CN111592043A - Synthesis method and application of molybdenum trioxide quantum dots - Google Patents

Synthesis method and application of molybdenum trioxide quantum dots Download PDF

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CN111592043A
CN111592043A CN202010359229.XA CN202010359229A CN111592043A CN 111592043 A CN111592043 A CN 111592043A CN 202010359229 A CN202010359229 A CN 202010359229A CN 111592043 A CN111592043 A CN 111592043A
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quantum dots
concentration
molybdenum trioxide
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molybdenum
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CN111592043B (en
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陈晓勇
张泽宇
洪应平
梁庭
贾平岗
雷程
李晨
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North University of China
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    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/02—Oxides; Hydroxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
    • C09K11/68—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals containing chromium, molybdenum or tungsten
    • C09K11/681—Chalcogenides
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/6402—Atomic fluorescence; Laser induced fluorescence
    • C—CHEMISTRY; METALLURGY
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    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Abstract

The invention relates to a synthesis method and application of molybdenum trioxide quantum dots, wherein the synthesis method comprises the steps of S1, dissolving potassium permanganate in water, and adjusting the pH value to acidity; s2, adding molybdenum disulfide into the solution obtained in the step S1, and heating in a water bath until the reaction is completed; s3, centrifuging the solution obtained in the step S2, taking supernate, adding absolute ethyl alcohol and hydrogen peroxide solution into the supernate, and carrying out hydrothermal reaction in a reaction kettle to obtain the molybdenum trioxide quantum dots. Application of molybdenum trioxide quantum dots to Cr2O7 2‑Detection of (3). The synthesis method of the invention does not use a surfactant, andthe valence of molybdenum in the prepared quantum dots is high, so that the prepared quantum yield is high, and the synthesized MoO3Quantum dots can be used for Cr2O7 2‑Rapid and highly sensitive detection of Cr2O7 2‑The detection limit width of the probe is 0-3 mu mol/L, and the detection limit can reach 59 nmol/L.

Description

Synthesis method and application of molybdenum trioxide quantum dots
Technical Field
The invention relates to molybdenum trioxide quantum dots (MoO)3QDs) and application thereof, belonging to the technical field of material preparation.
Background
As an excellent semiconductor nanomaterial, the molybdenum oxide nanomaterial is widely applied to various aspects such as catalysts, gas sensing, solar electromagnetic, photochromic, lithium ion batteries, thin film and container, field effect transistors, antibacterial and anticancer effects, and the like due to good optical properties and good biocompatibility. Molybdenum oxide quantum dots (MoO) as reported by xiao et alxQDs) and their use in captopril, Pi, TNT and Hg+The high sensitivity detection shows that MoO isxQDs have great advantages in detection.
In recent years, people are dedicated to developing different synthetic methods to prepare molybdenum oxide nano materials with different morphologies because the physical and chemical properties of the molybdenum oxide nano materials are closely related to the morphologies of the molybdenum oxide nano materials. Existing MoOxThe preparation method mainly comprises a hydrothermal method: the method comprises the steps of carrying out chemical reaction in a sealed pressure vessel by using water as a solvent under the conditions of high temperature and high pressure, wherein the solubility of a compound in water is greater than that of a corresponding oxide in water, so that the compound is dissolved in water to precipitate the oxide, and the compound is synthesized MoO3A nanoribbon. An oxidation method: for example, 10.4mmol/L molybdenum powder is dissolved in 22mLH2O2Cooling to 0 deg.C in mixed solution of molybdenum trioxide and distilled water, adding 2mL of acetic acid dropwise under stirring, removing solvent under vacuum condition, cleaning, drying, and heating for 30min to obtain molybdenum trioxide nanoparticles (MoO)3NPs). Stripping method: usually in MoO3Is a source of Mo, and is a molybdenum source,adding surfactant to perform intercalation stripping. A photoetching method: by ultraviolet light on MoO3Further etching of the nanoparticles to form quantum dots. However, the method is limited, so that the prepared quantum yield is low, the surfactant is difficult to remove, and the like, and the new MoO is calledxQuantum dot preparation means. While the existing MoOxThe work of quantum dots in the aspect of detection mostly focuses on detection of Pi and drug and biosensing, the sample is insufficient, and obviously, the application of the quantum dots still needs to be further expanded and innovated, so that a novel preparation technology is provided, and the quantum dots are applied to Cr for the first time2O7 2-Detection of (3).
