CN110055070A - A kind of Ratio-type green emission fluorescent material - Google Patents
A kind of Ratio-type green emission fluorescent material Download PDFInfo
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- CN110055070A CN110055070A CN201910348977.5A CN201910348977A CN110055070A CN 110055070 A CN110055070 A CN 110055070A CN 201910348977 A CN201910348977 A CN 201910348977A CN 110055070 A CN110055070 A CN 110055070A
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- C—CHEMISTRY; METALLURGY
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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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
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7772—Halogenides
- C09K11/7773—Halogenides with alkali or alkaline earth metal
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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"
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- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
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- 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
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6432—Quenching
Abstract
The invention belongs to phosphor field more particularly to a kind of Ratio-type green emission fluorescent material and its as the application of Ratio-type fluorescent pH probe.A kind of Ratio-type green emission fluorescent material, the molecular formula of the basis material of the fluorescent material are Ce/Tb:NaLu0.2Gd0.8F4, the fluorescent material is under the conditions of ultraviolet light 254nm excitation wavelength, Ce3+Broadband emission, emission wavelength range 300-480nm, Tb is presented3+Most strong emission peak central wavelength be 550nm, integrally show stronger green emission；As pH increases to 10, Tb from 43+Ion and Ce3+Apparent variation occurs for the fluorescence intensity ratio of ion.The surface ligand protonation or deprotonation process and energy transmission that the present invention is responded by pH regulate and control, method to realize the detection of Ratio-type fluorescent pH, to obtain there is high light chemical stability, hypotoxicity and the highly sensitive inorganic fluorescent pH probe material of fast-response to provide new thinking, is expected to be widely used in pH detection field.
Description
Technical field
The invention belongs to phosphor field more particularly to a kind of Ratio-type green emission fluorescent material and its conducts
The application of Ratio-type fluorescent pH probe.
Background technique
Common pH detection method mainly has pH test paper and electrochemistry pH meter, and pH test paper is only applicable to rough measure, electrification
It is big to learn pH meter size, design is complicated, is only used for single-point detection, and may not apply to gadget and cellular environment detection.Base
Fast in the pH detection method response of fluorescence, spatial resolution is high, can telemeasurement, exploitation fluorescent pH probe material has important
Scientific research value and practical significance.Current fluorescent pH probe material mainly includes organic fluorescent dye, quantum dot and gold
Category-organic framework materials, they have the disadvantages that optical stability is poor, and detection range is small and toxicity is big etc..Compare and
Speech, active ions doping fluoride nano crystalline substance show broad band transmitting, high light chemical stability and low bio-toxicity, extensively
The general research using field of biomedicine.
Trivalent cerium ion (Ce3+) there is very strong 4f-5d transition characteristic, Ce3+The fluoride nano material of sensitization, which shines, imitates
Rate is high, Ce3+In ultra-violet (UV) band, there is also radiation transistions.Gd3+Ion and Ce3+Ion has very matched excited level, with Gd3+
Ion is that energy bridges center, can be further improved the fluorescence efficiency of active ions.Lemon acid surfaces contain three carboxyl light
It can roll into a ball, with the variation of pH, reversible protonation and deprotonation process can be showed.Therefore, we with citric acid be with
Body is prepared for uniform Ce using solvent-thermal method3+/Tb3+It is co-doped with NaLu0.2Gd0.8F4It is nanocrystalline, Ce3+Ultraviolet light is absorbed, is passed through
Gd3+Excitation energy is passed to active ions Tb3+, while obtaining efficient green emission, there is also Ce3+In long wave ultraviolet
The radiation transistion in area.As pH changes to 10, Tb from 43+The luminous intensity of ion gradually weakens, Ce3+The luminous intensity of ion is first
Increase after decrease, is detection signal with the fluorescence intensity ratio of Tb/Ce, Ratio-type fluorescence may be implemented in the range of pH is 4-10
PH detection.
Summary of the invention
It is an object of the present invention to provide a kind of Ratio-type green emission fluorescent material, the basis materials of the fluorescent material
Molecular formula be Ce/Tb:NaLu0.2Gd0.8F4, carboxyl functional group is had on the surface of basis material；The fluorescent material is ultraviolet
Under the conditions of light 254nm excitation wavelength, Ce3+Broadband emission, emission wavelength range 300-480nm, Tb is presented3+Most strong emission peak
Central wavelength is 550nm, integrally shows stronger green emission；As pH increases to 10, Tb from 43+Ion and Ce3+Ion
Fluorescence intensity ratio apparent variation occurs.
As a kind of specific embodiment, the carboxyl functional group provides for citric acid.
