CN113789167B - Preparation method of room-temperature phosphorescent material based on carbon nano tube - Google Patents
Preparation method of room-temperature phosphorescent material based on carbon nano tube Download PDFInfo
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Abstract
The invention discloses a preparation method of a room temperature phosphorescent material based on carbon nanotubes, which takes carboxylated single-wall carbon nanotubes as a main body, boric acid and urea as dispersion matrix precursors, the carbon nanotubes are embedded into a matrix, and hydrogen bonds and covalent bonds are formed at the interface between the carbon nanotubes and the matrix for microwave reaction, so as to prepare the room temperature phosphorescent material based on the nanotubes, and the material has the following characteristics: 1) Embedding the dispersed carboxylated single-wall carbon nanotubes into a matrix, and realizing room-temperature scaliness of the carbon nanotube base for the first time; 2) Hydrogen bond and covalent bond formed by carboxylated single-wall carbon nanotubes and matrix at the interface are important factors for realizing phosphorescence; 3) The service life reaches 476.6ms, and the macroscopic afterglow exceeds 4.0s; 4) The material is synthesized by one-step reaction, the raw materials are cheap, the operation is simple, no byproducts are generated, and the yield is close to 100%.
Description
Technical Field
The invention relates to the technical field of low-dimensional carbon nano room-temperature phosphorescence, in particular to a preparation method of a carbon nano tube-based room-temperature phosphorescence material.
Background
Room temperature phosphorescent materials are receiving increasing attention due to their attractive optical properties for wide application in information security, optoelectronics and biochemistry. Low-dimensional carbon materials are a general term for a class of materials, and become important components in the field of room temperature phosphorescent materials due to their unique geometry, tunable structure, good biocompatibility, environmental friendliness, and excellent optical and electronic properties. Among them, the optical properties of single-walled carbon nanotubes are attracting attention because of their wide application prospects. To date, some strategies have been developed to achieve photoluminescence of carbon nanotubes by dispersion and functionalization. One of the most common techniques is to sonicate nanotubes in aqueous suspension with a surfactant, which molecules adsorb to the sidewalls of the dispersed single-walled carbon nanotubes to produce an electrostatic or sterically stabilized aqueous dispersion from which the carbon nanotubes can be purified and separated by the liquid phase method; in addition, photoluminescence was observed by a method of growing single carbon nanotubes in zeolite channels.
Although the above research has promoted the development of the optical properties of carbon nanotubes, the short luminescence lifetime (nanosecond level) has limited the development and application of the optical properties of carbon nanotubes. Therefore, development of a carbon nanotube-based room temperature phosphorescent material with long lifetime has breakthrough significance. There are many researches on low-dimensional carbon nano room temperature phosphorescent materials at present, and the researches mainly focus on room temperature phosphorescence of carbon quantum dots and graphene. Summarizing the reported literature, the most prominent challenges in achieving low dimensional carbon nano room temperature phosphorescent materials are triplet exciton deficiency and non-radiative deactivation. The strategies they take are as follows: on the one hand, introducing hetero atoms (e.g., N, P, F, and B) with empty P orbitals, the energy level difference between the triplet and singlet states is reduced, thereby effectively filling the triplet excitons; on the other hand, the non-radiative transition process is inhibited by limiting the rate of non-radiative transition by immobilization (formation of hydrogen bonds, covalent bonds, intercalation of matrix, etc.).
Disclosure of Invention
The invention aims to provide a preparation method of a carbon nanotube-based room-temperature phosphorescent material, which takes carboxylated single-wall carbon nanotubes as a main body and obtains the nanotube-based room-temperature phosphorescent material by the synergistic fixation effect of hydrogen bonds and covalent bonds.
To achieve the purpose, the invention adopts the following technical scheme:
1. the preparation process of carbon nanotube base room temperature phosphorescent material with carboxylated single wall carbon nanotube as main body and boric acid and urea as precursor of dispersed matrix includes the following steps:
1) Preparing an aqueous dispersion of carbon nanotubes. Dispersing the carbon nano tube in a sample bottle containing deionized water, carrying out ultrasonic treatment, and standing to obtain a carbon nano tube dispersion liquid with uniform upper layer for standby.
