CN109294577B - NaYF4Eu @ CDs composite material and preparation method and application thereof - Google Patents
NaYF4Eu @ CDs composite material and preparation method and application thereof Download PDFInfo
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
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- 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
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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- G—PHYSICS
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- 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
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6432—Quenching
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- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
Abstract
The invention belongs to the technical field of materials, and discloses NaYF4Eu @ CDs composite material and preparation method and application thereof. Firstly synthesizing NaYF4Eu, CDs solution and silicon dioxide sol, mixing the three solutions, mechanically stirring to generate composite material solution, drying and grinding to generate NaYF4Eu @ CDs composite particles. By adjusting NaYF4Eu, CDs and silica sol can change the color of light emitted under 395nm excitation from blue light to white light to red light, and effectively realize the regulation and control of the color of light emission. The invention mainly utilizes the regulation of the ratio of the red light to the blue light to realize the regulation of the emission spectrum. The preparation method provided by the invention has the advantages of simple process, easiness in operation, low cost and environmental friendliness, and the obtained composite material particles have good stability. The composite material can meet the application requirements in different fields of ion detection, white light LED lamps and the like.
Description
Technical Field
The invention belongs to the field of materials, and particularly relates to NaYF4Eu @ CDs composite material and preparation method and application thereof.
Background
Multicolor luminescent materials are attracting increasing attention due to their potential applications in flexible full-color displays, a variety of biomarkers and next generation light sources. It would be highly advantageous to be able to obtain color modulation from the same luminescent composition under single wavelength excitation. In recent years, many multicolor luminescent materials have been developed, including rare earth metal-based nanoparticles, semiconductor Quantum Dot (QD) polymer dots, molecular nanomaterials, and organic fluorescent dyes. However, the practical application of these materials is hampered by low emission Quantum Yields (QYs), poor water solubility, the possibility of photobleaching and complex preparation procedures. Thus, it has been found that environmentally friendly and low toxicity materials suitable for use in multicolor light emitting devices remain challenging.
Rare earth ion doped inorganic Nanocrystals (NCs) have potential applications in many modern optoelectronic devices. NaYF4Nanocrystals have attracted much attention in the past few years as host matrices for luminescent Rare Earth (RE) ions, and their use continues to expand. Active research on lanthanide doped nano-phosphors began more than a decade ago. Since then, significant progress has been made in the preparation and understanding of the relationship between their luminescent properties and the resulting morphology. Recently, NaYF has been used4Co-doping of the host with ions was investigated as the host matrix. The main argument is that the rare earth is doped with NaYF4The nanocrystal has an ultraviolet and infrared narrow emission band (<10nm), spectral range, large stokes shift, long emission decay time (mus or ms), weak bleaching, no flicker, etc. Lower toxicity compared to II-VI Nanocrystals (NCs) such as CdS and CdSe. At the same time, they can also exhibit magnetic properties and can be used for multifunctional probes. All of these factors have a large impact on their potential applications.
Carbon Dots (CDs), comprising a class of attractive fluorescent-based nanoparticles, are characterized by their excellent properties, such as high biocompatibility, low cytotoxicity, chemical inertness and attractive Photoluminescence (PL) properties. It is considered to be an outstanding alternative to traditional metal quantum dots. They exhibit strong absorption and efficient blue emission in the near ultraviolet spectral region, which makes them suitable as blue-emitting components for multicolor emission. However, achieving efficient solid state light emitting materials remains a challenge because of PL annihilation of the solid state matrix solution for light sources transferred from its parent colloid. This is mainly caused by the aggregation of CD. Therefore, further discovery of the synthesis of solid-state luminescent carbon dots is needed.
Disclosure of Invention
In order to overcome the disadvantages and shortcomings of the prior art, the invention provides a NaYF4A preparation method of the Eu @ CDs composite material.
The invention also aims to provide NaYF prepared by the preparation method4Eu @ CDs composite material.
