CN104357056B - Preparation method of europium-doped sodium gadolinium fluoride red light-emitting porous nanocrystal material - Google Patents
Preparation method of europium-doped sodium gadolinium fluoride red light-emitting porous nanocrystal material Download PDFInfo
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Abstract
The invention discloses a preparation method of a europium-doped sodium gadolinium fluoride red light-emitting porous nanocrystal material, relating to a light-emitting nano material of which the nominal composition is NaGd[1-x]EuxF4 (x=0-10 mol%). The red light-emitting porous nanocrystal material has the advantages of favorable dispersity, controllable crystal form structure and shape, high fluorescence intensity, low rare-earth consumption due to porous structure, energy saving and the like. The preparation technique is simple and does not need any surfactant; and the whole reaction is carried out in the water solution without using any organic solvent, so the method is economical and environment-friendly and is convenient for industrial production.
Description
Technical field：
The present invention relates to a kind of rare-earth europium ion doping gadolinium fluoride sodium emitting red light porous nanocrystalline material and preparation method,
Belong to rear-earth-doped luminous material preparing technical field.
Background technology：
NaYF4And NaGdF4Have Deng alkali metal rare earth fluoride that phonon energy is low, multi-phonon non-radiative relaxation is low, luminous
The features such as efficiency high, in green illumination light source, nano photoelectronic devices, FPD, biomedical imaging, biomarker and mirror
The aspect such as fixed has broad application prospects, by the common concern of Chinese scholars.NaYF4And NaGdF4Be respectively provided with six sides and
Cube two kinds of crystal structures, the luminous efficiency of hexagonal crystallographic texture is significantly larger than cubic crystal structure, wherein hexagonal crystallographic texture
NaYF4It is well-known most preferably upper conversion host material.
Gadolinium（Gd3+）Ion has larger energy gaps, realizes other rare earth ions frequently as a kind of sensitized ions
（Eu3+, Dy3+, Tb3+Deng）Lower conversion light；Ytterbium can be passed through simultaneously（Yb3+）Ion and upper conversion ions（Er3+, Tm3+,
Ho3+Deng）Be co-doped with, in NaGdF4Efficient rare earth ion up-conversion luminescence is realized in matrix.And utilize matrix cation Gd3+
Paramagnetic performance, this nanocrystalline can be simultaneously as good magnetic resonance contrast agent.Therefore, rear-earth-doped NaGdF4Nano particle
It is expected to become a kind of and integrate that upper and lower conversion is luminous and the multi-functional nanometer material of magnetic property.In addition, Gd3+Ionic radius
Compare Y3+Slightly larger, use Gd3+Replace Y3+Matrix cation as such nanocrystal will be helpful to the mutually nanocrystalline life of hexagonal crystal
Become, and can clearly shorten reaction required time, reduce reaction temperature and improve up-conversion luminescence efficiency (Nature 2010,
463, 1061-1065).
At present, there are many methods can be for preparing uniform particle diameter, the rear-earth-doped NaGdF of morphology controllable4Light and receive
Rice corpuscles, including hydro-thermal method, complexed-precipitation method, high temperature organic solvent hydrothermal method, sol-gel process etc..These preparation methods are not only
Have that the reaction time is oversize, efficiency is low to some extent, severe reaction conditions, particle are big, product regularity and bad dispersibility etc.
Shortcoming, and be usually associated with harmful by-products and produce.On the other hand, porous or hollow ball structure nanocrystalline due to its mesopore
The presence of gap, rare-earth usage is few, and luminous intensity is high, has therefore saved the rare earth resources of preciousness, has received the extensive concern of people.
Guo Gao et al. adopts one step hydro thermal method, reacts 10h when 320 DEG C, has obtained NaYF4Multi-pore micron rod structure, it is about 3
～5 μm, about 1 μm of diameter, aperture about 28.5 nm；But under the same reaction conditions, the NaGdF of preparation4Sub-micron crystal is simultaneously
Do not show loose structure（Nanoscale, 2013, 5, 351）.Up to the present, without any surfactant,
With NaGdF4Monodisperse porous nanocrystalline document for matrix and patent yet there are no open report.
