CN115044039A - Multifunctional nanowire with adjustable surface groups and components and super-assembly preparation method thereof - Google Patents
Multifunctional nanowire with adjustable surface groups and components and super-assembly preparation method thereof Download PDFInfo
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Abstract
The invention relates to a super-assembly preparation method of a multifunctional nanowire with adjustable surface groups and components, which comprises the following steps: adding m-aminophenol, hexamethylenetetramine and Cetyl Trimethyl Ammonium Bromide (CTAB) into an aqueous solution for hydrothermal reaction to obtain an oligomer-CTAB metastable micelle solution, diluting the solution, adding a functional precursor, and continuing to react to obtain the multifunctional nanowire with the adjustable surface groups and components. The method comprises the steps of taking m-aminophenol as a precursor, taking hexamethylenetetramine as a cross-linking agent and a precursor of a catalyst, taking hexadecyl trimethyl ammonium bromide (CTAB) as a template agent, taking other functional components as subsequent addition precursors, firstly obtaining a pre-stabilized micelle through a hydrothermal method, and then diluting and adding the required functional precursors to obtain the nanowire material with adjustable surface groups and components. The method is simple and easy to operate, environment-friendly, strong in sustainability and capable of realizing large-scale production.
Description
Technical Field
The invention relates to the field of preparation of multifunctional nano materials, in particular to a multifunctional nanowire with adjustable surface groups and components and a super-assembly preparation method thereof.
Background
One-dimensional nanostructures such as nanorods, metal wires, nanobelts, nanotubes and the like have extremely high length-diameter ratio and large surface area, and attract the attention of a great deal of researchers. The one-dimensional nano materials can be synthesized by adopting various technologies such as a high-temperature catalysis process, a pulse laser ablation, chemical vapor deposition, a gas-solid-liquid growth process, mixed powder evaporation, an epitaxial growth process, a hard template and the like. However, the synthesis and application of these materials are greatly limited by the harsh and complicated reaction conditions, and the components of the existing one-dimensional materials are single, so that it is difficult to synthesize the one-dimensional nano-materials with adjustable components and functions in situ. With more and more importance placed on low cost, high throughput, high yield and easy production, template synthesis becomes the first choice for synthesizing one-dimensional nanomaterials.
However, it is still a great challenge to prepare one-dimensional nano-materials by soft template method. The simultaneous control of the stability of the micelle and the polymerization rate of the components is one of the biggest difficulties, and in addition, how to precisely control the components and functional groups is a challenge. Therefore, the development of a new soft template technology to prepare the novel multifunctional one-dimensional nano material has important scientific and practical significance.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a multifunctional nanowire with adjustable surface groups and components and a super-assembly preparation method thereof, wherein the nanowire is simple and easy to operate, environment-friendly and strong in sustainability, and can realize large-scale production.
The purpose of the invention can be realized by the following technical scheme:
a super-assembly preparation method of a multifunctional nanowire with adjustable surface groups and components comprises the following steps: adding m-aminophenol, hexamethylenetetramine and Cetyl Trimethyl Ammonium Bromide (CTAB) into an aqueous solution for hydrothermal reaction to obtain an oligomer-CTAB metastable micelle solution, diluting the solution, adding a functional precursor, and continuing to react to obtain the multifunctional nanowire with the adjustable surface groups and components.
In the technical scheme, cetyl trimethyl ammonium bromide CTAB is used as a template agent, m-aminophenol is used as a precursor, and hexamethylenetetramine is used as a precursor of a cross-linking agent and a catalyst to prepare the multifunctional nanowire.
Cetyl trimethyl ammonium 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, with formaldehyde as the crosslinking agent and ammonia as the catalyst. M-aminophenol and limited formaldehyde are subjected to phenolic aldehyde condensation reaction to generate oligomers, the oligomers enter hydrophobic regions in micelles to stabilize the micelles, and a pre-stabilized micelle solution is obtained after reaction for a certain time. And then diluting the solution, adding a certain amount of target precursor, continuing to react, and reacting the target precursor and the oligomer together for polymerization to obtain the nano wire with different surface components and functional groups. The surface components and properties of the nanowires can be regulated by the type of precursor added after dilution. 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 further preferably 4-10 mg/mL.
Further, the mass concentration of the hexamethylenetetramine is 0.2-200mg/mL, preferably 4-50mg/mL, and further preferably 10-30 mg/mL.