Disclosure of Invention
Technical problem to be solved
In order to solve the technical problems that the quantum yield is low, a surfactant is difficult to remove and the like in the prior art, the invention provides a method for synthesizing molybdenum trioxide quantum dots, and provides a novel application of the molybdenum trioxide quantum dots.
(II) technical scheme
In order to achieve the purpose, the invention adopts the main technical scheme that:
a method for synthesizing molybdenum trioxide quantum dots comprises the following steps:
s1, dissolving potassium permanganate in water, and adjusting the pH value to acidity by using acid;
s2, adding molybdenum disulfide into the solution obtained in the step S1, and heating in a water bath until the reaction is completed;
s3, centrifuging the solution obtained in the step S2, taking supernate, adding absolute ethyl alcohol and hydrogen peroxide solution into the supernate, and carrying out hydrothermal reaction in a reaction kettle to obtain the molybdenum trioxide quantum dots.
In a preferred embodiment, in step S1, the adjusting with acid is with sulfuric acid, and the pH value is 1-2.
In a preferred embodiment, in the step S1, the concentration of the potassium permanganate is 1-9 g/L.
In a preferred embodiment, in step S2, the molybdenum disulfide is added in an amount of 50% to 100% by mass of potassium permanganate.
In a preferred embodiment, in step S2, the temperature of the water bath heating is 25 ℃ or room temperature.
In a preferred embodiment, in step S3, the centrifugation is performed at a rate of 8000 Xg for a period of 10min to 30 min.
In a preferred embodiment, in step S3, the volume ratio of the supernatant to the absolute ethanol and hydrogen peroxide solution is ethanol: hydrogen peroxide: adding the supernatant in a ratio of 5:3:2, wherein the concentration of the hydrogen peroxide solution is 30%, the temperature of the reaction kettle is 180-200 ℃, and the hydrothermal reaction time is 8-10 h
The molybdenum trioxide quantum dots synthesized by the method have the average particle size of 5.25nm and the average height of 5.5 nm; the lattice spacing of the quantum dots is 0.26 nm.
Molybdenum trioxide quantum dots or molybdenum trioxide quantum dots synthesized by adopting method and used for Cr2O7 2-Application in concentration detection.
The application is preferably that the molybdenum trioxide quantum dots are used for Cr2O7 2-The concentration detection method comprises the following steps: dissolving molybdenum trioxide quantum dots by adopting absolute ethyl alcohol, and respectively adding Cr with different known concentrations2O7 2-Measuring the fluorescence intensity emitted at 440nm of the standard solution under the excitation wavelength of 370nm as a standard solution, wherein the range of different concentrations is 0-3 mu mol/L; when Cr is present2O7 2-At a concentration of 0, the fluorescence intensity measured is designated I0；Cr2O7 2-At different concentrations, the measured fluorescence intensity was recorded as I and calculated (I)0-I)/I0A value of (b), will know Cr2O7 2-Is the abscissa, and is calculated corresponding to I (I)0-I)/I0The value of (d) is taken as the ordinate, and a standard curve is drawn; for the measured fluorescence intensity of the sample to be measured, finding out the point corresponding to the fluorescence intensity corresponding to the standard curve to obtain the Cr of the sample2O7 2-Concentration of (2)。
The inventor verifies through a large number of experiments that Cr is adopted2O7 2-The standard solution has a good linear relation between 0 and 3 mu mol/L and can be used for drawing a standard curve, so that Cr2O7 2-The concentration of the standard curve is preferably 0 to 3. mu. mol/L.
In the application, the concentration of the molybdenum trioxide quantum dots is preferably 0.0002-0.4 mol/L; the known different concentrations of Cr2O7 2-The standard solution is preferably a standard solution whose concentration is increased by 2 to 4 times based on 0.0005 to 0.15. mu. mol/L.