Content of the invention：
Present invention proposition is a kind of to prepare the method mixing europium gadolinium fluoride sodium emitting red light porous nanocrystalline material.
The present invention another object is that provide said method preparation mix europium gadolinium fluoride sodium emitting red light porous nanocrystalline material.
The concrete technical scheme of the present invention is as follows：
A kind of preparation method mixing europium gadolinium fluoride sodium emitting red light porous nanocrystalline material, the group of this material is divided into：
NaGd1-x Eu x F4(x=0～10 mol%), the preparation process of this material is as follows：
1）Measure Gd (NO3)3With Eu (NO3)3Solution is dissolved in distilled water, obtains [Gd (NO3)3+Eu(NO3)3] mixing
Solution, wherein Gd3+With Eu3+Mol ratio be (1-x):X, wherein 0<x<0.1, take the 1/5～1/8 of this mixed liquor volume to stay
With；Add urea in above-mentioned mixed solution, heat 2～3 h when 90 DEG C, be slowly formed white precipitate；Will be heavy for gained white
Shallow lake centrifugal sedimentation, and with distillation water washing 1～2 time, being then transferred in another container, adds distilled water, and ultrasonic disperse 15～
20 min, then magnetic agitation 0.5～1 h, obtain white suspension A；Wherein, the addition of urea and Gd in suspension A3+'s
Mol ratio is（15～22）：1；
2）The aqueous solution of NaF, Gd in wherein NaF and suspension A is added in suspension A3+Mol ratio be（8～10）：
1, magnetic agitation, so that reactant is sufficiently mixed, obtain white suspension B；
3）Then add step 1 in suspension B）[Gd (the NO continuing to employ3)3+Eu(NO3)3] mixed solution, continue magnetic force
Stirring 0.5～1 h obtains suspension C；
4）Suspension C is transferred in reactor, reactor volume compactedness be 70%-80%, put it in baking oven
Hydro-thermal process 12～20 h at a temperature of 160～180 DEG C；Reaction utilizes centrifugal sedimentation completely afterwards, and by the white depositions obtaining
Washed respectively 2～3 times with distilled water and absolute ethyl alcohol, the pH value to filtrate is neutrality；White depositions are in 70～80 DEG C of conditions
Lower drying 4～8 h, you can obtain mixing europium gadolinium fluoride sodium emitting red light porous nanocrystalline material.
The design further of the present invention is：
Step 1）In, Gd (NO3)3The concentration of solution is 0.2-0.4 mol/L；Eu(NO3)3The concentration of solution is 0.1-0.2
mol/L.
Step 2）In, the concentration of described NaF solution is 2～4 mol/L.
Prepared by said method mixes europium gadolinium fluoride sodium emitting red light porous nanocrystalline material.This is nanocrystalline to have porous knot
Structure, pore diameter range 3-5 nm.
Compared with prior art, the present invention has following remarkable advantage：
1）The present invention prepares porous nano crystal structure using special experimental technique.Obtain after NaF is reacted with suspension A
Suspension B, because NaF is excessive, unnecessary F- adsorbs on sediment surface.[Gd (the NO continuing to employ is added in suspension B3)3+
Eu(NO3)3] solution, by F-- rare earth ion-F-Coupling, will be nanocrystalline for formation crosslinked together for the precipitation particle being formed, in water
Under thermal rection condition, due to crystallizing into phase, nanocrystalline be internally formed vacancy, finally give porous nano crystal structure.
2）It is not necessary to add surfactant, whole reaction carries out, does not have preparation process is simple of the present invention in aqueous
Using any organic solvent, economic and environment-friendly, it is easy to industrialized production.
3）What this method obtained mixes europium gadolinium fluoride sodium emitting red light porous nanocrystalline, not only has from Eu3+Deng rare earth from
It is multicolor luminous that son activates, and has from matrix cation Gd3+Paramagnetism, thus merging luminous and paramagnetism is one
Body, is a kind of multi-functional nanometer material having significant application value in biomedicine.
