CN106350057A - Preparation method of fluorescent hybrid nanoparticles - Google Patents
Preparation method of fluorescent hybrid nanoparticles Download PDFInfo
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- CN106350057A CN106350057A CN201610686464.1A CN201610686464A CN106350057A CN 106350057 A CN106350057 A CN 106350057A CN 201610686464 A CN201610686464 A CN 201610686464A CN 106350057 A CN106350057 A CN 106350057A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
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- 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
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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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- C—CHEMISTRY; METALLURGY
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- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/18—Metal complexes
- C09K2211/182—Metal complexes of the rare earth metals, i.e. Sc, Y or lanthanide
Abstract
The invention discloses a preparation method of fluorescent hybrid nanoparticles. The preparation method includes: preparing ternary complexes of rare-earth europium under the alkaline condition (adjustment with a water solution of sodium hydroxide) prior to dispersing via an alkaline solution (adjustment with ammonium hydroxide); subjecting the alkaline solution to further hybrid reaction with silica gel; on the premises of reducing particle size of silicon dioxide, enabling dispersibility of the ternary complexes of the rare-earth europium in silicon dioxide nanoparticles to be improved. The obtained fluorescent hybrid nanoparticles are obviously improved in fluorescence property, fluorescence strength is doubled that of a pure complex, fluorescence decay trend is alleviated, fluorescence life is prolonged, and raw materials good in fluorescence property are provided for photoluminescence materials.
Description
Technical field
The present invention relates to fluorescent material technical field, more particularly, to a kind of preparation method of fluorescence nano hybrid particle.
Background technology
Why rare earth has excellent luminescent properties, is it to have special energy translation function that (i.e. electronics is not
Produce energy with the transition between energy level) and special 4f electron structure.But rare earth ion is in the specific absorbance ε of near ultraviolet band
Very little, therefore, luminous efficiency is relatively low.The sixties in 20th century, weissman is found that " antenna effect (antenna effect) ",
This theory makes the luminous efficiency of rare earth ion be improved.But find after further research, organic network of rare earth ion
Compound heat stability is poor, high concentration when be susceptible between concentration self-quenching phenomenon, preparation method and microstructure the compatibility
Mismatch etc. constrains practical application in terms of optical physicss for the rare-earth complex.
Solve these problems and improve the method for rare earth material fluorescence intensity and be mainly, luminescence rare earth ion and inorganic matrix
Material forms composite, or luminescence rare earth ion forms composite with macromolecular compound.The invention mainly relates to be
The first research direction.1985, r.reisfeld and its team utilized sol-gel process by serial organic fluorescence molecule embedding
To nano silicon and nanometer sio2-tio2In thin film, by the test of fluorescence property, draw what fluorescence property was improved
Conclusion, and foretell application prospect in terms of laser and solaode for this kind of material.1997, k.machida and
G.adachi is prepared for the organic rare-earth complex compound of silicon dioxide embedded europium and terbium using sol-gel process, and has drawn embedding
The conclusion that rear thermal property and fluorescence property are all improved, but be not given directly perceived in the sign forming embedding structure
Effectively image；2002, professor m.morita was also prepared for silicon dioxide embedded organic RE complexation using sol-gel process
Thing, this time they are extended for cerium, samarium, europium and four kinds of elements of terbium the species of rare earth, and mainly have studied temperature and annealing right
The impact of rare-earth complex fluorescence property.During 2004 to 2007 years, Chinese Academy of Sciences's Changchun optical precision optical machinery is ground with physics
Jiu Suo Qin Wei flat (w.p.qin) professor and its research team's microemulsion method and sedimentation are prepared for silicon dioxide embedded organic dilute
Native complex, fluorescence intensity is improved, and fluorescence lifetime reduces.
Content of the invention
The technical problem being existed based on background technology, the present invention proposes a kind of preparation side of fluorescence nano hybrid particle
Method, the method chemical reaction condition is simple, and product is stable, repeatable strong, gained fluorescence-causing substance good luminous performance, optical property
Stable.