(III) advantageous effects
The invention has the beneficial effects that:
the invention provides a novel MoO3The method for synthesizing the quantum dots synthesizes the high-fluorescence MoO by using industrial molybdenum disulfide as a precursor, potassium permanganate as an oxidant and hydrogen peroxide as a stripping agent3Quantum dots, characterized by AFM, TEM, XPS, fluorescence spectroscopy.
The synthetic method does not use a surfactant, the valence state of molybdenum in the synthesized quantum dots is high, the yield of the prepared quantum is high, and the synthesized MoO3Quantum dots can be used for Cr2O7 2-Rapid and highly sensitive detection of Cr2O7 2-The detection limit width of the probe is 0-3 mu mol/L, and the detection limit can reach 59 nmol/L. The absolute quantum yield of the quantum dots prepared by the method can reach 24.5 percent, the quantum dots are blue fluorescence under a 365nm ultraviolet lamp, and the research on the prepared quantum dots shows that MoO3The strong fluorescence emitted at 440nm of QDs excited at 370nm can follow Cr2O7 2-The increase in concentration occurs as effective quenching occurs when Cr2O7 2-When the concentration reaches 3 mu mol/L, the quenching degree can reach 95 percent, and a fluorescent sensor can be constructed based on the quenching degree and used for Cr2O7 2-The sensor has good selectivity and interference resistance, and can be used for Cr2O7 2-Fast and high sensitivity ofDetection of (3).
Drawings
FIG. 1 is a radio-microscopic image (TEM) of the product prepared in example 1;
FIG. 2 is a MoO prepared in example 13QDSTest results of Atomic Force Microscopy (AFM);
FIG. 3 is a MoO prepared in example 13Photographs in 3D mode under QDs atomic force microscope;
FIG. 4 is a MoO prepared in example 13Particle size distribution under QDS atomic force microscope;
FIG. 5 shows MoO3XPS test results of QDS, full spectrum data;
FIG. 6 is 3d orbit spectroscopy data for Mo;
FIG. 7 is the spectral data of the 2p track of S;
FIG. 8 shows MoO3Ultraviolet absorption spectra and fluorescence spectra of QDs;
FIG. 9 shows the following Cr2O7 2-Increased concentration of MoO3Changes in QDs fluorescence spectra;
FIG. 10 shows the sum of the concentrations of dichromate added (I)0-I)/I0A linear relationship.
Detailed Description
For the purpose of better explaining the present invention and to facilitate understanding, the present invention will be described in detail by way of specific embodiments with reference to the accompanying drawings.
Example 1
And (3) synthesis of quantum dots: accurately weighing 15mg of potassium permanganate, dissolving the potassium permanganate in 10mL of water, adjusting the pH value to 2 by using sulfuric acid, then adding 8mg of molybdenum disulfide, carrying out water bath at 25 ℃ for 10min, centrifuging at 8000 Xg for 10min, taking 2mL of supernate, adding 10mL of absolute ethyl alcohol and 3mL of 30% hydrogen peroxide, carrying out hydrothermal reaction at 180 ℃ in a reaction kettle for 10h to obtain a solution, dialyzing, freeze-drying and finally obtaining powder.
The dimensions and heights of the obtained products were measured using (JEM2100F) transmission electron microscope TEM and (Bruker dimension icon) atomic force microscope AFM, respectively. The elemental composition and the bonding structure of the compounds were characterized by x-ray photoelectron spectroscopy XPS (seemer fly Escalab250Xi), the absolute fluorescence quantum yield was determined by an (erburg FLS1000) fluorescence spectrometer, and the fluorescence spectrum and the ultraviolet absorption spectrum of the solution were recorded by fluorescence spectrometers F-7000 (japanese hitachi) and UV-2450 (japanese shimadzu).
The diameter of the prepared quantum dots is observed through a TEM, as shown in FIG. 1, the prepared quantum dots can be more obviously dispersed uniformly in the TEM, the particle size distribution diagram of the quantum dots is shown in the upper left corner of FIG. 1, the high-resolution transmission electron microscope (HTEM) diagram of the quantum dots is shown in the upper right corner of FIG. 1, the lattice spacing of the quantum dots is 0.26nm and is correspondingly (220) crystal face under the HTEM, meanwhile, statistical measurement is carried out on 200 dots in FIG. 1, the average particle size of the prepared quantum dots is finally obtained to be 5.25nm, and as shown in the AFM test shown in FIG. 2, the average height of the quantum dots is 5.0-5.5 nm. Fig. 3 shows a photograph of the quantum dots in a 3D mode of an atomic force microscope, which shows that the quantum dots are uniformly distributed and that the average particle size is 5.0 to 5.5nm, which is an auxiliary evidence for indicating the synthesis of the quantum dots, and fig. 4 shows a result of a particle size distribution test of the atomic force microscope, which shows that the particle size distribution of the quantum dots is uniform and that the particle size test shows that the synthesis is successful.
