CN111678906A - MoS2Surface-enhanced Raman substrate made of Ag-N-doped graphene nanocomposite and preparation method thereof - Google Patents
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Abstract
The invention relates to a MoS2an-Ag-nitrogen doped graphene nanocomposite surface enhanced Raman substrate and a preparation method thereof. Firstly, taking aminopyrene as a raw material, carrying out hydrothermal reaction to prepare nitrogen-doped graphene quantum dots, and then carrying out esterification and addition polymerization to obtain an NG-HDO film; then surface Ag nano particle modification is carried out, and finally MoS is carried out2And (4) coating the nano particles. By the above-mentioned production method, canThe defects of large background noise signal, insufficient detection signal intensity and poor sensitivity existing in the common graphene-based surface enhanced Raman substrate are overcome, and the MoS with high detection signal intensity, excellent detection accuracy and excellent sensitivity is obtained2The surface of the-Ag-nitrogen doped graphene nanocomposite is enhanced by Raman spectroscopy.
Description
Technical Field
The invention belongs to a nano composite material, and particularly relates to a semiconductor-Ag-nitrogen doped graphene nano composite material and application thereof in a surface enhanced Raman substrate.
Background
The nano composite material has wide application in various fields according to different materials. Among them, the nanoprobe in the nano detection analysis technology is one of the most common application fields of the nano composite material.
For the detection and analysis technology, Surface Enhanced Raman Spectroscopy (SERS) is the most commonly used detection and analysis technology, and has the advantages of high sensitivity, traceless detection, wide application range and the like. The noble metal nano particles and the composite film thereof have higher surface plasmon resonance effect and are the first generation of surface enhanced Raman substrates. Among noble metals, Ag has high activity, low cost and the widest application range. However, the precious metal alone as a substrate probe is easily interfered, and the accuracy and sensitivity of detection are not sufficient. Therefore, scientific researchers combine semiconductors with good forbidden bandwidth on the surface of the noble metal nanoparticles, and the intensity of detection signals can be obviously enhanced. However, the background signal of the semiconductor material itself causes a certain interference to the final detection signal, and the aggregation of particles is easily generated on the surface of the base probe having the nanoparticle structure, which is insufficient in the stability of the detection result.
With the advent of graphene, the excellent physical, chemical and electrical properties of graphene attract extensive application research on graphene by extensive researchers. In the aspect of the surface-enhanced Raman substrate probe, the graphene is used as a substrate, the noble metal nano particles and the semiconductor are grown on the surface of the graphene, and then the graphene is used as the surface-enhanced Raman substrate probe, so that the specific surface area of the probe can be effectively increased, the strength of a detection signal is enhanced, and the detection sensitivity is improved. The common graphene has excellent conductivity, but the detection signal of the surface enhanced raman substrate probe taking the graphene as the substrate is still large in noise signal, and the application of the graphene in the aspect of accurate qualitative and quantitative detection and analysis is still insufficient.
In known research results, the electrochemical performance and the cycling stability of the nitrogen-doped graphene are superior to those of common graphene, because the doped nitrogen atoms can induce to form high local charges on the surface of the graphene and generate high spin density, the chemical activity of the graphene is improved. However, at present, research on nitrogen-doped graphene is mainly applied to the field of batteries, and few applications related to other fields, particularly the field of surface enhanced raman substrates, exist.
Therefore, aiming at the defects of the existing surface enhanced Raman substrate, the invention aims to provide the surface enhanced Raman substrate with strong detection signal, high sensitivity and good stability.
Disclosure of Invention
According to the invention, on the basis of improving the detection accuracy, sensitivity and the like of the surface-enhanced Raman substrate probe, the nitrogen-doped graphene is introduced, so that the interference of background signals in detection signals is improved, and the detection signal intensity and sensitivity of the probe are enhanced.
MoS2The preparation method of the-Ag-nitrogen doped graphene nanocomposite surface enhanced Raman substrate comprises the following steps:
(1) carrying out hydrothermal reaction on aminopyrene in a sodium hydroxide aqueous solution to obtain a nitrogen-doped graphene quantum dot solution;
(2) carrying out vacuum filtration on the nitrogen-doped graphene quantum dot solution obtained in the step (1), and carrying out self-assembly to obtain a nitrogen-doped graphene thin film (NG) with a self-supporting structure;
(3) soaking the nitrogen-doped graphene film NG obtained in the step (2) in a tetrahydrofuran solution of 2, 4-heptadecadiyne-1-ol (HDO) for esterification, and then performing addition polymerization reaction by ultraviolet irradiation to obtain an NG-HDO film;
(4) ultrasonically dispersing the NG-HDO film obtained in the step (3) in water, then adding silver nitrate, performing magnetic stirring, finally adding a sodium citrate solution, controlling the temperature to be 80-90 ℃, and preserving the heat for 30min until the solution becomes dark green, so as to obtain a dispersion liquid of the NG-HDO film with Ag nano particles modified on the surface;
(5) adding sodium molybdate and cysteine into the dispersion liquid of the NG-HDO film modified with the Ag nano particles on the surface obtained in the step (4), uniformly mixing, and reacting for 8-12h at the temperature of 180-; finally separating and purifying to obtain the MoS2The surface of the-Ag-nitrogen doped graphene nanocomposite is enhanced by Raman spectroscopy.