Further, the mass concentration of the cetyltrimethylammonium bromide CTAB is 0.1-100mg/mL, preferably 2-20mg/mL, and more preferably 4-10 mg/mL.
Furthermore, the mass ratio of the m-aminophenol, the cetyl trimethyl ammonium bromide CTAB, the hexamethylenetetramine and the functional precursor is (0.2-100): 0.2-200: (0.1-100): 0.01-4).
Preferably, the preparation method of the soft nanowire comprises the following steps of mixing m-aminophenol, Cetyl Trimethyl Ammonium Bromide (CTAB) and hexamethylenetetramine in a mass ratio of (2-20) to (4-50) to (2-20).
Preferably, the charging ratio of the m-aminophenol to the aqueous solution is 1.0g to 100 g. Preferably, the mass of the target precursor added into the diluted solution is 0.1-1 g.
Further, the functional precursor comprises thiourea, hexadecyl triethoxy silicon, ruthenium trichloride or platinum tetrachloride.
Further, the temperature of the hydrothermal reaction is 60-200 ℃. Before dilution, the time of hydrothermal reaction is 0.5-3 h; after dilution, the reaction time is 1-72 h.
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 12-48 h.
Further preferably, the temperature is 90-110 ℃, the reaction time before dilution is 1.5-2.5h, and the reaction time before dilution is 18-36 h.
Further, the dilution is performed by diluting the volume of the pre-stabilized solution by 10 to 1000 times, preferably 50 to 500 times.
A multifunctional nanowire with adjustable surface groups and components prepared by the super-assembly preparation method. The obtained material has the appearance of a one-dimensional nanowire, and the surface components and properties of the material can be effectively regulated and controlled.
Compared with the prior art, the invention has the following advantages:
(1) the invention provides a novel multifunctional nanowire material. The method is simple and easy to operate, is environment-friendly, and can realize large-scale production;
(2) the novel multifunctional nanowire obtained by the preparation method is obtained by assembling an oligomer pre-stabilized micelle and a target precursor;
(3) the surface components and functions of the multifunctional nanowire material obtained by the invention can be effectively regulated and controlled by the content of the target precursor added during dilution.
Drawings
FIG. 1 is a Transmission Electron Micrograph (TEM) of the multifunctional nanowire prepared in example 1;
FIG. 2 is a high magnification TEM image of the multifunctional nanowire prepared in example 1;
FIG. 3 is a high power transmission electron microscopy (HRTEM) image and an element distribution mapping image of the multifunctional nanowire prepared in example 1;
FIG. 4 is a TEM image of the multifunctional nanowire prepared in example 2;
FIG. 5 is an HRTEM image and an element distribution mapping image of the multifunctional nanowire prepared in example 2;
FIG. 6 is a TEM image of the multifunctional nanowire prepared in example 3;
FIG. 7 is an HRTEM image and an element distribution mapping image of the multifunctional nanowire prepared in example 3;
FIG. 8 is a TEM image of the multifunctional nanowire prepared in example 4;
FIG. 9 is an HRTEM image and an element distribution mapping image of the multifunctional nanowire prepared in example 4;
fig. 10 is a TEM image of the multifunctional nanowire prepared in example 3.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following embodiments.
A super-assembly preparation method of a multifunctional nanowire with adjustable surface groups and components comprises the following steps: adding m-aminophenol, hexamethylenetetramine and Cetyl Trimethyl Ammonium Bromide (CTAB) into an aqueous solution for hydrothermal reaction to obtain an oligomer-CTAB metastable micelle solution, diluting the solution, adding a functional precursor, and continuing to react to obtain the multifunctional nanowire with the adjustable surface groups and components. The obtained material has the appearance of a one-dimensional nanowire, and the surface components and properties of the material can be effectively regulated and controlled. The functional precursor comprises thiourea, hexadecyl triethoxy silicon, ruthenium trichloride or platinum tetrachloride.
M-aminophenol was purchased from Aladdin, Inc. under the A301746-500g brand. Hexamethylene tetramine is purchased from Aladdin under the trade name H116380-100 g. Cetyl trimethyl ammonium bromide CTAB adopted in the embodiment is purchased from Aladdin company, the product number is H108983-100g, and the CTAB is referred to as CTAB in the following; thiourea was purchased from Aladdin, Inc. under a product number of T112512-100 g. Hexadecyltriethoxysilane was purchased from Aladdin under the designation H404566-25 ml. Ruthenium trichloride was purchased from Aladdin under the designation R119430-1 g. Platinum tetrachloride was purchased from Aladdin under the designation P121688-1 g.