XPS technology is adopted to prepare MoO3The chemical states of Mo and S in QDs were investigated, and the results of full spectrum data are shown in FIG. 5, in which the peaks of Mo3d, Mn2p, O1S, S2p were all clearly observed, in high-resolution spectrograms, the 3d orbital spectrograms of Mo are shown in FIG. 6, the 2p orbital spectrograms of S are shown in FIG. 7, and the characteristic peaks at 235.6ev and 232.8ev in Mo3d correspond to Mo, respectively6+3d3/2And 3d5/2The oxidation of Mo element, compared with MoS, is demonstrated2Powder, MoO prepared3The S2S peak in QDs disappeared, the binding energy of S2p increased, 169.3ev and 170.1ev demonstrated the existence of the S element, corresponding to SO4 2-The existence form of the element S in the formula indicates MODisappearance of the-S bond, thus illustrating the MoO prepared according to the invention3Mo in QDs is +6 valence and is high valence MoO3The quantum dot of (1).
Example 2
Working examples1 MoO prepared3And the quantum dots are diluted by absolute ethyl alcohol so that the concentration of the quantum dots is 0.35 mmol/L. The UV absorption spectrum and the fluorescence spectrum of the solution were recorded using a UV absorption spectrometer and an F-7000 fluorescence spectrometer under 370nm as excitation light source.
Obtained MoO3The ultraviolet absorption spectrum and fluorescence spectrum of QDs are shown in FIG. 8, and MoO is shown at the upper left corner of FIG. 83The QDs is a photograph under visible light, wherein the ultraviolet absorption spectrum is measured by an ultraviolet absorption spectrometer, the fluorescence spectrum is measured by an instrument, the position and intensity of the emitted wavelength can be changed under the excitation of different wavelengths, the excitation wavelength with the strongest emission intensity is generally selected for excitation, the solution to be measured is excited at the wavelength, the emission spectrum (red line) is obtained, and the position of the peak of the spectrum with the strongest emission is taken as the wavelength for measurement, and the excitation spectrum (blue line) is obtained. The results show that the prepared quantum dots have weak absorption near 260nm in ultraviolet absorption spectrum, and the prepared quantum dots are tested for fluorescence spectrum, so that the prepared quantum dots have the wavelength of 371nm in λ ex and 441nm in λ em, and show that the prepared quantum dots have the wavelength of 371nm in excitation light and 441nm in emission light. Prepared MoO3QDs are pale yellow under visible light, and quantum dots fluoresce blue under a 365nm ultraviolet lamp, and the absolute quantum yield is measured to be 24.5%.
The MoO to be obtained3QDs adopts ethanol solution to prepare 0.35mmol/L, adds 3mL into the cuvette, measures the fluorescence emission spectrum at excitation light wavelength 370nm, i.e. the concentration of dichromate ion is 0, then adds 10 μ L of dichromate solution with concentration of 0.03 μmol/L into the cuvette, measures the fluorescence emission spectrum after mixing, and similarly, measures MoO with concentration of 0.35mmol/L3Adding 0.06 mu mol/L dichromate solution 10 mu L into a 3mL cuvette of QDs solution, uniformly mixing, measuring the fluorescence emission spectrum of the solution, gradually increasing the concentration of the dichromate solution to 3 mu mol/L, measuring the fluorescence emission spectrum of the solution, drawing a fluorescence curve spectrum as shown in figure 9, wherein MoO is3The strong fluorescence emitted at 440nm of QDs excited at 370nm can follow Cr2O7 2-An increase in concentration occurs with efficient quenching,and when Cr is present2O7 2-When the concentration reaches 3 mu mol/L, the quenching degree can reach 95 percent. The addition of the dichromate (standard solution) is shown to reduce the fluorescence intensity along with the increase of the addition amount of the dichromate, and the linear relation between the solution fluorescence intensity and the concentration appears, which shows that the solution can be added with Cr according to the condition that the solution fluorescence intensity is at the highest peak, namely 440nm2O7 2-The concentration of the fluorescent substance is in a linear relation, the fluorescent substance is used for detecting the solution with unknown concentration after a standard curve is drawn, and the corresponding concentration is found from the standard curve by measuring the value of the fluorescence intensity at 440nm after the unknown solution is added, so that the detection aim is fulfilled.