A kind of preparation method of fluorescence nano hybrid particle, comprises the following steps:
A, prepare the ethanol solution of Europium chloride, the ethanol solution of α-thenoyltrifluoroacetone and the ethanol of Phen are molten
Liquid；
B, the 3 kinds of solution hybrid reactions taking in step a, pipet Deca sodium hydrate aqueous solution, adjusting ph value is 8-11,
The complex obtaining is centrifuged to obtain paste product；
C, the complex obtaining step b are centrifuged to obtain paste product, with acetone solution up to clear；
D, the solution obtaining step c are added in tri-distilled water and the mixed solution of strong aqua ammonia, stir 0.5-1 hour, shape
Become stable solution；
E, ethanol is mixed with tri-distilled water, then be separately added into strong aqua ammonia and tetraethyl orthosilicate；
The solution that f, the solution obtaining step d are obtained with step e mixes under stirring, continues reaction 0.5-1 little
When；
The solution centrifugal that g, step f obtain, alcohol is washed 2 times, puts 40-55 DEG C of thermostatic drying chamber drying, obtains white powder,
It is fluorescence nano hybrid particle.
Preferably, in described step a, the preparation method of the ethanol solution of Europium chloride is: weighs europiumsesquioxide white
Powder simultaneously adds deionized water, stirring, makes white powder become pasty state, is placed in 50 DEG C of water-baths and dropwise adds under conditions of magnetic agitation
Enter salt aqueous acid, until white paste becomes the solution of transparent clarification；Gained settled solution is utilized Rotary Evaporators
Boil off unnecessary moisture, and so that excessive hydrochloric acid is fully volatilized, then be dried through thermostatic drying chamber, obtain water white Europium chloride
Crystal, with anhydrous alcohol solution.
Preferably, the ethanol of the Europium chloride that the concentration of the solution prepared in described step a is respectively as follows: 0.1mol/l is molten
Liquid, the ethanol solution of the α-thenoyltrifluoroacetone of 0.3mol/l, the ethanol solution of the Phen of 0.1mol/l.
The present invention compared with the preparation method of existing SiO 2 hybrid organic rare-earth complex compound, the ternary complexation of rare-earth europium
Thing (adjusts) preparation in the basic conditions again through alkaline solution (adjusting with strong aqua ammonia) dispersion with the aqueous solution of sodium hydroxide, afterwards with
The further hybrid reaction of silica dioxide gel, on the basis of reducing nano silicon particle diameter, makes the ternary of Europium
Dispersibility in Nano particles of silicon dioxide for the complex improves.
The invention has benefit that:
1st, adopt the fluorescence nano hybrid particle of present invention preparation, fluorescence property is significantly improved, with pure complex
Fluorescence intensity is compared and is doubled, and fluorescence decay trend relaxes, and fluorescence lifetime improves.
2nd, a kind of preparation method of fluorescence nano hybrid particle involved in the present invention, will provide glimmering for embedded photoluminescent material
The excellent raw material of optical property.
Brief description
Transmission electron microscope structure and morphology figure during Fig. 1: embodiment 1 fluorescence nano hybrid particle liquid condition.
The fluorescence emission spectrogram of compound of Fig. 2: embodiment 1 fluorescence nano hybrid particle.
(built-in little figure is vertical seat for the fluorescence decay curve of Fig. 3: embodiment 1 fluorescence nano hybrid particle and fluorescence lifetime value
Mark takes fluorescence decay curve during common logarithm).
Specific embodiment
Embodiment 1:
A kind of preparation method of fluorescence nano hybrid particle, comprises the following steps:
(1) weigh and record 25ml round-bottomed flask quality, 0.5cm specification fusiform rotor quality, weigh europiumsesquioxide
White powder 0.125g, in round-bottomed flask, adds 1ml deionized water, stirring, makes white powder become pasty state, be placed in 50 DEG C of water-baths
It is added dropwise over salt aqueous acid under conditions of magnetic agitation, until white paste becomes the solution of transparent clarification.
(2) gained settled solution is boiled off unnecessary moisture using Rotary Evaporators, and so that excessive hydrochloric acid is fully volatilized,
It is dried through thermostatic drying chamber, obtain water white Europium chloride crystal, calculate 0.0008mol again.
(3) measure 8ml dehydrated alcohol, dissolve water white transparency Europium chloride crystal, the ethanol obtaining 0.1mol/l Europium chloride is molten
Liquid.
