 that the nanowire prepared has a linear structure and is uniformly dispersed; FIG. 2 is a further enlarged TEM image, seen with a smooth surface; according to statistics, the average size is 30 nm. The Scanning Electron Microscope (SEM) of the nanowire prepared in this example is shown in fig. 3-4, and further shows dispersibility and 1D structural characteristics. The mapping graph of the nanowire prepared in the embodiment is shown in fig. 5, which shows that C, O, N elements are uniformly distributed, and the obtained nitrogen-doped carbon material is indicated.
Example 2
Super-assembly preparation method of one-dimensional soft interface nanowire
100mL of deionized water was removed and added to a 250mL Erlenmeyer flask, then 0.3g of m-aminophenol (3 mg/mL) and 1.0g of CTAB (10 mg/mL) and 0.45g of hexamethylenetetramine (4.5 mg/mL) were added to the solution and stirred for 2 hours. The Erlenmeyer flask was then placed in an oven at 100deg.C and allowed to react for 2 hours. 1mL of the solution was taken out and added to 199mL of deionized water, stirred for 2 hours, and then reacted in an oven at 100℃for 36 hours. Cooling to room temperature, suction filtering, washing with water and ethanol respectively, and drying to obtain the one-dimensional nanowire material.
The TEM image of the nanowire material prepared in this example is shown in fig. 6, and it can be seen from fig. 6 that the diameter of the nanowire prepared is about 10 nm.
Example 3
Super-assembly preparation method of one-dimensional soft interface nanowire
100mL of deionized water was removed and added to a 250mL Erlenmeyer flask, then 1.0g of m-aminophenol (10 mg/mL) and 1.0g of CTAB (10 mg/mL) and 1.5g of hexamethylenetetramine (15 mg/mL) were added to the solution and stirred for 2 hours. The Erlenmeyer flask was then placed in an oven at 100deg.C and allowed to react for 2 hours. 1mL of the solution was taken out and added to 199mL of deionized water, 0.2g of m-aminophenol and 0.3g of hexamethylenetetramine were simultaneously added thereto, and the mixture was stirred for 2 hours, and then the reaction was continued in an oven at 100℃for 36 hours. Cooling to room temperature, suction filtering, washing with water and ethanol respectively, and drying to obtain the one-dimensional nanowire material.
The TEM image of the nanowire material prepared in this example is shown in fig. 7, and it can be seen from fig. 7 that the diameter of the nanowire prepared is about 80 nm.
Example 4
Super-assembly preparation method of one-dimensional soft interface nanowire
100mL of deionized water was removed and added to a 250mL Erlenmeyer flask, then 1.0g of m-aminophenol (10 mg/mL) and 1.0g of CTAB (10 mg/mL) and 1.5g of hexamethylenetetramine (15 mg/mL) were added to the solution and stirred for 2 hours. The Erlenmeyer flask was then placed in an oven at 100deg.C and allowed to react for 2 hours. 1mL of the solution was taken out and added to 199mL of deionized water, 0.6g of m-aminophenol and 0.9g of hexamethylenetetramine were simultaneously added, and the mixture was stirred for 2 hours, and then the reaction was continued in an oven at 100℃for 36 hours. Cooling to room temperature, suction filtering, washing with water and ethanol respectively, and drying to obtain the one-dimensional nanowire material.
The TEM image of the nanowire material prepared in this example is shown in fig. 8, and it can be seen from fig. 8 that the diameter of the nanowire prepared is about 160 nm.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the invention in any way, and any person skilled in the art may make modifications or alterations to the disclosed technical content to the equivalent embodiments. However, any simple modification, equivalent variation and variation of the above embodiments according to the technical substance of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (2)
1. A super-assembly preparation method of a one-dimensional soft interface nanowire is characterized by comprising the following steps: adding m-aminophenol, cetyl trimethyl ammonium bromide CTAB and hexamethylenetetramine into an aqueous solution for hydrothermal reaction, then diluting, and continuing the reaction to obtain a one-dimensional soft interface nanowire, wherein the mass concentration of the m-aminophenol is 0.1-100 mg/mL; the mass concentration of the hexamethylenetetramine is 0.2-200 mg/mL; the mass concentration of the cetyl trimethyl ammonium bromide CTAB is 0.1-100 mg/mL; the mass ratio of the m-aminophenol to the cetyl trimethyl ammonium bromide CTAB to the hexamethylenetetramine is 1:1:1.5;
the temperature of the hydrothermal reaction is 60-200 ℃; the hydrothermal reaction time is 0.5-3h before dilution; after dilution, the reaction time is 1-72 h; the pre-stabilized solution volume is diluted 10-1000 times during the dilution.
2. A one-dimensional soft interface nanowire prepared by the super-assembly preparation method of claim 1.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109087814A (en) * | 2018-08-06 | 2018-12-25 | 武汉理工大学 | Situ Nitrogen Doping porous carbon nanofiber electrode material and its magnanimity preparation method and application |
| CN110078031A (en) * | 2019-05-27 | 2019-08-02 | 中国科学技术大学 | A kind of Te nano wire three-dimensional aeroge, preparation method and its application |
| CN111892037A (en) * | 2020-07-31 | 2020-11-06 | 复旦大学 | Porous nano-wire carbon material and super-assembly preparation method thereof |
| WO2020224483A1 (en) * | 2019-05-05 | 2020-11-12 | Qingdao Institute Of Bioenergy And Bioprocess Technology Chinese Academy Of Sciences | Method for preparing catalyst support loaded with a first metal and a second metal |
| CN113582161A (en) * | 2021-08-10 | 2021-11-02 | 复旦大学 | Small-size porous nitrogen-doped carbon nanoparticles and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109087814A (en) * | 2018-08-06 | 2018-12-25 | 武汉理工大学 | Situ Nitrogen Doping porous carbon nanofiber electrode material and its magnanimity preparation method and application |
| WO2020224483A1 (en) * | 2019-05-05 | 2020-11-12 | Qingdao Institute Of Bioenergy And Bioprocess Technology Chinese Academy Of Sciences | Method for preparing catalyst support loaded with a first metal and a second metal |
| CN110078031A (en) * | 2019-05-27 | 2019-08-02 | 中国科学技术大学 | A kind of Te nano wire three-dimensional aeroge, preparation method and its application |
| CN111892037A (en) * | 2020-07-31 | 2020-11-06 | 复旦大学 | Porous nano-wire carbon material and super-assembly preparation method thereof |
| CN113582161A (en) * | 2021-08-10 | 2021-11-02 | 复旦大学 | Small-size porous nitrogen-doped carbon nanoparticles and preparation method thereof |
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