CN111004625B - Method for enhancing graphite phase carbon nitride defect state electrochemiluminescence - Google Patents
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Abstract
The invention discloses a method for enhancing graphite phase carbon nitride defect state electrochemiluminescence, which realizes local denitrification and recombination of common carbon nitride through high-temperature treatment so as to realize local graphitization; and then the strong oxidizing property of the concentrated nitric acid is utilized to destroy the formed local graphite structure, so that the graphite phase carbon nitride forms more surface defects. Compared with the common graphite phase carbon nitride material, the electrochemiluminescence activity of the graphite phase carbon nitride material obtained by the method is improved by 5-20 times, and the signal is more stable. Has better popularization value and application prospect.
Description
Technical Field
The invention belongs to the field of material preparation, and particularly relates to a method for enhancing graphite phase carbon nitride defect state electrochemiluminescence.
Background
Graphite phase carbon nitride (g-C) 3 N 4 ) Mainly consists of two elements of nitrogen and carbon, and is a two-dimensional soft material. g-C, unlike graphene 3 N 4 Is a semiconductor with a moderate bandgap (approximately 2.7 eV). Thus, g-C 3 N 4 Have many very unique properties including catalysis, photocatalysis, fluorescence, electrochemiluminescence, etc. In particular, the outstanding electrochemiluminescence activity of the compound is generally concerned by a large number of analysts. As a new electrogenerated chemiluminescence body, g-C 3 N 4 Can form a coreactant system with the peroxydisulfate to generate a strong cathodoluminescence signal, thereby having wide application prospect in the field of analysis and detection. With respect to g-C 3 N 4 The current research result is generally considered to be related to the band gap of the electrochemiluminescence mechanism, and the important role of the surface defect state is generally ignored. The invention introduces a method for improving g-C 3 N 4 Surface defect density to improve its electrochemiluminescence activity.
The invention realizes partial denitrification and recombination of common carbon nitride through high-temperature treatment, thereby realizing partial graphitization. And then the strong oxidizing property of the concentrated nitric acid is utilized to destroy the formed local graphite structure, so that the graphite phase carbon nitride forms more surface defects. Compared with the common graphite phase carbon nitride material, the electrochemiluminescence activity of the graphite phase carbon nitride material obtained by the method is obviously improved, and the signal is more stable.
Disclosure of Invention
The invention aims to provide a method for improving graphite phase carbon nitride (g-C) 3 N 4 ) The method for enhancing the electrochemiluminescence activity of the graphite-phase carbon nitride nano material by using the surface defect density solves the problems of low electrochemiluminescence activity and unstable signals of the common graphite-phase carbon nitride nano material.
In order to realize the purpose, the technical scheme of the invention is as follows:
a method for enhancing graphite phase carbon nitride defect state electrochemiluminescence comprises the following steps:
(1) Conventional preparation of graphite phase carbon nitride
The bulk graphite phase carbon nitride is prepared by a solid phase thermal polymerization method. Weighing a certain amount of precursor, placing the precursor in a muffle furnace, heating to 550 ℃ at the heating rate of 2.3 ℃/min, preserving heat for 4 hours to ensure that the precursor is fully polymerized to obtain yellow blocky carbon nitride, naturally cooling to room temperature, and grinding into powder for later use.
Preferably, the precursor can be one of carbon and nitrogen compounds such as melamine, dicyandiamide and urea, and the dosage is 5 g.
(2) High temperature treatment
The common carbon nitride can realize local denitrification and recombination through high-temperature treatment, thereby realizing local graphitization. Specifically, the method comprises the following steps: and (2) placing the powder obtained in the step (1) in a tube furnace, vacuumizing the inside of a quartz tube by using a vacuum pump, introducing inert gas to restore to the standard atmospheric pressure, repeating the step for 3 times to ensure that the inside of the tube is in the inert gas atmosphere, setting the temperature to be 650-750 ℃, keeping the reaction for 0.5-3 h, and cooling to room temperature for later use.