(4) preparation of organic rare-earth complex compound: the ethanol solution of configuration 0.3mol/l α-thenoyltrifluoroacetone,
The ethanol solution of 0.1mol/l Phen, with the ethanol solution three of 0.1mol/l Europium chloride according to 1:1:1 mol ratio magnetic
Power stirring reaction 2 hours, Deca sodium hydrate aqueous solution 10 makes ph=8, generates the ternary complexes of europium, 8000 revs/min
Centrifugation, alcohol wash each product once, obtaining 2ml acetone solution up to clear.
(5) preparation of nanometer titanium dioxide Silica hydrogel: 33.35ml ethanol is mixed in glass container with 13.5ml tri-distilled water
Close, then be separately added into 0.7ml strong aqua ammonia and 2.45ml tetraethyl orthosilicate, prepare the particle diameter 200 of gained nano silicon ±
60nm.
(6) add the mixing of the strong aqua ammonia of 15ml tri-distilled water and micro 25%-28% molten in the solution that step (4) obtains
Liquid, magnetic agitation 1 hour, form stable solution.
(7) generation of fluorescence nano hybrid particle: the solution that step (6) is obtained is added under conditions of magnetic agitation
Step (5) resulting solution, reacts 1 hour.
(8) solution centrifugal that step (7) obtains, alcohol is washed 2 times, puts 40-55 DEG C of thermostatic drying chamber drying, obtains white powder
End.
After testing, obtain transmission electron microscope structure and morphology during embodiment 1 fluorescence nano hybrid particle liquid condition
Figure (Fig. 1)；The fluorescence emission spectrogram of compound (Fig. 2) of embodiment 1 fluorescence nano hybrid particle；Embodiment 1 fluorescence nano hybrid particle
Fluorescence decay curve and fluorescence lifetime value (built-in little figure is that vertical coordinate takes fluorescence decay curve during common logarithm) (Fig. 3).
Embodiment 2
A kind of preparation method of fluorescence nano hybrid particle, comprises the following steps:
(1) preparation of organic rare-earth complex compound: such as the method in embodiment 1, the ethanol of configuration 0.1mol/l Europium chloride is molten
Liquid, the ethanol solution of 0.3mol/l α-thenoyltrifluoroacetone, the ethanol solution of 0.1mol/l Phen, three is according to 1:
The mol ratio magnetic agitation of 1:1 is reacted 2 hours, Deca sodium hydrate aqueous solution 13, ph=9, generates the ternary complexes of europium,
8000 revs/min of centrifugations, alcohol wash each product once, obtaining 2ml acetone solution up to clear.
(2) preparation of nanometer titanium dioxide Silica hydrogel: 33.35ml ethanol is mixed in glass container with 13.5ml tri-distilled water
Close, then be separately added into 0.7ml strong aqua ammonia and 2.45ml tetraethyl orthosilicate, prepare the particle diameter 150 of gained nano silicon ±
60nm.
(3) add the mixing of the strong aqua ammonia of 15ml tri-distilled water and micro 25%-28% molten in the solution that step (1) obtains
Liquid, magnetic agitation 1 hour, form stable solution.
(4) generation of fluorescence nano hybrid particle: the solution that step (3) is obtained is added under conditions of magnetic agitation
Step (2) resulting solution, reacts 1 hour.
(5) solution centrifugal that step (4) obtains, alcohol is washed 2 times, puts 40-55 DEG C of thermostatic drying chamber drying, obtains white powder
End.
Embodiment 3
A kind of preparation method of fluorescence nano hybrid particle, comprises the following steps:
(1) preparation of organic rare-earth complex compound: such as the method in embodiment 1, the ethanol of configuration 0.1mol/l Europium chloride is molten
Liquid, the ethanol solution of 0.3mol/l α-thenoyltrifluoroacetone, the ethanol solution of 0.1mol/l Phen, three is according to 1:
The mol ratio magnetic agitation of 1:1 is reacted 2 hours, Deca sodium hydrate aqueous solution 15, ph=11, generates the ternary complexation of europium
Thing, 8000 revs/min of centrifugations, alcohol wash each product once, obtaining 4ml acetone solution up to clear.
(2) preparation of nanometer titanium dioxide Silica hydrogel: 33.35ml ethanol is mixed in glass container with 13.5ml tri-distilled water
Close, then be separately added into 0.7ml strong aqua ammonia and 2.45ml tetraethyl orthosilicate, prepare the particle diameter 130 of gained nano silicon ±
60nm.