4）What this method obtained mix europium gadolinium fluoride sodium emitting red light porous nanocrystalline shows preferable monodispersity, and
Size is less, and by changing process conditions, controllable products therefrom is long 100～150 nm, the regular rod of diameter 20～50 nm
Shape is nanocrystalline.
5）What this method obtained mix europium gadolinium fluoride sodium emitting red light porous nanocrystalline has loose structure, aperture about 3-5
Nm, and fluorescence intensity is very strong, peak shape is sharp.Porous nanocrystalline rare-earth usage is few, has saved the rare earth resources of preciousness.
Brief description
Fig. 1 is the X-ray diffraction spectrogram mixing europium gadolinium fluoride sodium porous nanocrystalline prepared by embodiment 1.
Fig. 2 is the transmission electron microscope picture mixing europium gadolinium fluoride sodium porous nanocrystalline prepared by embodiment 1.
Fig. 3 is the high resolution TEM figure mixing europium gadolinium fluoride sodium porous nanocrystalline prepared by embodiment 1.
Fig. 4 is the exciting light spectrogram mixing europium gadolinium fluoride sodium porous nanocrystalline prepared by embodiment 1.
Fig. 5 is the launching light spectrogram mixing europium gadolinium fluoride sodium porous nanocrystalline prepared by embodiment 1.
Specific embodiment：
With reference to being embodied as example, the technical solution of the present invention is further described, these embodiments are not
It is understood that as being the restriction to technical solution.
Embodiment 1：
The present invention mixes europium gadolinium fluoride sodium emitting red light porous nanocrystalline material, and group is divided into：NaGd1-x Eu x F4, whereinx= 5
mol %.Its concrete preparation process is as follows：
1）Measure the Gd (NO of 9.5 ml respectively3)3Solution（Concentration is 0.4 mol/L）Eu (NO with 1 ml3)3Solution
（Concentration is 0.2 mol/L）It is dissolved in 150 ml distilled water, obtain [Gd (NO3)3+Eu(NO3)3] mixed solution, take out 25 ml
Continue to employ.Add 3 g urea in mixed solution, heat 2 h when 90 DEG C, be slowly formed white precipitate.By gained white precipitate
Centrifugal sedimentation, and with distillation water washing 1 time, being then transferred in beaker, adds 40 ml distilled water, ultrasonic disperse 15 min, so
Magnetic agitation 0.5 h afterwards, obtains white suspension A；
2）Add the aqueous solution of 14 ml NaF in suspension A, its concentration is 2 mol/L, magnetic agitation makes reactant
It is sufficiently mixed, obtain white suspension B；
3）Then add step 1 in suspension B）25 ml [Gd (the NO continuing to employ3)3+Eu(NO3)3] mixed solution, continue
Continuous magnetic agitation 0.5 h, obtains suspension C.
4）Suspension C is transferred in reactor, reactor volume compactedness is 80%, puts in baking oven in 180 DEG C of temperature
Lower hydro-thermal process 20 h；Reaction utilizes centrifugal sedimentation completely afterwards, and by the white depositions obtaining distilled water and absolute ethyl alcohol
Wash 3 times respectively, the pH value to filtrate is neutrality；White depositions are dried under the conditions of 75 DEG C 6 h, you can obtain mixing europium
Gadolinium fluoride sodium emitting red light porous nanocrystalline material.
Embodiment 2：
The present invention mixes europium gadolinium fluoride sodium emitting red light porous nanocrystalline material, and group is divided into：NaGd1-x Eu x F4, whereinx= 2
mol %.Its concrete preparation process is as follows：
1）Measure the Gd (NO of 9.8 ml respectively3)3Solution（Concentration is 0.4 mol/L）Eu (NO with 0.8 ml3)3Molten
Liquid（Concentration is 0.1 mol/L）It is dissolved in 180 ml distilled water, obtain [Gd (NO3)3+Eu(NO3)3] mixed solution, take out 30
Ml continues to employ.Add 3.5 g urea in mixed solution, heat 2.5 h when 90 DEG C, be slowly formed white precipitate.Gained is white
Color pelleting centrifugation settles, and with distillation water washing 2 times, is then transferred in beaker, addition 30 ml distilled water, ultrasonic disperse 18
Min, then magnetic agitation 0.5 h, obtain white suspension A；
2）Add the aqueous solution of 8 ml NaF in suspension A, its concentration is 4 mol/L, magnetic agitation makes reactant
It is sufficiently mixed, obtain white suspension B；
3）Then add step 1 in suspension B）30 ml [Gd (the NO continuing to employ3)3+Eu(NO3)3] mixed solution, continue
Continuous magnetic agitation 1 h, obtains suspension C.