Preferably, the inert gas can be one of nitrogen or argon, the heating rate is 5 ℃/min, the temperature is set to be 750 ℃, and the holding time is 0.5 h.
(3) Reflux of nitric acid
The strong oxidizing property of the concentrated nitric acid can destroy the local graphite structure formed by high-temperature treatment, so that more surface defects are formed by graphite phase carbon nitride. Specifically, the method comprises the following steps: and (3) adding a proper amount of the powder obtained after the high-temperature treatment in the step (2) into concentrated nitric acid for oxidizing and refluxing for a certain time. After the reaction is finished, obtaining a solid through suction filtration and separation, washing the solid to be neutral, drying and storing the solid in a dry environment for later use.
The concentration of the concentrated nitric acid is 4-16 mol/L, the reflux time is 6-36 h, preferably, the mass of the used carbon nitride powder is 1 g, the concentration of the concentrated nitric acid is 8mol/L, and the reflux time is 24 h.
(4) Electrochemiluminescence activity assay
And (3) dripping carbon nitride turbid liquid with certain mass on the surface of a clean glassy carbon electrode for drying and standby. An electrochemiluminescence detector is adopted, a saturated silver/silver chloride electrode is used as a reference electrode, a platinum electrode is used as a counter electrode, a glassy carbon electrode modified with carbon nitride is used as a working electrode, and a three-electrode system is adopted to measure the electrochemiluminescence activity of common carbon nitride and specially treated carbon nitride in electrolyte.
Preferably, the mass of the carbon nitride finally modified on the glassy carbon electrode is 5. Mu.g, and the electrolyte is 0.1 mol/L phosphate buffer solution containing 1 mM potassium persulfate, and the pH value thereof is 7.4. The scanning mode is cyclic voltammetry, the applied voltage is 0 to-1.3V, the scanning speed is 0.1V/s, and the voltage of a photomultiplier tube is 850V.
Has the advantages that: compared with the prior art, the invention has the following advantages:
1. the invention firstly proposes that the local graphitization of the carbon nitride can be realized through high-temperature treatment, and the formed local graphite structure is destroyed by utilizing the oxidation of concentrated nitric acid, so that more surface defects are formed on the graphite phase carbon nitride.
2. Compared with common carbon nitride, the carbon nitride prepared by the invention has higher electrochemiluminescence activity and stability and good application prospect.
Drawings
FIG. 1 is a general g-C 3 N 4 High power transmission electron micrographs of;
FIG. 2 is g-C of partial graphitization after high temperature treatment 3 N 4 High power transmission electron micrographs of;
FIG. 3 is a graph of g-C of high surface defect density after nitric acid reflux 3 N 4 High power transmission electron micrographs of;
FIG. 4 shows a general g-C 3 N 4 （CN 550 ) And the high surface defect density g-C of the present invention 3 N 4 （CN 750 ) Comparison of electrochemiluminescence spectra of (a);
FIG. 5 shows a general g-C 3 N 4 （CN 550 ) And g-C of high surface defect density of the present invention 3 N 4 （CN 750 ) At the same massComparative plot of electrochemiluminescence intensity.
Detailed Description
For further disclosure, but not limitation, the present invention is described in further detail below with reference to examples.
Example 1:
(1) Weighing 5 g melamine solid powder, placing in a muffle furnace, heating to 550 ℃ at a heating rate of 2.3 ℃/min, keeping the temperature for 4 hours to obtain yellow block-shaped carbon nitride, and grinding into powder. Transferring the sample into a tubular furnace, taking argon as protective gas, repeatedly vacuumizing and introducing the protective gas for 3 times before calcination, wherein the gas flow rate is 50 sccm, heating to 750 ℃ from room temperature at 5 ℃/min during calcination, continuously reacting at the temperature for 0.5 h, and then cooling to room temperature to obtain orange fluffy powder, namely the obtained sample, wherein a high-power transmission electron microscope picture of the sample is shown in figure 2, and a graphite structure formed after high-temperature treatment is shown in a dotted frame in the figure. Compared with common carbon nitride (shown in figure 1), the transmission electron microscope image of the carbon nitride has clearer lattice stripes, which shows that the carbon nitride is locally deaminated and recombined to form a graphitized structure after being treated at the high temperature of 750 ℃.