Still another objective of the present invention is to provide a NaYF structure as mentioned above4Application of Eu @ CDs composite material. The method is used for realizing the regulation and control of the emission spectrum and realizing the change from blue light to white light to red light under a single excitation wavelength.
The purpose of the invention is realized by the following technical scheme:
NaYF4The preparation method of the Eu @ CDs composite material comprises the step of firstly synthesizing NaYF4Eu nano particles, CDs solution and silicon dioxide sol are mixed and stirred, and then the composite material is obtained through drying and grinding.
The NaYF4The preparation method of the Eu @ CDs composite material specifically comprises the following steps:
(1)NaYF4preparing Eu nano particles: adding 1.538mmol of sodium chloride into a beaker filled with 30mL of ethylene glycol, uniformly stirring, adding 0.4-0.6 mL of Polyethyleneimine (PEI) into the mixed solution, stirring for 30 minutes, then adding 1mmol of rare earth ion solution, stirring until the solution is clear, adding 4mmol of ammonium fluoride, and stirring for 10 minutes; transferring the obtained solution into a high-pressure autoclave, placing the high-pressure autoclave in an oven to be heated and reacted for 12 hours at the temperature of 200 ℃, naturally cooling the high-pressure autoclave to room temperature after the reaction is finished, centrifugally separating a sample, washing the sample for 3 times by using water and ethanol, and then freeze-drying the sample to obtain NaYF4Eu nanoparticles; the rare earth ion solution comprises 95 mass percent of Y3+And 5% by mass of Eu3+；
(2) Synthesis of CDs: placing 10mL of the organosilane compound, 0.4g of anhydrous citric acid, and 10mL of water in a beaker and stirring for 15 minutes; the mixture solution was transferred to a 50mL teflon-lined stainless steel autoclave and heated at 180 ℃ for 12 hours; after the reaction, the mixture was cooled to room temperature; extracting and purifying with ethyl acetate and petroleum ether to obtain light brown solution, and performing rotary evaporation on the obtained solution to obtain CDs;
(3)NaYF4preparing a Eu @ CDs composite material: TEOS, EtOH, hydrochloric acid with pH 2 and H2O is added into the mixture in a molar ratio of 1: 4: 0.2: 5 mixing to prepare silicon dioxide sol; NaYF is added4Adding Eu nano particles into 4mL of silicon dioxide sol, pouring CDs solution into the Eu nano particles, and keeping stirring the obtained mixture system until uniform gel is formed; vacuum drying the derivatized gel at 80 deg.C for 12 hours, grinding the resulting dried material to form uniform particles to obtain NaYF4Eu @ CDs composite material.
The molecular weight of the polyethyleneimine in the step (1) is 25000; the autoclave is a polytetrafluoroethylene lining reaction kettle; the freeze drying is carried out at the temperature of-40 to-90 ℃ and under the air pressure of 8 to 20 Pa.
The organosilane compound in the step (2) is 3- (2-aminoethylamino) propyltrimethoxysilane (AEAPMS), allyltrimethylsilane or trialkoxysilane.
The CDs solution in the step (3) is ethanol solution of CDs.
NaYF prepared by the preparation method4Eu @ CDs composite material.
NaYF as described above4Application of Eu @ CDs composite material in ion detection, wherein the ion detection refers to Fe3+And (6) detecting.
NaYF as described above4Application of the Eu @ CDs composite material in preparation of white light LEDs.
The preparation of the white light LED is to obtain epoxy resin and NaYF through mechanical stirring4A mixture of Eu @ CDs composites, then the mixture was integrated on a UV-LED chip under 395nm excitation and a white LED was obtained by drying at 60 ℃ for 4 hours; the white light LED obtains the light emission of the white light color development LED under the voltage of 3.2V and the test current of 300 mA.