Wherein in the step (1), the concentration of the aminopyrene is 0.002-0.02mol/L, and the concentration of the sodium hydroxide is 0.05-0.5 mol/L; the temperature of the hydrothermal reaction is 150 ℃ and 200 ℃.
In the step (3), the concentration of a tetrahydrofuran solution of 2, 4-heptadecadiyne-1-ol (HDO) is 3-5g/L, and the mass ratio of the nitrogen-doped graphene film to the 2, 4-heptadecadiyne-1-ol is 10-20: 1; the ultraviolet irradiation time is 1-3h, and the ultraviolet wavelength is 365 nm.
Wherein, in the step (4), the concentration of the aqueous dispersion of the NG-HDO film is controlled to be 1-3wt%, and after silver nitrate is added, the concentration of the silver nitrate is controlled to be 10-20 wt%.
Wherein in the step (5), the mass ratio of the NG-HDO film to the sodium molybdate to the cysteine is controlled to be 1: (10-15): (10-15).
Through the method, the invention also prepares the MoS2The surface of the-Ag-nitrogen doped graphene nanocomposite is enhanced by Raman spectroscopy.
In the invention, the specially-made nitrogen-doped graphene is adopted as the substrate, so that the intensity, the detection accuracy and the sensitivity of a detection signal are obviously improved.
The method for preparing the nitrogen-doped graphene by taking the aminopyrene as the raw material and carrying out the hydrothermal reaction is simple, the thickness of the graphene is uniform and is about the thickness of 2-3 layers of single-layer graphene, the nitrogen-doped graphene substrate with the quasi-two-dimensional structure can provide an effective large specific surface area, the active point positions of the surface enhanced Raman substrate in detection are increased, and the detection signal intensity and sensitivity are improved. Moreover, the prepared graphene quantum dots have a single crystal structure and good structural stability, and guarantee is provided for the stability of the surface enhanced Raman substrate.
The method has the advantages that the nitrogen-doped graphene is further subjected to esterification and addition polymerization, so that the strength and the conductivity of the graphene can be effectively improved, the excellent electromagnetic shielding efficiency is obtained, the background interference resistance of the surface enhanced Raman substrate is enhanced, and the detection accuracy and sensitivity of the surface enhanced Raman substrate are improved.
Detailed Description
The present invention will be described in detail with reference to specific examples, but the present invention is not limited thereto.
Example 1
MoS2The preparation method of the-Ag-nitrogen doped graphene nanocomposite surface enhanced Raman substrate comprises the following steps:
(1) carrying out hydrothermal reaction on aminopyrene in a sodium hydroxide aqueous solution to obtain a nitrogen-doped graphene quantum dot solution;
(2) carrying out vacuum filtration on the nitrogen-doped graphene quantum dot solution obtained in the step (1), and carrying out self-assembly to obtain a nitrogen-doped graphene thin film (NG) with a self-supporting structure;
(3) soaking the nitrogen-doped graphene film NG obtained in the step (2) in a tetrahydrofuran solution of 2, 4-heptadecadiyne-1-ol (HDO) for esterification, and then performing addition polymerization reaction by ultraviolet irradiation to obtain an NG-HDO film;
(4) dispersing the NG-HDO film obtained in the step (3) in water at an ultrasonic temperature, then adding silver nitrate, performing magnetic stirring, finally adding a sodium citrate solution, controlling the temperature to be 90, and preserving the heat for 30min until the solution becomes dark green, so as to obtain a dispersion liquid of the NG-HDO film with the surface modified with Ag nano particles;
(5) adding sodium molybdate and cysteine into the dispersion liquid of the NG-HDO film modified with the Ag nano particles on the surface obtained in the step (4), uniformly mixing, and reacting for 8-12h at the temperature of 180-; finally separating and purifying to obtain the MoS2The surface of the-Ag-nitrogen doped graphene nanocomposite is enhanced by Raman spectroscopy.