Another object of the present invention is to provide the preparation method of the fluorescent material, and this method includes step below
It is rapid:
1) by 0.3-0.78 mMs of gadolinium nitrate, 0.1-0.2 mMs of lutecium nitrate, 0.1-0.3 mMs of cerous nitrate, 0.02-
0.12 mM of terbium nitrate, 1-5 mMs of sodium chloride are added in 4-10 milliliters of H2O with 2-4 mMs of trisodium citrate, stir
It mixes 10-15 minutes and obtains clear solution A；
2) 20 milliliters of ethylene glycol are added in solution A, continue stirring 20-30 minutes；
3) 3-5 mMs of ammonium fluoride is added in the solution that step 2 obtains, continues stirring 30-60 minutes, obtains translucent cream
Turbid；
4) solution that step 3) obtains is transferred in 50 milliliters of pyroreaction kettles, is placed in blast heating case, in 100-180
DEG C reaction 5-12 hours, product is obtained after furnace cooling；
5) the product ethyl alcohol and deionized water centrifuge washing for obtaining step 4), dry 1-3 is small in vacuum freezing drying oven
When obtain final product.
The advantages of method of the invention is that simple, at low cost, yield is high, and products therefrom good dispersion, shape are uniform.
Another object of the present invention is to provide the fluorescent material for the application in the detection of Ratio-type fluorescent pH.
Another object of the present invention is to provide a kind of Ratio-type fluorescent pH probe, which includes the phosphor
Material.
Another object of the present invention is to provide a kind of Ratio-type fluorescent pH detection device, which includes described glimmering
Light pH probe.
Due to the adoption of the above technical solution, product of the present invention is the surface ligand proton based on pH response to the present invention
The Ratio-type nano fluorescent pH probe material of change/deprotonation and energy transmission regulation.It is characterized in that, in preparation process
In, using trisodium citrate as surface ligand, provide carboxyl functional group abundant；Pass through a small amount of Lu3+Ion doping guarantees the effect that shines
While rate, regulate and control nanocrystalline pattern, obtains uniformly monodispersed cluster type nanocrystalline material；As pH is gradually increased, table
Face citrate ligand deprotonation, Ce3+→Gd3+Energy transfer efficiency weaken, further suppress Tb3+Excited level
Electronics filling process, so that Tb3+The luminous intensity of ion gradually weakens, and Ce3+Ion then due to surface ligand electronegativity and
Increased trend after first weakening is presented in the variation of energy transfer efficiency；Tb3+With Ce3+Fluorescence intensity ratio with pH variation present
Apparent variation；Vice versa, this process is reversible change, can be applied to the detection of pH.Ratio-type detection method is not by outer
The interference of boundary's environment has very high accuracy.It is this by pH response surface ligand protonation or deprotonation process with
And energy transmission regulation, Lai Shixian Ratio-type fluorescent pH detection method, for obtain have high light chemical stability, hypotoxicity with
And the highly sensitive inorganic fluorescent pH probe material of fast-response provides new thinking, is expected to widely be made in pH detection field
With.
Detailed description of the invention
Fig. 1: Ce/Tb:NaLu in embodiment 10.2Gd0.8F4Nanocrystalline X-ray diffractogram.
Fig. 2: Ce/Tb:NaLu in embodiment 10.2Gd0.8F4Nanocrystalline scanning transmission electron microscope figure.
Fig. 3: Ce/Tb:NaLu in embodiment 10.2Gd0.8F4Nanocrystalline, under condition of different pH fluorescence spectra,
Middle excitation wavelength is 254nm.
Fig. 4: Ce/Tb:NaLu in embodiment 10.2Gd0.8F4It is nanocrystalline, Tb3+With Ce3+Luminous intensity ratio changes with pH
Curve graph.
Specific embodiment
A specific embodiment of the invention is made a detailed explanation with reference to the accompanying drawing.
Embodiment 1
By 0.54 mM of gadolinium nitrate, by 0.2 mM of lutecium nitrate, 0.2 mM of cerous nitrate, 0.06 mM of terbium nitrate, 1 milli
Mole nacl and 4 mMs of trisodium citrates, are added in 10 milliliters of water, stir 15 minutes；Then in the above solution
20 milliliters of ethylene glycol are added, stir 20 minutes；It adds 4 mMs of ammonium fluorides and stirs 30 minutes；The above solution is transferred to
In 50 milliliters of pyroreaction kettle, 120oC keeps the temperature 5 hours；After cooling, with deionized water and dehydrated alcohol centrifuge washing,
In vacuum freezing drying oven, dry 1h obtains final product.
Powder x-ray diffraction analysis the result shows that: products therefrom be pure six sides NaGdF4Phase (Fig. 1).Scanning transmission electronics
Micro- sem observation shows that its pattern is uniform monodisperse cluster type nano particle (Fig. 2), and single clustered particles size is about 90nm.