2) Preparation and treatment of the reaction solution. Deionized water, boric acid, urea and the uniform carbon nanotube dispersion in step 1) were added into a clean 100ml small beaker and sonicated for 3-5min.
3) Placing the small beaker containing the reaction liquid in the step 2) in a microwave oven for microwave reaction, embedding the carbon nano tube into a matrix, and forming a hydrogen bond and a covalent bond at the interface between the carbon nano tube and the matrix to obtain off-white solid powder.
4) After the reaction is finished, the product in the step 3) is scraped by a medicine spoon while the reaction is hot, and is quickly transferred into a dry sample bottle for sealing and preservation.
2. According to a further technical scheme, the carbon nanotubes in the step 1) are carboxylated single-walled carbon nanotubes containing defects.
3. According to a further technical scheme, the ultrasonic time in the step 1) is 2 hours, and the ultrasonic treatment is carried out for 3 minutes.
4. According to a further embodiment, the mass ratio of boric acid to urea in step 2) is about 1:2, and the deionized water is present in an amount sufficient to dissolve the boric acid and urea.
5. According to a further technical scheme, the conditions of the microwave reaction in the step 3) are as follows: the gear is high fire, and the reaction time is 10min.
Compared with the prior art, the invention has the following beneficial effects:
embedding the dispersed carboxylated single-walled carbon nanotubes into a matrix to realize the carbon nanotube-based room temperature phosphorescent material for the first time; hydrogen bonds and covalences formed by carboxylated single-wall carbon nanotubes and a matrix at the interface are important factors for realizing phosphorescence; the service life reaches 476.6ms, and the macroscopic afterglow exceeds 4.0s; the invention synthesizes materials by adopting one-step reaction, has cheap raw materials, simple operation, no byproducts and yield approaching 100 percent.
Drawings
FIG. 1 is a photograph showing the room temperature phosphorescent material prepared in example 1 of the present invention under sunlight, when the ultraviolet lamp is irradiated (fluorescence) and after the ultraviolet lamp is turned off (phosphorescence).
FIG. 2 is a graph showing the morphology of the carbon nanotube-based room temperature phosphorescent material of example 1 of the present invention under high power transmission electron microscopy;
FIG. 3a is a C1 s high resolution X-ray photoelectron spectroscopy (XPS) contrast plot of the phosphorescent material (C-CNT@BNO) prepared in example 1 of the present invention and its matrix (BNO), wherein the abscissa indicates binding energy and the ordinate indicates relative photoelectron flow intensity;
FIG. 3b is a Fourier transform infrared spectrum (FTIR) comparison plot of the long persistence material (c-CNT@BNO) prepared in example 1 of the invention and its matrix (BNO), wherein the abscissa is wave number and the ordinate is transmittance (%);
FIG. 4a is a Fourier transform infrared spectrum (FTIR) comparison plot of the long persistence material (c-CNT@BNO) prepared in example 1 of the invention and its reactants (c-CNT, urea and BA), wherein the abscissa is wavenumber and the ordinate is transmittance (%);
FIG. 4B is a B1 s high resolution X-ray photoelectron spectroscopy (XPS) contrast plot of the phosphorescent material prepared in example 1 of the present invention, wherein the abscissa represents binding energy or kinetic energy and the ordinate represents relative photoelectron flow intensity;
FIG. 5a is a graph showing fluorescence and phosphorescence spectra of the carbon nanotube-based room temperature phosphorescent material of example 1 of the present invention after excitation by 240nm (optimal excitation wavelength) ultraviolet light, wherein the abscissa indicates wavelength and the ordinate indicates intensity;
FIG. 5b is a graph showing the phosphorescence lifetime of the carbon nanotube-based room temperature phosphorescent material of example 1 of the present invention after excitation by 240nm (optimal excitation wavelength) ultraviolet light.