Example 3
MoO prepared in example 13Diluting the quantum dot with anhydrous ethanol to concentration of 0.35mmol/L, adding 3mL into a cuvette, and recording the measured peak value emitted at 440nm, i.e. fluorescence intensity, as I under excitation wavelength of 370nm0Adding 10 microliter of dichromate standard solution with the concentration of 0.13 mu mol/L into the cuvette, measuring the fluorescence intensity of the solution as I, recording the spectrum, adding 3mL of MoO with the concentration of 0.35mmol/L into a new cuvette, and adding MoO with the concentration of 3mL and the concentration of 0.13 mu mol/L into the cuvette3Adding 10 microliter of dichromate standard solution with the concentration of 0.26 mu mol/L into the quantum dot solution, measuring the fluorescence intensity once again, and calculating according to the fluorescence intensity measured by adding dichromate standard solution with the concentration of 2 times to 3 mu mol/L (I)0-I)/I0The values of (A) are plotted as ordinate and concentration of dichromate radical as abscissa, and a standard curve is plotted. As shown in FIG. 10, when Cr is present2O7 2-At a concentration of 0-0.15. mu. mol/L, MoO3Fluorescence recovery factor (I) of QDs0-I/I0) And Cr2O7 2-Has a good linear relation with the concentration of (A), and the linear equation is that y is 0.0173x-0.0048 (R)20.9979, n 11), for Cr2O7 2-The detection limit of (2) is as low as 59nmol/L (3 sigma/K) (sigma is the standard deviation after correcting blank signal, K is the slope of fitted line) and is used to detect solution with unknown concentration, and MoO is taken3Diluting the quantum dots with absolute ethyl alcohol to make the concentration of the quantum dots be 0.35mmol/L, taking 3mL of the quantum dots, adding the quantum dots into a cuvette, adding 10 microliters of solution to be detected, and performing excitation at an excitation wavelengthAt 370nm, measuring the fluorescence intensity emitted at 440nm, corresponding to the standard curve, and finding out the corresponding concentration according to the corresponding fluorescence intensity on the curve of the fluorescence intensity and the concentration to obtain the Cr in the solution to be measured2O7 2-The concentration of (c).
Example 4 detection of a simulated sample
The simulation was supplemented with a concentration of 0.2. mu. mol/LK2Cr2O7The aqueous solution of (1) was used as a solution to be measured, a standard curve was prepared according to the method of example 3, and then the concentration was taken as 0.35mmol/LMoO3Adding 3ml of quantum dot ethanol solution into a cuvette, adding 10 microliters of solution to be detected, measuring the fluorescence intensity emitted at 440nm under the excitation wavelength of 370nm, and corresponding to a standard curve to obtain Cr in the solution to be detected2O7 2-The concentration of (A) is 0.205 mu mol, which indicates that the measurement error is less than 5 percent, and indicates that the detection result is reliable and credible.
Example 5 interference test
The present embodiment will not affect the MoO under the condition of detecting the existence of other ions3Quantum dot for Cr2O7 2-The specific interfering ion is Cd2+，Na+，Cu2+，Zn2+，Mg2+，Hg+，Ni2+，K+，Mn2+，Cl-，NO3 -，SO4 2-，F-The addition amount is 50 mu mol, and the detection result shows that the solution added with the interfering ions and the solution not added with the interfering ions have no change on the fluorescence intensity, and shows that MoO3Fluorescence intensity of Quantum dots for Cr2O7 2-There is a response, no response to other ions, indicating MoO3Quantum dots can be used for Cr only2O7 2-Accuracy of concentration detection.