The invention synthesizesA state luminous blue soluble carbon dot which is grafted to NaYF by a simple sol-gel method4: eu matrix. Hydrolysis and condensation reactions of silica precursors can combine CD with highly soft impurities. NaYF4: eu @ CDs is used in silica gel networks for the production of multicolor phosphors. By modulating CDs/NaYF4: eu and by adjusting the excitation wavelength, the color emission can systematically go from blue to white to red. The fluorescence ratio method is more robust and convenient for practical applications than measurements based on single intensities. This is because the built-in calibration provided by the simultaneous detection of both signals under single wavelength excitation overcomes the inaccuracy of probe concentration and the small variations of the optoelectronic system. Fe3+Quenching effect on carbon dots enables NaYF4The luminescence properties of the Eu @ CDs complexes are suitable as Fe3+The fluorescence ratio sensor has a sensing range of 0-350 mu M.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the invention adopts silica sol as a composite material substrate to connect NaYF4Eu and CDs, and the method is green and environment-friendly.
(2) The composite material prepared by the invention can effectively regulate and control the change of the luminescent color of the composite material at a single excitation wavelength, and has strong fluorescence and stability.
(3) The composite material of the invention has simple preparation process and realizes Fe3+The ratio fluorescence detection and the white light LED lamp assembly are simple in required instruments and equipment, easy to operate, low in production cost and wide in application range.
Drawings
FIG. 1 shows NaYF4Eu, CDs and NaYF4XRD pictures of Eu @ CDs.
FIG. 2 is a scanning electron microscope and transmission image of NaYF4 Eu, CDs and NaYF4 Eu @ CDs composite material, wherein a and b are NaYF4Eu and NaYF4Scanning electron microscope pictures of Eu @ CDs; c and d are transmission electron microscope pictures and high-resolution transmission electron microscope pictures of CDs; e and f are NaYF4Transmission electron microscopy pictures and magnified pictures of Eu @ CDs.
FIG. 3 is a fluorescence spectrum in which a is solidFluorescence spectra of state CDs under different excitations; b is a fluorescence spectrum of the CDs solution under different excitations; c is a histogram of the fluorescence intensity of different metal ions added into the CDs solution under 365nm excitation; d is Fe with different concentrations under 365nm excitation3+The fluorescence spectrum is added into the carbon dot solution, and the inset is a line graph.
FIG. 4 shows different concentrations of Fe under 395nm laser excitation3+In NaYF4I.e. the fluorescence spectrum in Eu @ CDs solution.
FIG. 5 shows binding of NaYF using 395nm chip4The luminous spectrum of a white LED lamp manufactured by Eu @ CDs nano composite material and the luminous effect graph of the manufactured LED lamp.
Detailed Description
The present invention is further illustrated by the following examples, which are provided only for illustrating the present invention, but the scope of the present invention is not limited thereto.
Example 1:
(1) adding 1.538mmol of sodium chloride into a beaker filled with 30mL of ethylene glycol, uniformly stirring, adding 0.4-0.6 mL of Polyethyleneimine (PEI) into the mixed solution, stirring for 30 minutes, then adding 1mmol of rare earth ion solution, stirring until the solution is clear, adding 4mmol of ammonium fluoride, and stirring for 10 minutes; transferring the obtained solution into a high-pressure autoclave, placing the high-pressure autoclave in an oven to be heated and reacted for 12 hours at the temperature of 200 ℃, naturally cooling the high-pressure autoclave to room temperature after the reaction is finished, centrifugally separating a sample, washing the sample for 3 times by using water and ethanol, and then freeze-drying the sample to obtain NaYF4Eu nano-particles, wherein the rare earth ion solution comprises 95 percent of Y by mass3+And 5% by mass of Eu3+。
(2) 10mL of AEAPMS, 0.4g of anhydrous citric acid and 10mL of water were placed in a beaker and stirred for 15 minutes, and the mixture solution was transferred to a 50mL Teflon-lined stainless steel autoclave and heated at 180 ℃ for 12 hours; after the reaction, the autoclaved mixture was cooled to room temperature, and the resulting light brown solution was purified by multiple extractions with ethyl acetate and petroleum ether; finally, the light brown solution was subjected to rotary evaporation to give CDs; and finally, dissolving the product in 20mL of ethanol to obtain a CDs solution.