FIG. 6a is the UV-Vis absorption spectrum and phosphorescent excitation spectrum of the carbon nanotube-based room temperature phosphorescent material in example 1 of the present invention.
FIG. 6b is a graph of fluorescence and phosphorescence spectra of a product obtained by a control experiment using hydroxylated carbon nanotubes, wherein the internal pictures are optical photographs of the product under sunlight, ultraviolet light and turning off an ultraviolet lamp, respectively.
Detailed Description
To facilitate understanding of the present invention, examples are set forth below. The examples are merely provided to aid in understanding the invention and should not be construed as a specific limitation of the invention. It should be noted that modifications and adaptations to the present invention may occur to one skilled in the art without departing from the principles of the present invention and are intended to be comprehended within the scope of the present invention.
Example 1
The preparation process of carbon nanotube base room temperature phosphorescent material includes the following steps:
1) Preparing aqueous dispersion of carbon nano tube. Dispersing excessive carboxylated single-wall carbon nanotubes in a wide-mouth sample bottle containing 20ml of deionized water, carrying out ultrasonic treatment for 2 hours, and standing for 3 minutes for standby, thus obtaining an upper-layer uniform carbon nanotube dispersion liquid.
2) Preparation and treatment of the reaction solution. 13.5ml deionized water, 0.6g boric acid, 0.3g urea, 1.5ml of the uniform carbon nanotube dispersion of step 1) were added to a clean 100ml small beaker and sonicated for 3-5min.
3) Placing the small beaker containing the reaction liquid in the step 2) into a microwave oven for microwave reaction, wherein the gear is high fire, and the reaction time is 10min. An off-white solid powder was obtained.
4) After the reaction is completed, the product is scraped by a medicine spoon while the product is hot and rapidly transferred into a dry sample bottle, and the sample bottle is sealed and stored.
The following characterization was performed for the product:
1. taking photographs of the carbon nano tube-based room temperature phosphorescent material under sunlight, when the ultraviolet lamp irradiates and after the ultraviolet lamp is turned off
The fluorescent powder presents grey white powder under sunlight, emits blue fluorescence and green phosphorescence, and the phosphorescence can last for more than 4 s.
2. Analyzing the shape, size and aggregation state of the carbon nanotube-based room temperature phosphorescent material by using a scanning electron microscope
Dispersing the powder of the carbon nano tube-based room temperature phosphorescent material in the step 4) into deionized water, and standing for 24 hours to ensure that the powder is dispersed to the greatest extent. Dripping on the micro-grid carbon film, baking, and scanning by high-power transmission electron microscope. The test results are shown in fig. 2, and it can be seen from the pictures that the carbon nanotubes are in a single dispersed state under the action of the matrix.
3. Verification of the Hydrogen bonding formed newly in the phosphorescent Material prepared in example 1 of the present invention
As shown in fig. 3a, the C1 s binding energy of c=o blue shifted from 289.4eV to 289.6eV; in FIG. 3b, the stretching vibration peak of hydroxyl (-OH) or hydrogen bond in the carbon nanotube-based room temperature phosphorescent material (c-CNT@BNO) (3435-3200 cm -1 ) Becomes stronger relative to its matrix (BNO). Indicating the presence of hydrogen bonds in the nanotube-based room temperature phosphorescent material.
4. Verification of the newly formed covalent bond of the phosphorescent material prepared in example 1 of the present invention
FTIR of phosphorescent materials can represent the surface chemical bonding conditions, as shown in fig. 4a, corresponding chemical bonds to the starting materials used to synthesize the nanoparticles, such as c-CNT, urea, and B-O, N-H, C =o. Furthermore, 1250cm -1 The absorption peak at this point may be derived fromNewly formed B-C bonds. B1 s high-resolution X-ray photoelectron spectrum shows that B-O (193.1 eV) and BCO exist in the long afterglow powder 2 (192.6 eV) and B-N (190.8 eV) bonds. The two mutually prove that B-C bonds are generated in the prepared phosphorescent material.