The mass concentration of m-aminophenol is 0.1-100mg/mL, preferably 2-20mg/mL, and more preferably 4-10 mg/mL. The mass concentration of hexamethylenetetramine is 0.2-200mg/mL, preferably 4-50mg/mL, and more preferably 10-30 mg/mL. The mass concentration of cetyltrimethylammonium bromide CTAB is 0.1-100mg/mL, preferably 2-20mg/mL, and more preferably 4-10 mg/mL.
The mass ratio of the m-aminophenol, the cetyl trimethyl ammonium bromide CTAB, the hexamethylene tetramine and the functional precursor is (0.2-100): (0.2-200): 0.1-100): 0.01-4. The mass ratio of the m-aminophenol, the cetyl trimethyl ammonium bromide CTAB and the hexamethylenetetramine is (2-20): (4-50): (2-20).
The feeding ratio of the m-aminophenol to the aqueous solution is 1.0g to 100 g. The mass of the target precursor is 0.1-1g added into the diluted solution.
The temperature of the hydrothermal reaction is 60-200 ℃. Before dilution, the hydrothermal reaction time is 0.5-3 h; after dilution, the reaction time is 1-72 h. 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 12-48 h. Further preferably, the temperature is 90-110 ℃, the reaction time before dilution is 1.5-2.5h, and the reaction time before dilution is 18-36 h. The volume of the pre-stabilized solution is diluted 10 to 1000 times, preferably 50 to 500 times, during the dilution.
Example 1
A super-assembly preparation method of a multifunctional nanowire with adjustable surface groups and components comprises the following steps:
20mL of deionized water was removed and added to a 50mL glass vial, and then 0.2g of m-aminophenol (10mg/mL), 0.2g of CTAB (10mg/mL) and 0.3g of hexamethylenetetramine (15mg/mL) were added to the solution and stirred for 2 hours. The vial was then placed in an oven at 100 ℃ and allowed to react for 2 hours. 0.1mL of the solution was taken out and added to 9.9mL of deionized water, and after 0.2g of thiourea was added and stirred for 2 hours, the reaction was continued for 36 hours after placing the mixture in an oven at 100 ℃. Cooling to room temperature, carrying out suction filtration, respectively washing with water and ethanol, and drying to obtain the one-dimensional sulfur-doped nanowire material.
As shown in fig. 1-3, a Transmission Electron Microscope (TEM) of the multifunctional nanowire prepared in this example shows that the multifunctional nanowire prepared in fig. 1 has a linear structure and is uniformly dispersed; FIG. 2 is a further enlarged TEM image, visible as having a one-dimensional line structure; statistically, the average size is 20 nm. The multifunctional high-power transmission electron microscope (HRTEM) and mapping images prepared in this example are shown in fig. 3, and fig. 3 shows C, O, N, S elements are uniformly distributed, which indicates that the obtained nanowire material is surface-doped with S.
Example 2
A super-assembly preparation method of a multifunctional nanowire with adjustable surface groups and components comprises the following steps:
20mL of deionized water was removed and added to a 50mL glass vial, and then 0.2g of m-aminophenol (10mg/mL), 0.2g of CTAB (10mg/mL) and 0.3g of hexamethylenetetramine (15mg/mL) were added to the solution and stirred for 2 hours. The vial was then placed in an oven at 100 ℃ and allowed to react for 2 hours. 0.1mL of the solution was taken out and added to 9.9mL of deionized water, and 0.2g of hexadecyltriethoxy silicon was added and stirred for 2 hours, after which the reaction was continued in an oven at 100 ℃ for 36 hours. Cooling to room temperature, carrying out suction filtration, respectively washing with water and ethanol, and drying to obtain the one-dimensional silicon-doped nanowire material.
A Transmission Electron Microscope (TEM) of the multifunctional nanowire prepared in this example is shown in fig. 4, and fig. 1 shows that the multifunctional nanowire prepared in this example has a linear structure; statistically, the average size is 20 nm. The multifunctional high-power transmission electron microscope image and mapping image prepared in this example are shown in fig. 5, and fig. 5 shows C, O, N, Si elements uniformly distributed, which indicates that the obtained surface-doped Si nanowire material.