4）Suspension C is transferred in reactor, reactor volume compactedness is 70%, puts in baking oven in 170 DEG C of temperature
Lower hydro-thermal process 15 h；Reaction utilizes centrifugal sedimentation completely afterwards, and by the white depositions obtaining distilled water and absolute ethyl alcohol
Wash 2 times respectively, the pH value to filtrate is neutrality；White depositions are dried under the conditions of 70 DEG C 8 h, you can obtain mixing europium
Gadolinium fluoride sodium emitting red light porous nanocrystalline material.
Embodiment 3：
The present invention mixes europium gadolinium fluoride sodium emitting red light porous nanocrystalline material, and group is divided into：NaGd1-x Eu x F4, whereinx= 8
mol%.Its concrete preparation process is as follows：
1）Measure the Gd (NO of 9.2 ml respectively3)3Solution（Concentration is 0.4 mol/L）Eu (NO with 1.6 ml3)3Molten
Liquid（Concentration is 0.2 mol/L）It is dissolved in 200 ml distilled water, obtain [Gd (NO3)3+Eu(NO3)3] mixed solution, take out 35
Ml continues to employ.Add 4 g urea in mixed solution, heat 3 h when 90 DEG C, be slowly formed white precipitate.Will be heavy for gained white
Shallow lake centrifugal sedimentation, and with distillation water washing 1 time, being then transferred in beaker, adds 30 ml distilled water, ultrasonic disperse 20 min,
Then magnetic agitation 0.5 h, obtains white suspension A；
2）Add the aqueous solution of 15 ml NaF in suspension A, its concentration is 2 mol/L, so that reactant is sufficiently mixed,
Obtain white suspension B；
3）Then add step 1 in suspension B）35 ml [Gd (the NO continuing to employ3)3+Eu(NO3)3] mixed solution, continue
Continuous magnetic agitation 0.5 h, obtains suspension C.
4）Suspension C is transferred in reactor, reactor volume compactedness is 80%, puts in baking oven in 170 DEG C of temperature
Lower hydro-thermal process 15 h；Reaction utilizes centrifugal sedimentation completely afterwards, and by the white depositions obtaining distilled water and absolute ethyl alcohol
Wash 3 times respectively, the pH value to filtrate is neutrality；White depositions are dried under the conditions of 80 DEG C 4 h, you can obtain mixing europium
Gadolinium fluoride sodium emitting red light porous nanocrystalline material.
Test case：
Performance measurement is carried out to the europium gadolinium fluoride sodium emitting red light porous nanocrystalline material of mixing of embodiment one preparation：
Mix europium gadolinium fluoride sodium emitting red light porous nanocrystalline material and there is good crystallinity, the interplanar distance of its diffraction cutting edge of a knife or a sworddValue and relative intensity and NaGdF4Standard card（27-0699）ListeddValue is consistent with relative intensity, belongs to hexagonal crystal system,
As shown in Figure 1.
This NaGdF4：Eu3+Porous nanocrystalline material has Rod-like shape, a diameter of 20～50 nm, length be 100～
150nm, as shown in Figure 2.
This NaGdF4：Eu3+Porous nanocrystalline material has loose structure, aperture about 3-5 nm, as shown in Figure 3.