5. Optical performance of carbon nano tube based room temperature phosphorescent material is tested by adopting steady state/transient state fluorescence spectrometer
FIGS. 5a and 5b are respectively a fluorescence spectrum diagram, a phosphorescence spectrum diagram and a phosphorescence attenuation diagram of the carbon nanotube-based room temperature phosphorescent material of example 1 after excitation by ultraviolet light with an optimal excitation wavelength (240 nm), wherein the optimal emission wavelengths of fluorescence and phosphorescence are 463nm and 480nm, respectively, and blue fluorescence and green phosphorescence are presented; the phosphorescent lifetime is 476.6ms.
6. Analysis of luminescence sources of carbon nanotube-based room temperature phosphorescent materials by comparing UV-Vis absorption spectra and excitation spectra in combination with control experiments
FIG. 6a is a UV-Vis absorption spectrum and a phosphorescence excitation spectrum of a carbon nanotube-based room temperature phosphorescent material of example 1 of the present invention. Absorption spectrum (dotted line) shows strong absorption peak at 240nm and weak shoulder near 300nm, and sp originated from typical graphene structure (c=c) 2 Pi-pi transition in carbon and n-pi transition of carbonyl (c=o) on the surface of carbon nanotube. The phosphorescence excitation spectrum (solid line) shows a narrow peak at 240nm, with a high overlap with the absorption region of the c=c bond, indicating that the triplet excited state is mainly derived from local sp 2 -pi transition in the C subdomain; meanwhile, the overlap of the excitation peak around 355nm and the weak shoulder around 300nm of the absorption spectrum means that the n-pi transition of c=o may be another source of phosphorescence. C=o has been shown to be effective in enhancing spin-orbit coupling and promoting triplet exciton generation. To determine the key role of c=o in achieving carbon nanotube-based room temperature phosphorescence, a control experiment was performed with hydroxylated carbon nanotubes (h-CNTs) instead of carboxylated carbon nanotubes (C-CNTs) in example 1. FIG. 6b is a graph of fluorescence and phosphorescence spectra of a product obtained by a control experiment performed on hydroxylated carbon nanotubes, and the internal pictures are optical photographs of the product under sunlight, ultraviolet light and turning off an ultraviolet lamp, respectively. It was found that neither fluorescence nor phosphorescence was present, probably due to h-CNTsThere is no c=o bond. The key role of c=o in achieving carbon nanotube-based room temperature phosphorescence was demonstrated.
In summary, the carbon nanotube-based room temperature phosphorescent material of example 1 of the present invention emits light from the above two sources.
Claims (2)
1. A preparation method of a carbon nano tube-based room temperature phosphorescent material is characterized by comprising the following steps: the method takes carboxylated single-walled carbon nanotubes as a main body, takes boric acid and urea as a dispersion matrix precursor and comprises the following steps:
1) Dispersing carboxylated single-walled carbon nanotubes in deionized water for ultrasonic treatment, and standing to obtain an upper uniform carboxylated single-walled carbon nanotube dispersion;
2) Adding deionized water, boric acid and urea to a clean container to form a dispersion matrix precursor solution, wherein the mass ratio of the boric acid to the urea is about 2:1, and the deionized water is used for dissolving the boric acid and the urea; mixing the aqueous dispersion liquid of the carbon nano tube which is uniform in the step 1) with a dispersion matrix precursor solution, and carrying out ultrasonic treatment;
3) Placing the container containing the reaction liquid in the step 2) in a microwave oven for microwave reaction, embedding the carboxylated single-walled carbon nanotubes into a matrix, and forming hydrogen bonds and covalent bonds at the interface between the carboxylated single-walled carbon nanotubes and the matrix to obtain off-white solid powder; the covalent bond is a B-C bond.
2. The method for preparing the carbon nanotube-based room temperature phosphorescent material according to claim 1, wherein the method comprises the steps of: the ultrasonic time in the step 1) is 2 hours, and the ultrasonic treatment is carried out for 3 minutes.
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