(3) add the mixing of the strong aqua ammonia of 15ml tri-distilled water and micro 25%-28% molten in the solution that step (1) obtains
Liquid, magnetic agitation 1 hour, form stable solution.
(4) generation of fluorescence nano hybrid particle: the solution that step (3) is obtained is added under conditions of magnetic agitation
Step (2) resulting solution, reacts 1 hour.
(5) solution centrifugal that step (4) obtains, alcohol is washed 2 times, puts 40-55 DEG C of thermostatic drying chamber drying, obtains white powder
End.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept equivalent or change in addition, all should be included within the scope of the present invention.
Claims (4)
1. a kind of preparation method of fluorescence nano hybrid particle is it is characterised in that comprise the following steps:
A, prepare ethanol solution, the ethanol solution of α-thenoyltrifluoroacetone and the ethanol solution of Phen of Europium chloride；
B, the 3 kinds of solution hybrid reactions taking in step a, pipet Deca sodium hydrate aqueous solution, adjusting ph value is 8-11, obtains
Complex be centrifuged to obtain paste product；
C, the complex obtaining step b are centrifuged to obtain paste product, with acetone solution up to clear；
D, the solution obtaining step c are added in tri-distilled water and the mixed solution of strong aqua ammonia, stir 0.5-1 hour, are formed steady
Fixed solution；
E, ethanol is mixed with tri-distilled water, then be separately added into strong aqua ammonia and tetraethyl orthosilicate；
The solution that f, the solution obtaining step d are obtained with step e mixes under stirring, continues reaction 0.5-1 hour；
The solution centrifugal that g, step f obtain, alcohol is washed 2 times, puts 40-55 DEG C of thermostatic drying chamber drying, obtains white powder, as
Fluorescence nano hybrid particle.
2. the preparation method of fluorescence nano hybrid particle as claimed in claim 1 is it is characterised in that in described step a, chlorine
The preparation method changing the ethanol solution of europium is: weighs europiumsesquioxide white powder and adds deionized water, stirring, and make white powder
End becomes pasty state, is placed in 50 DEG C of water-baths and is added dropwise over salt aqueous acid under conditions of magnetic agitation, until white paste becomes
Become the solution of transparent clarification；Gained settled solution is boiled off unnecessary moisture using Rotary Evaporators, and so that excessive hydrochloric acid is filled
Divide volatilization, then be dried through thermostatic drying chamber, obtain water white Europium chloride crystal, with anhydrous alcohol solution.
3. the preparation method of fluorescence nano hybrid particle as claimed in claim 1 is it is characterised in that join in described step a
The concentration of the solution of system is respectively as follows: the ethanol solution of the Europium chloride of 0.1mol/l, the α-thenoyltrifluoroacetone of 0.3mol/l
Ethanol solution, the ethanol solution of the Phen of 0.1mol/l.
4. the preparation method of fluorescence nano hybrid particle as claimed in claim 1 is it is characterised in that comprise the following steps:
(1) weigh and record 25ml round-bottomed flask quality, 0.5cm specification fusiform rotor quality, weigh europiumsesquioxide white
Powder 0.125g, in round-bottomed flask, adds 1ml deionized water, stirring, makes white powder become pasty state, be placed in 50 DEG C of water-baths in magnetic
It is added dropwise over salt aqueous acid, until white paste becomes the solution of transparent clarification under conditions of power stirring；
(2) gained settled solution is boiled off unnecessary moisture using Rotary Evaporators, and so that excessive hydrochloric acid is fully volatilized, then warp
Thermostatic drying chamber is dried, and obtains water white Europium chloride crystal, calculates 0.0008mol；
(3) measure 8ml dehydrated alcohol, dissolve water white transparency Europium chloride crystal, obtain the ethanol solution of 0.1mol/l Europium chloride；
(4) preparation of organic rare-earth complex compound: the ethanol solution of configuration 0.3mol/l α-thenoyltrifluoroacetone, 0.1mol/l
The ethanol solution of Phen, anti-according to the mol ratio magnetic agitation of 1:1:1 with the ethanol solution three of 0.1mol/l Europium chloride
Answer 2 hours, Deca sodium hydrate aqueous solution 10 makes ph=8, generate the ternary complexes of europium, 8000 revs/min of centrifugations, alcohol are washed
Each product once, obtaining 2ml acetone solution is up to clear；
(5) preparation of nanometer titanium dioxide Silica hydrogel: 33.35ml ethanol is mixed in glass container with 13.5ml tri-distilled water, then
It is separately added into 0.7ml strong aqua ammonia and 2.45ml tetraethyl orthosilicate, prepare the particle diameter 200 ± 60nm of gained nano silicon；
(6) mixed solution of the strong aqua ammonia of 15ml tri-distilled water and micro 25%-28%, magnetic are added in the solution that step (4) obtains
Power stirs 1 hour, forms stable solution；
(7) generation of fluorescence nano hybrid particle: the solution that step (6) is obtained is added to step under conditions of magnetic agitation
(5) resulting solution, reacts 1 hour；
(8) solution centrifugal that step (7) obtains, alcohol is washed 2 times, puts 40-55 DEG C of thermostatic drying chamber drying, obtains white powder,
It is fluorescence nano hybrid particle.