Wherein in the step (1), the concentration of the aminopyrene is 0.01mol/L, and the concentration of the sodium hydroxide is 0.1 mol/L; the temperature of the hydrothermal reaction was 170 ℃.
In the step (3), the concentration of the tetrahydrofuran solution of 2, 4-heptadecadiyne-1-ol (HDO) is 4g/L, and the mass ratio of the nitrogen-doped graphene film to the 2, 4-heptadecadiyne-1-ol is 15: 1; the ultraviolet irradiation time is 2h, and the ultraviolet wavelength is 365 nm.
Wherein, in the step (4), the concentration of the aqueous dispersion of the NG-HDO film is controlled to be 2wt%, and after silver nitrate is added, the concentration of the silver nitrate is controlled to be 15 wt%.
In the step (5), the mass ratio of the NG-HDO film, the sodium molybdate and the cysteine is controlled to be 1: 12: 12.
example 2
MoS2The preparation method of the-Ag-nitrogen doped graphene nanocomposite surface enhanced Raman substrate comprises the following steps:
(1) carrying out hydrothermal reaction on aminopyrene in a sodium hydroxide aqueous solution to obtain a nitrogen-doped graphene quantum dot solution;
(2) carrying out vacuum filtration on the nitrogen-doped graphene quantum dot solution obtained in the step (1), and carrying out self-assembly to obtain a nitrogen-doped graphene thin film (NG) with a self-supporting structure;
(3) soaking the nitrogen-doped graphene film NG obtained in the step (2) in a tetrahydrofuran solution of 2, 4-heptadecadiyne-1-ol (HDO) for esterification, and then performing addition polymerization reaction by ultraviolet irradiation to obtain an NG-HDO film;
(4) ultrasonically dispersing the NG-HDO film obtained in the step (3) in water, then adding silver nitrate, carrying out magnetic stirring, finally adding a sodium citrate solution, controlling the temperature at 90 ℃, and carrying out heat preservation for 30min until the solution becomes dark green, thus obtaining a dispersion liquid of the NG-HDO film with Ag nano particles modified on the surface;
(5) adding sodium molybdate and cysteine into the dispersion liquid of the NG-HDO film modified with the Ag nano particles on the surface obtained in the step (4), uniformly mixing, and reacting for 8-12h at the temperature of 180-; finally separating and purifying to obtain the MoS2The surface of the-Ag-nitrogen doped graphene nanocomposite is enhanced by Raman spectroscopy.
Wherein in the step (1), the concentration of the aminopyrene is 0.005mol/L, and the concentration of the sodium hydroxide is 0.05 mol/L; the temperature of the hydrothermal reaction was 180 ℃.
In the step (3), the concentration of a tetrahydrofuran solution of 2, 4-heptadecadiyne-1-ol (HDO) is 3g/L, and the mass ratio of the nitrogen-doped graphene film to the 2, 4-heptadecadiyne-1-ol is 20: 1; the ultraviolet irradiation time is 1h, and the ultraviolet wavelength is 365 nm.
Wherein, in the step (4), the concentration of the aqueous dispersion of the NG-HDO film is controlled to be 3wt%, and after silver nitrate is added, the concentration of the silver nitrate is controlled to be 20 wt%.
Wherein in the step (5), the mass ratio of the NG-HDO film to the sodium molybdate to the cysteine is controlled to be 1: 10: 10.
example 3
MoS2The preparation method of the-Ag-nitrogen doped graphene nanocomposite surface enhanced Raman substrate comprises the following steps:
(1) carrying out hydrothermal reaction on aminopyrene in a sodium hydroxide aqueous solution to obtain a nitrogen-doped graphene quantum dot solution;
(2) carrying out vacuum filtration on the nitrogen-doped graphene quantum dot solution obtained in the step (1), and carrying out self-assembly to obtain a nitrogen-doped graphene thin film (NG) with a self-supporting structure;
(3) soaking the nitrogen-doped graphene film NG obtained in the step (2) in a tetrahydrofuran solution of 2, 4-heptadecadiyne-1-ol (HDO) for esterification, and then performing addition polymerization reaction by ultraviolet irradiation to obtain an NG-HDO film;
(4) ultrasonically dispersing the NG-HDO film obtained in the step (3) in water, then adding silver nitrate, carrying out magnetic stirring, finally adding a sodium citrate solution, controlling the temperature at 85 ℃, and carrying out heat preservation for 30min until the solution becomes dark green, thus obtaining a dispersion liquid of the NG-HDO film with Ag nano particles modified on the surface;
(5) adding sodium molybdate and cysteine into the dispersion liquid of the NG-HDO film modified with the Ag nano particles on the surface obtained in the step (4), uniformly mixing, and reacting for 8-12h at the temperature of 180-; finally separating and purifying to obtain the MoS2The surface of the-Ag-nitrogen doped graphene nanocomposite is enhanced by Raman spectroscopy.