(2) Weighing 1 g of the finally obtained sample in the step (1) into a 250mL round-bottom flask, adding 100 mL nitric acid with the concentration of 8mol/L, refluxing 24 h under the heating condition of 130 ℃, then performing suction filtration to separate out solids, washing with water to be neutral, drying and placing in a dry environment for later use, wherein a TEM image is shown in figure 3, and a pore structure formed after the nitric acid is refluxed is shown in a dotted line frame in the figure. After nitric acid reflux, not only the graphitized structure formed by high-temperature treatment is damaged, but also the existence of pores shows that the continuity of the original carbon nitride structure is also damaged, thereby leading to the increase of defect state density.
(3) Accurately weighing 25 mg and fixing the volume of the finally obtained sample in the step (2) to 50 mL. 10 μ L of the solution was dropped on a glassy carbon surface and dried at room temperature for use. The glassy carbon electrode modified with carbon nitride was scanned for stability at a potential of 0 to-1.3V in 0.1M phosphate buffer (pH = 7.4) electrolyte containing 1 mM potassium persulfate, and the light intensity I was recorded and the corresponding electrochemiluminescence spectrum was recorded. Compared with common carbon nitride which is not treated by high temperature and nitric acid oxidation, the electrochemiluminescence result is shown inFig. 4 and 5. g-C obtained after high-temperature treatment and nitric acid reflux 3 N 4 The luminous intensity is ordinary g-C 3 N 4 13.2 times of luminous intensity and common g-C in electrochemical luminescence spectrum 3 N 4 The two emission peaks at 434 nm and 461 nm are red shifted to 481 nm and combined into one peak. The reason for this may be that the partially deaminized, reformed graphitized g-C is treated at high temperature and refluxed with nitric acid 3 N 4 The graphitized structure of the compound is destroyed, the surface defects are increased, the electrochemical luminescence activity is enhanced, and the shape and the position of an emission peak in an electrochemical luminescence spectrum are changed.
Example 2:
(1) Weighing 5 g melamine solid powder, placing in a muffle furnace, heating to 550 ℃ at a heating rate of 2.3 ℃/min, preserving heat for 4 hours to obtain yellow block-shaped carbon nitride, and grinding into powder. Transferring the mixture into a tubular furnace, taking argon as protective gas, repeatedly vacuumizing and introducing the protective gas for 3 times before calcination, wherein the gas flow rate is 50 sccm, heating to 650 ℃ from room temperature at 5 ℃/min during calcination, continuously reacting at the temperature for 1 h, and then cooling to room temperature to obtain dark yellow powder, namely the obtained sample.
(2) Weighing 1 g of the sample finally obtained in the step (1) into a 250mL round-bottom flask, adding nitric acid 100 mL with the concentration of 16 mol/L, refluxing 24 h under the heating condition of 130 ℃, then performing suction filtration to separate out a solid, washing with water to be neutral, drying and placing in a dry environment for later use.
(3) Accurately weighing 25 mg and fixing the volume of the finally obtained sample in the step (2) to 50 mL. 10 μ L of the solution was dropped on a glassy carbon surface and dried at room temperature for use. The glassy carbon electrode modified with carbon nitride was scanned stably in 0.1M phosphate buffer (pH = 7.4) electrolyte at a potential of 0 to-1.3V containing 1 mM potassium persulfate, the light intensity I was recorded, and the corresponding electrochemiluminescence spectrum was recorded. Compared with the commonly prepared carbon nitride, the luminous intensity of the material is enhanced by 5.9 times, and the emission peak in an electrochemical luminescence spectrum is slightly red-shifted.