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Cited By (6)
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| CN108034420A (en) * | 2017-12-27 | 2018-05-15 | 青岛大学 | Inorganic nano-particle embedding terbium complex hybrid luminescent materials and preparation method thereof |
| CN108091767A (en) * | 2017-12-25 | 2018-05-29 | 青岛大学 | The preparation method of rare-earth complex doping silicon dioxide microspheres solution and modified solar battery |
| CN109504366A (en) * | 2019-01-07 | 2019-03-22 | 青岛大学 | A kind of rare-earth complex cladding nano-hollow SiO2With cladded type rare-earth complex and preparation method thereof |
| CN109777015A (en) * | 2019-01-22 | 2019-05-21 | 青岛大学 | A kind of preparation method of the luminous hydrogel material of PEG graft polymers |
| CN111270520A (en) * | 2020-01-17 | 2020-06-12 | 青岛大学 | Flexible fabric capable of efficiently emitting light to detect bacteria and preparation method and application thereof |
| CN113004888A (en) * | 2021-02-24 | 2021-06-22 | 青岛大学 | Europium complex doped TiO2Nano particle fluorescence sensing material, preparation method and application |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108091767A (en) * | 2017-12-25 | 2018-05-29 | 青岛大学 | The preparation method of rare-earth complex doping silicon dioxide microspheres solution and modified solar battery |
| WO2019127765A1 (en) * | 2017-12-25 | 2019-07-04 | 青岛大学 | Methods for preparing rare-earth-complex-doped silica microsphere solution and modified solar cell |
| CN108091767B (en) * | 2017-12-25 | 2019-07-23 | 青岛大学 | The preparation method of rare-earth complex doping silicon dioxide microspheres solution and modified solar battery |
| CN108034420A (en) * | 2017-12-27 | 2018-05-15 | 青岛大学 | Inorganic nano-particle embedding terbium complex hybrid luminescent materials and preparation method thereof |
| CN109504366A (en) * | 2019-01-07 | 2019-03-22 | 青岛大学 | A kind of rare-earth complex cladding nano-hollow SiO2With cladded type rare-earth complex and preparation method thereof |
| CN109777015A (en) * | 2019-01-22 | 2019-05-21 | 青岛大学 | A kind of preparation method of the luminous hydrogel material of PEG graft polymers |
| CN109777015B (en) * | 2019-01-22 | 2021-04-13 | 青岛大学 | Preparation method of PEG (polyethylene glycol) grafted polymer luminescent hydrogel material |
| CN111270520A (en) * | 2020-01-17 | 2020-06-12 | 青岛大学 | Flexible fabric capable of efficiently emitting light to detect bacteria and preparation method and application thereof |
| CN111270520B (en) * | 2020-01-17 | 2022-03-18 | 青岛大学 | Flexible fabric capable of efficiently emitting light to detect bacteria and preparation method and application thereof |
| CN113004888A (en) * | 2021-02-24 | 2021-06-22 | 青岛大学 | Europium complex doped TiO2Nano particle fluorescence sensing material, preparation method and application |
| CN113004888B (en) * | 2021-02-24 | 2023-06-06 | 青岛大学 | Europium complex doped TiO 2 Nanoparticle fluorescent sensing material, preparation method and application |
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