Example 3
A super-assembly preparation method of a multifunctional nanowire with adjustable surface groups and components comprises the following steps:
20mL of deionized water was removed and added to a 50mL glass vial, and then 0.2g of m-aminophenol (10mg/mL), 0.2g of CTAB (10mg/mL) and 0.3g of hexamethylenetetramine (15mg/mL) were added to the solution and stirred for 2 hours. The vial was then placed in an oven at 100 ℃ and allowed to react for 2 hours. 0.1mL of the solution was taken out and added to 9.9mL of deionized water, and 0.1g of ruthenium trichloride was added thereto and stirred for 2 hours, after which the reaction was continued in an oven at 100 ℃ for 36 hours. Cooling to room temperature, carrying out suction filtration, washing with water and ethanol respectively, and drying to obtain the one-dimensional ruthenium-doped nanowire material.
A Transmission Electron Microscope (TEM) of the multifunctional nanowire prepared in this example is shown in fig. 6, and fig. 1 shows that the multifunctional nanowire prepared in this example has a linear structure; statistically, the average size is 20 nm. The multifunctional high-power transmission electron microscope image and mapping image prepared in this example are shown in fig. 7, and fig. 7 shows C, O, N, Ru elements are uniformly distributed, which indicates that the obtained surface-doped Ru nanowire material.
Example 4
A super-assembly preparation method of a multifunctional nanowire with adjustable surface groups and components comprises the following steps:
20mL of deionized water was removed and added to a 50mL glass vial, and then 0.2g of m-aminophenol (10mg/mL), 0.2g of CTAB (10mg/mL) and 0.3g of hexamethylenetetramine (15mg/mL) were added to the solution and stirred for 2 hours. The vial was then placed in an oven at 100 ℃ and allowed to react for 2 hours. 0.1mL of the solution was taken out and added to 9.9mL of deionized water, and 0.1g of platinum tetrachloride was added and stirred for 2 hours, after which the reaction was continued for 36 hours in an oven at 100 ℃. And cooling to room temperature, carrying out suction filtration, washing with water and ethanol respectively, and drying to obtain the one-dimensional platinum-doped nanowire material.
A Transmission Electron Microscope (TEM) of the multifunctional nanowire prepared in this example is shown in fig. 8, and it can be seen from fig. 1 that the multifunctional nanowire prepared in this example has a linear structure; statistically, the average size is 20 nm. The multifunctional high-power transmission electron microscope image and mapping image prepared in this example are shown in fig. 9, and fig. 9 shows C, O, N, Pt elements are uniformly distributed, which indicates that the obtained nanowire material with surface doped with Pt is obtained.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (10)
1. A super-assembly preparation method of a multifunctional nanowire with adjustable surface groups and components is characterized by comprising the following steps: adding m-aminophenol, hexamethylenetetramine and Cetyl Trimethyl Ammonium Bromide (CTAB) into an aqueous solution for hydrothermal reaction to obtain an oligomer-CTAB metastable micelle solution, diluting the solution, adding a functional precursor, and continuing to react to obtain the multifunctional nanowire with the adjustable surface groups and components.
2. The method for preparing the super-assembly of the multifunctional nanowire with tunable surface groups and components according to claim 1, wherein the mass concentration of the m-aminophenol is 0.1-100 mg/mL.
3. The method of claim 1, wherein the concentration of hexamethylenetetramine is 0.2-200 mg/mL.
4. The method of claim 1, wherein the CTAB is present in a concentration of 0.1-100mg/mL by mass.
5. The method of claim 1, wherein the mass ratio of m-aminophenol, cetyltrimethylammonium bromide CTAB, hexamethylenetetramine and the functional precursor is (0.2-100): 0.2-200): 0.1-100: 0.01-4.
6. The method of claim 1, wherein the functional precursor comprises thiourea, hexadecyltriethoxy silane, ruthenium trichloride, or platinum tetrachloride.
7. The method for preparing the multifunctional nanowire with the tunable surface groups and components in the super-assembly manner according to claim 1, wherein the temperature of the hydrothermal reaction is 60-200 ℃.
8. The method for preparing the multifunctional nanowire with the adjustable surface groups and components in the super-assembly manner according to claim 1, wherein the hydrothermal reaction time is 0.5-3h before dilution; after dilution, the reaction time is 1-72 h.
9. The method for preparing the multifunctional nanowires with tunable surface groups and components in the super-assembly manner of claim 1, wherein the volume of the pre-stabilized solution is diluted by 10-1000 times during the dilution.
10. A multifunctional nanowire with tunable surface groups and components prepared by the method of microfabrication according to any one of claims 1-9.
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Application publication date: 20220913 |