(3)TEOS, EtOH, hydrochloric acid with pH 2 and H2O is added into the mixture in a molar ratio of 1: 4: 0.2: 5 mixing to prepare silicon dioxide sol; the NaYF obtained in the step (1) is treated4Adding Eu nano particles into 4mL of silicon dioxide sol, and pouring the CDs solution obtained in the step (2) into the Eu nano particles; the mixture system is kept stirring until a uniform gel is formed; drying the derivatized gel at 80 ℃ under vacuum for 12 hours; the final dried product was ground to uniform granules. Namely NaYF4Yb, Er @ CDs composite material.
FIG. 1 is a NaYF prepared in example 14Eu, CDs and NaYF4XRD pattern of Eu @ CDs particles from which NaYF can be seen4Eu is consistent with the peak position of the standard card, which shows that pure phase NaYF is obtained4Eu. While NaYF4Eu @ CDs showed the occurrence of 200 peaks, demonstrating the presence of carbon dot doping.
In FIG. 2, a is NaYF prepared in example 14Scanning electron microscope pictures of Eu particles, from which it can be seen that NaYF4Eu is spherical with a particle size of about 35 nm. B in FIG. 2 is NaYF prepared in example 14Scanning electron microscope picture of Eu @ CDs composite material, as can be seen from the figure, NaYF4Eu has different concave-convex particles on the surface, which indicates the generation of the composite material. In FIG. 2, c and d are high resolution transmission electron microscope images of carbon dots, and the average particle size of the carbon dots is about 2 nm. E and f in FIG. 2 are NaYF4Transmission electron microscopy and magnification of Eu @ CDs, it can be seen that carbon dots exist in NaYF4: eu surface.
In FIG. 3, a is the fluorescence spectrum of the solid CDs prepared in example 1 under different excitations, and the optimal emission of 453nm is achieved under 360nm excitation, b is the fluorescence spectrum of the CDs solution under different excitations, and the optimal emission of 454nm is achieved under 360nm excitation, and the carbon dots maintain the stable solid-state liquid state fluorescence optical phenomenon; c is a fluorescence intensity histogram when different metal ions are added into the CDs solution under 365nm excitation, Fe3+ generates an obvious quenching effect on carbon point luminescence, and simultaneously shows good selectivity; d is Fe with different concentrations under 365nm excitation3+The fluorescence spectrum is added into the carbon dot solution, the inset is a line graph, and the linear correlation index reaches 0.98.
Example 2:
NaYF obtained in example 1 was used4Carrying out metal ion detection on the Eu @ CDs composite material. First, we use various metal ion solutions, such as Ag+，Al3+，Ca2+，Cd2+，Cr2+，Cu2+， Fe2+，Fe3+，Hg2+，K+，Li+，Mg2+，Mn2+，Na+，Ni+，Zn2+. In the detection experiment, NaYF is added4Eu @ CDs nanocomposite is dispersed in an aqueous solution at a concentration of 10mg/mL, and a solution of various metal ions at a concentration of 400. mu.M is added to the solution. After uniform mixing, fluorescence measurements were performed with the same excitation. In further experiments, 10mg/mL NaYF was prepared4Eu @ CDs nanocomposite solution with addition of Fe at different concentrations3+(0. mu.M-350. mu.M). Fluorescence measurements were performed at 395nm excitation.
FIG. 4 shows different concentrations of Fe under 395nm laser excitation in this example3+In NaYF4I.e. the fluorescence spectrum in Eu @ CDs solution. The compound generates blue region emission and red region emission under 395nm excitation, and Fe3+The compound produces quenching effect on the blue light emitting part, and the red light part is not obviously changed, thereby achieving the purpose of ratio fluorescence detection and having obvious detection effect.