Example 3:
(1) Weighing 5 g melamine solid powder, placing in a muffle furnace, heating to 550 ℃ at a heating rate of 2.3 ℃/min, preserving heat for 4 hours to obtain yellow block-shaped carbon nitride, and grinding into powder. Transferring the material to a tubular furnace, taking nitrogen as protective gas, repeatedly vacuumizing and introducing the protective gas for 3 times before calcination, wherein the gas flow rate is 50 sccm, heating to 750 ℃ from room temperature at 5 ℃/min during calcination, continuously reacting at the temperature for 1 h, and then cooling to room temperature to obtain orange fluffy powder, namely the obtained sample.
(2) Weighing 1 g of the sample finally obtained in the step (1) into a 250mL round-bottom flask, adding 100 mL nitric acid with the concentration of 16 mol/L, refluxing 8 h under the heating condition of 130 ℃, then performing suction filtration to separate out a solid, washing with water to be neutral, drying and placing in a dry environment for later use.
(3) Accurately weighing 25 mg and fixing the sample obtained in the step (2) to 50 mL. 10 μ L of the solution was dropped on a glassy carbon surface and dried at room temperature for use. The glassy carbon electrode modified with carbon nitride was scanned stably in 0.1M phosphate buffer (pH = 7.4) electrolyte at a potential of 0 to-1.3V containing 1 mM potassium persulfate, the light intensity I was recorded, and the corresponding electrochemiluminescence spectrum was recorded. Compared with the commonly prepared carbon nitride, the luminous intensity of the material is enhanced by 7.3 times, and the emission peak in an electrochemical luminescence spectrum is slightly red-shifted.
The above examples are only for describing the preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should be made within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (3)
1. A method for enhancing graphite phase carbon nitride defect state electrochemiluminescence is characterized in that: placing graphite-phase carbon nitride in a vacuum tube furnace, and performing high-temperature treatment under the protection of inert atmosphere to perform local denitrification and recombination to obtain locally graphitized carbon nitride nanosheets; refluxing the obtained product and concentrated nitric acid to destroy a graphitized structure in the product, and finally filtering and washing to obtain a carbon nitride nanosheet with high defect state density and ultrahigh electrochemiluminescence activity; the high-temperature treatment temperature is 750 ℃, and the high-temperature treatment time is 0.5-3 h; the concentration of the concentrated nitric acid is 8mol/L, and the reflux time is 6-36 h.
2. The method of enhancing graphite phase carbon nitride defect state electrochemiluminescence according to claim 1, wherein: the graphite-phase carbon nitride is prepared by taking melamine, dicyandiamide or urea as raw materials and carrying out thermal polymerization.
3. The method of enhancing graphite phase carbon nitride defect state electrochemiluminescence according to claim 1, wherein: the inert atmosphere used is nitrogen or argon.
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| CN108355702A (en) * | 2018-03-23 | 2018-08-03 | 辽宁大学 | A kind of bigger serface carbon defects graphite phase carbon nitride photochemical catalyst and its preparation method and application |
| CN108380237A (en) * | 2018-05-04 | 2018-08-10 | 辽宁大学 | Nitrogen defect graphite phase carbon nitride nanosheet photocatalyst and the preparation method and application thereof |
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| CN108355702A (en) * | 2018-03-23 | 2018-08-03 | 辽宁大学 | A kind of bigger serface carbon defects graphite phase carbon nitride photochemical catalyst and its preparation method and application |
| CN108380237A (en) * | 2018-05-04 | 2018-08-10 | 辽宁大学 | Nitrogen defect graphite phase carbon nitride nanosheet photocatalyst and the preparation method and application thereof |
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| Improved fluorescence test of chromium (VI) in aqueous solution with g-C3N4 nanosheet and mechanisms;Ying-Sha Liu, et al.;《Materials Research Bulletin》;20181128;第112卷;第9–15页 * |
| Ying-Sha Liu, et al..Improved fluorescence test of chromium (VI) in aqueous solution with g-C3N4 nanosheet and mechanisms.《Materials Research Bulletin》.2018,第112卷 * |
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