Under the excitation of wavelength 254nm xenon lamp, Ce/Tb:NaLu0.2Gd0.8F4Show very strong Tb3+Ion and relatively weak Ce3+From
Son emission peak (Fig. 3), central wavelength is respectively 550nm and 350nm, integrally show bright green light, with pH from 4 by
It is cumulative to be added to 10, Tb3+Luminous intensity gradually weaken, Ce3+The luminous intensity of ion first weakens to be increased afterwards, Tb3+With Ce3+It is glimmering
Light strength ratio is presented with the increase of pH to be weakened；Vice versa, this process is reversible change, can be used for the inspection of Ratio-type fluorescent pH
It surveys.Its detection mechanism is as follows: as pH increases to 10 from 4 ,-the COOH that surface ligand is had changes through deprotonation process
For-COO-, cause and Ce3+Connected ligand electronegativity lowers, and increases Ce3+Covalency between ligand, so that Ce3+'s
Electron cloud expands, and produces redshift effect, and then reduce Ce3+→Gd3+Energy transfer efficiency, this further suppresses Tb3+
The filling probability of ion excited state electronics, eventually leads to Tb3+The luminous intensity of ion gradually weakens with the increase of pH；It is right
Ce3+For ion, in lower pH situation, due to ligand quenching effect and weaken, under high ph conditions, since energy transmission is imitated
The sharply decrease of rate and gradually increase；Vice versa, this process is reversible change.
Embodiment 2
By 0.67 mM of gadolinium nitrate, by 0.2 mM of lutecium nitrate, 0.1 mM of cerous nitrate, 0.03 mM of terbium nitrate, 1 milli
Mole nacl and 4 mMs of trisodium citrates, are added in 10 milliliters of water, stir 15 minutes；Then in the above solution
20 milliliters of ethylene glycol are added, stir 20 minutes；It adds 4 mMs of ammonium fluorides and stirs 30 minutes；The above solution is transferred to
In 50 milliliters of pyroreaction kettle, 120oC keeps the temperature 5 hours；After cooling, with deionized water and dehydrated alcohol centrifuge washing,
In vacuum freezing drying oven, dry 1h obtains final product.The structure of the product and fluorescent characteristic are similar to Example 1.
The above are the descriptions to the embodiment of the present invention to keep this field special by the foregoing description of the disclosed embodiments
Industry technical staff can be realized or using the present invention.Various modifications to these embodiments carry out those skilled in the art
Saying will be apparent.The general principles defined herein can be the case where not departing from the spirit or scope of the present invention
Under, it realizes in other embodiments.Therefore, the present invention is not intended to be limited to these implementation columns shown in this article, but to accord with
Close the widest scope consistent with principles disclosed herein and novel point.
Claims (6)
1. a kind of Ratio-type green emission fluorescent material, which is characterized in that the molecular formula of the basis material of the fluorescent material is Ce/
Tb: NaLu0.2Gd0.8F4, carboxyl functional group is had on the surface of basis material；The fluorescent material is in ultraviolet light 254nm excitation wave
Under elongate member, Ce3+Broadband emission, emission wavelength range 300-480nm, Tb is presented3+Most strong emission peak central wavelength be
550nm integrally shows stronger green emission；As pH increases to 10, Tb from 43+Ion and Ce3+The fluorescence intensity of ion
Than apparent variation occurs.
2. a kind of Ratio-type green emission fluorescent material according to claim 1, which is characterized in that the carboxyl-functional
Group provides for citric acid.
3. the preparation method of fluorescent material described in claim 1, which is characterized in that this method includes the following steps:
1) by 0.3-0.78 mMs of gadolinium nitrate, 0.1-0.2 mMs of lutecium nitrate, 0.1-0.3 mMs of cerous nitrate, 0.02-
0.12 mM of terbium nitrate, 1-5 mMs of sodium chloride are added to 4-10 milliliters of H with 2-4 mMs of trisodium citrate2In O, stir
It mixes 10-15 minutes and obtains clear solution A；
2) 20 milliliters of ethylene glycol are added in solution A, continue stirring 20-30 minutes；
3) 3-5 mMs of ammonium fluoride is added in the solution that step 2 obtains, continues stirring 30-60 minutes, obtains translucent cream
Turbid；
4) solution that step 3) obtains is transferred in 50 milliliters of pyroreaction kettles, is placed in blast heating case, in 100-180
DEG C reaction 5-12 hours, product is obtained after furnace cooling；
5) the product ethyl alcohol and deionized water centrifuge washing for obtaining step 4), dry 1-3 is small in vacuum freezing drying oven
When obtain final product.
4. fluorescent material described in claim 1 is for the application in the detection of Ratio-type fluorescent pH.
5. a kind of Ratio-type fluorescent pH probe, which is characterized in that the probe includes fluorescent material described in claim 1.
6. a kind of Ratio-type fluorescent pH detection device, which is characterized in that the device includes that fluorescent pH as claimed in claim 4 is visited
Needle.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113969163A (en) * | 2020-07-24 | 2022-01-25 | Tcl科技集团股份有限公司 | Quantum dot composite material, preparation method thereof and environment temperature sensor |
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Cited By (1)
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| CN113969163A (en) * | 2020-07-24 | 2022-01-25 | Tcl科技集团股份有限公司 | Quantum dot composite material, preparation method thereof and environment temperature sensor |
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