Example 3:
obtaining epoxy resin and NaYF through mechanical stirring4A mixture of Eu @ CDs composite. The mixture was then carefully integrated on UV-LED chips (395nm) and WLED was obtained by drying at 60 ℃ for 4 hours.
FIG. 5 shows the present example using 395nm chip combined with white light emitting NaYF4: emission spectra of white LED lamps made from Eu @ CDs nanocomposites. In addition to the 395nm emission of the chip, there are also blue 465nm, red 589nm, 615nm and 695nm emissions. As can be seen in the inset, the LED lamp exhibits a strong white light emission.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (6)
1. NaYF4Eu @ CDs composite in Fe3+Application in detection.
2. Use according to claim 1, characterized in that: the NaYF4The preparation method of the Eu @ CDs composite material comprises the steps of firstly synthesizing NaYF4Eu nano particles, CDs solution and silicon dioxide sol are mixed and stirred, and then the composite material is obtained through drying and grinding.
3. Use according to claim 1, characterized in that: the NaYF4The preparation method of the Eu @ CDs composite material specifically comprises the following steps:
(1)NaYF4preparing Eu nano particles: adding 1.538mmol of sodium chloride into a beaker filled with 30mL of ethylene glycol, uniformly stirring, adding 0.4-0.6 mL of polyethyleneimine into the mixed solution, stirring for 30 minutes, then adding 1mmol of rare earth ion solution, stirring until the solution is clear, adding 4mmol of ammonium fluoride, and stirring for 10 minutes; transferring the obtained solution into a high-pressure autoclave, placing the high-pressure autoclave in an oven to be heated and reacted for 12 hours at the temperature of 200 ℃, naturally cooling the high-pressure autoclave to room temperature after the reaction is finished, centrifugally separating a sample, washing the sample for 3 times by using water and ethanol, and then freeze-drying the sample to obtain NaYF4Eu nanoparticles; the rare earth ion solution comprises 95 mass percent of Y3+And 5% by mass of Eu3+；
(2) Synthesis of CDs: placing 10mL of the organosilane compound, 0.4g of anhydrous citric acid, and 10mL of water in a beaker and stirring for 15 minutes; the mixture solution was transferred to a 50mL teflon-lined stainless steel autoclave and heated at 180 ℃ for 12 hours; after the reaction, the mixture was cooled to room temperature; extracting and purifying with ethyl acetate and petroleum ether to obtain light brown solution, and performing rotary evaporation on the obtained solution to obtain CDs;
(3)NaYF4preparing a Eu @ CDs composite material: TEOS, EtOH, hydrochloric acid with pH 2 and H2O is added into the mixture in a molar ratio of 1: 4: 0.2: 5 mixing to prepare silicon dioxide sol; NaYF is added4Adding Eu nano particles into 4mL of silicon dioxide sol, pouring CDs solution into the Eu nano particles, and keeping stirring the obtained mixture system until uniform gel is formed; vacuum drying the derivatized gel at 80 deg.C for 12 hours, grinding the resulting dried material to form uniform particles to obtain NaYF4Eu @ CDs composite material.
4. Use according to claim 3, characterized in that: the molecular weight of the polyethyleneimine in the step (1) is 25000; the autoclave is a polytetrafluoroethylene lining reaction kettle; the freeze drying is carried out at the temperature of-40 to-90 ℃ and under the air pressure of 8 to 20 Pa.
5. Use according to claim 3, characterized in that: the organosilane compound in the step (2) is 3- (2-aminoethylamino) propyltrimethoxysilane, allyltrimethylsilane or trialkoxysilane.
6. Use according to claim 3, characterized in that: the CDs solution in the step (3) is ethanol solution of CDs.
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