Comparative example
MoO prepared by the prior art3QDs method, 1g MoO3Adding 40ml of dimethyl sulfoxide into the powder, and ultrasonically intercalating and stripping for more than 4 hours to prepare the quantum yield of 15%. Can be used forThe method has high quantum yield.
The invention prepares MoO by combining an oxidation method and a stripping method3QDs, the prepared quantum dots have high fluorescence quantum yield (24.5%), emit blue fluorescence at 365nm and realize the first Cr pair2O7 2-Detection of, MoO3Fluorescence recovery factor (I) of QDs0-I/I0) And Cr2O7 2-Has a good linear relation with the concentration of (A), and the linear equation is that y is 0.0173x-0.0048 (R)20.9979, n 11), for Cr2O7 2-The detection limit of (2) is as low as 59nmol/L (3. sigma./K).
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in other forms, and any person skilled in the art can change or modify the technical content disclosed above into an equivalent embodiment with equivalent changes. 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 method for synthesizing molybdenum trioxide quantum dots is characterized by comprising the following steps:
s1, dissolving potassium permanganate in water, and adjusting the pH value to acidity by using acid;
s2, adding molybdenum disulfide into the solution obtained in the step S1, and heating in a water bath until the reaction is completed;
s3, centrifuging the solution obtained in the step S2, taking supernate, adding absolute ethyl alcohol and hydrogen peroxide solution into the supernate, and carrying out hydrothermal reaction in a reaction kettle to obtain the molybdenum trioxide quantum dots.
2. The method of claim 1, wherein in step S1, sulfuric acid is used for the adjustment, and the pH value is 1-2.
3. The synthesis method according to claim 1, wherein in step S1, the concentration of potassium permanganate is 1-9 g/L.
4. The synthesis method according to claim 1, wherein in step S2, the added amount of molybdenum disulfide is 50-100% of the mass of potassium permanganate.
5. The method of synthesis of claim 1, wherein in step S2, the water bath heating is at 25 ℃ or room temperature.
6. The method of synthesis according to claim 1, wherein in step S3, the centrifugation is performed at 8000 xg for 10-30 min.
7. The method of synthesis of claim 1, wherein in step S3, the supernatant is mixed with a solution of anhydrous ethanol and hydrogen peroxide in a ratio of ethanol: hydrogen peroxide: adding the supernatant at a ratio of 5:3:2, wherein the concentration of the hydrogen peroxide is 30%; the constant temperature of the reaction kettle is 180-200 ℃, and the hydrothermal reaction time is 8-10 h.
8. Application of molybdenum trioxide quantum dots or molybdenum trioxide quantum dots synthesized by adopting method of any one of claims 1 to 7 in Cr2O7 2-Application in concentration or content detection.
9. The use of claim 9, wherein the molybdenum trioxide quantum dots are used in Cr2O7 2-The concentration detection method comprises the following steps: dissolving molybdenum trioxide quantum dots by adopting absolute ethyl alcohol, and respectively adding Cr with different known concentrations2O7 2-As a standard solution, wherein the fluorescence intensity emitted by the standard solution at 440nm is measured when the excitation wavelength of the standard solution is 370nm and the concentration of Cr is 0-3 mu mol/L2O7 2-The fluorescence intensity measured at a concentration of 0 is recorded as I0，Cr2O7 2-For recording fluorescence intensity measured at different concentrationsFor I, calculate (I)0-I)/I0A value of (d); known Cr2O7 2-Is the abscissa, and is calculated corresponding to I (I)0-I)/I0The value of (d) is taken as the ordinate, and a standard curve is drawn; for the measured fluorescence intensity of the sample to be measured, finding out the point corresponding to the fluorescence intensity corresponding to the standard curve to obtain the Cr of the sample2O7 2-The concentration of (c).
10. The method of claim 9 for Cr2O7 2-The application of the molybdenum trioxide quantum dots in concentration or content detection is characterized in that the concentration of the molybdenum trioxide quantum dots is 0.0002-0.4 mol/L, and Cr with different known concentrations is2O7 2-The standard solution is a standard solution with concentration increased by 2-4 times based on 0.0005-0.15 mu mol/L.
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