Wherein in the step (1), the concentration of the aminopyrene is 0.02mol/L, and the concentration of the sodium hydroxide is 0.5 mol/L; the temperature of the hydrothermal reaction was 200 ℃.
In the step (3), the concentration of the tetrahydrofuran solution of 2, 4-heptadecadiyne-1-ol (HDO) is 5g/L, and the mass ratio of the nitrogen-doped graphene film to the 2, 4-heptadecadiyne-1-ol is 10: 1; the ultraviolet irradiation time is 3h, and the ultraviolet wavelength is 365 nm.
Wherein, in the step (4), the concentration of the aqueous dispersion of the NG-HDO film is controlled to be 1wt%, and after silver nitrate is added, the concentration of the silver nitrate is controlled to be 20 wt%.
Wherein in the step (5), the mass ratio of the NG-HDO film to the sodium molybdate to the cysteine is controlled to be 1: 15: 15.
Claims (6)
1. MoS2The preparation method of the-Ag-nitrogen doped graphene nanocomposite surface enhanced Raman substrate comprises the following steps:
(1) carrying out hydrothermal reaction on aminopyrene in a sodium hydroxide aqueous solution to obtain a nitrogen-doped graphene quantum dot solution;
(2) carrying out vacuum filtration on the nitrogen-doped graphene quantum dot solution obtained in the step (1), and carrying out self-assembly to obtain a nitrogen-doped graphene thin film (NG) with a self-supporting structure;
(3) soaking the nitrogen-doped graphene film NG obtained in the step (2) in a tetrahydrofuran solution of 2, 4-heptadecadiyne-1-ol (HDO) for esterification, and then performing addition polymerization reaction by ultraviolet irradiation to obtain an NG-HDO film;
(4) ultrasonically dispersing the NG-HDO film obtained in the step (3) in water, then adding silver nitrate, performing magnetic stirring, finally adding a sodium citrate solution, controlling the temperature to be 80-90 ℃, and preserving the heat for 30min until the solution becomes dark green, so as to obtain a dispersion liquid of the NG-HDO film with Ag nano particles modified on the surface;
(5) adding sodium molybdate and cysteine into the dispersion liquid of the NG-HDO film modified with the Ag nano particles on the surface obtained in the step (4), uniformly mixing, and reacting for 8-12h at the temperature of 180-; finally separating and purifying to obtain the MoS2The surface of the-Ag-nitrogen doped graphene nanocomposite is enhanced by Raman spectroscopy.
2. A MoS according to claim 12The preparation method of the-Ag-nitrogen doped graphene nano composite material surface enhanced Raman substrate is characterized in that in the step (1), the concentration of aminopyrene is 0.002-0.02mol/L, and the concentration of sodium hydroxide is 0.05-0.5 mol/L; the temperature of the hydrothermal reaction is 150-200-°C。
3. A MoS according to claim 12The preparation method of the-Ag-nitrogen-doped graphene nanocomposite surface enhanced Raman substrate is characterized in that in the step (3), the concentration of a tetrahydrofuran solution of 2, 4-heptadecadiyne-1-ol (HDO) is 3-5g/L, and the mass ratio of the nitrogen-doped graphene film to the 2, 4-heptadecadiyne-1-ol is 10-20: 1; the ultraviolet irradiation time is 1-3h, and the ultraviolet wavelength is 365 nm.
4. A MoS according to claim 12The preparation method of the-Ag-nitrogen doped graphene nano composite material surface enhanced Raman substrate is characterized in that in the step (4), the concentration of the aqueous dispersion of the NG-HDO film is controlled to be 1-3wt%, and after silver nitrate is added, the concentration of the silver nitrate is controlled to be 10-20 wt%.
5. A MoS according to claim 12The preparation method of the-Ag-nitrogen doped graphene nanocomposite surface enhanced Raman substrate is characterized in that in the step (5), the mass ratio of the NG-HDO film to the sodium molybdate to the cysteine is controlled to be 1: (10-15): (10-15).
6. A MoS according to any of claims 1 to 52The MoS 2-Ag-nitrogen-doped graphene nanocomposite surface enhanced Raman substrate prepared by the preparation method of the-Ag-nitrogen-doped graphene nanocomposite surface enhanced Raman substrate.
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