When monitoring wavelength and being 615 nm, the described excitation spectrum master mixing europium gadolinium fluoride sodium emitting red light porous nanocrystalline
The strong bands of a spectrum that peak is located at 273 nm, belong to Gd3+Ion8S7/2→6IJTransition, and the peak at 310 nm belongs to Gd3+Ion
's8S7/2→6PJTransition, the peak at 394.5 nm belongs to Eu3+Characteristic absorption, corresponds to7F0→5L6Transition, as shown in Figure 4.
Under the ultraviolet excitation of 273 nm and 394.5 nm, mix europium gadolinium fluoride sodium porous nanocrystalline and launch main peak and be located at
592 nm and the bright red of 615 nm, its corresponding Eu3+Ion5D0→7F1With5D0→7F2Transition, the transmitting of 695 nm
Peak corresponds to Eu3+Ion5D0→7F4Transition, as shown in Figure 5.Luminous intensity under the exciting of wherein 273 nm is higher than
394.5 nm excite, and illustrate by means of Gd3+The sensitization of ion, Gd3+By energy transfer to Eu after Ions Absorption energy3+, obtain
Strong Eu3+Red lower conversion of ion lights.
From above test result, this material has important in multiple fields and is widely applied value.
Certainly, the present invention also can have various embodiments, in the case of without departing substantially from present invention spirit and its essence, is familiar with this
The technical staff in field when can according to the present invention make various corresponding change and deform, but these corresponding change and deformation should
Belong to the protection domain of appended claims of the invention.
Claims (3)
1. a kind of preparation method mixing europium gadolinium fluoride sodium emitting red light porous nanocrystalline material, the group of this material is divided into：NaGd1- x Eu x F4, it is characterized in that：The preparation process of this material is as follows：
1）Measure Gd (NO3)3With Eu (NO3)3Solution is dissolved in distilled water, obtains [Gd (NO3)3+Eu(NO3)3] mixed solution,
Wherein Gd3+With Eu3+Mol ratio be (1-x):X, wherein 0<x<0.1, take the 1/5～1/8 of this mixed liquor volume to continue to employ；To
Add urea in above-mentioned mixed solution, heat 2～3 h when 90 DEG C, be slowly formed white precipitate；Gained white precipitate is centrifuged
Sedimentation, and with distillation water washing 1～2 time, be then transferred in another container, addition distilled water, ultrasonic disperse 15～20 min,
Then magnetic agitation 0.5～1 h, obtains white suspension A；Wherein, the addition of urea and Gd in suspension A3+Mol ratio
For（15～22）：1；
2）The aqueous solution of NaF, Gd in wherein NaF and suspension A is added in suspension A3+Mol ratio be（8～10）：1, magnetic
Power stirs, and so that reactant is sufficiently mixed, obtains white suspension B；
3）Then add step 1 in suspension B）[Gd (the NO continuing to employ3)3+Eu(NO3)3] mixed solution, continue magnetic agitation
0.5～1 h obtains suspension C；
4）Suspension C is transferred in reactor, reactor volume compactedness is 70%-80%, puts it in baking oven 160
Hydro-thermal process 12～20 h at a temperature of～180 DEG C；Reaction utilizes centrifugal sedimentation completely afterwards, and the white depositions obtaining are steamed
Distilled water and absolute ethyl alcohol wash 2～3 times respectively, and the pH value to filtrate is neutrality；White depositions are dry under the conditions of 70～80 DEG C
Dry 4～8 h, you can obtain mixing europium gadolinium fluoride sodium emitting red light porous nanocrystalline material.
2. preparation method according to claim 1, is characterized in that：Step 1）In, Gd (NO3)3The concentration of solution is 0.2-
0.4 mol/L；Eu(NO3)3The concentration of solution is 0.1-0.2 mol/L.
3. preparation method according to claim 1, is characterized in that：Step 2）In, the concentration of described NaF solution is 2～4
mol/L.
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| CN101787284A (en) * | 2010-02-10 | 2010-07-28 | 长春理工大学 | Upconversion luminescent hollow sphere using yttrium fluoride as ground substance and preparation method thereof |
| CN102618283A (en) * | 2012-02-24 | 2012-08-01 | 长春理工大学 | Method for preparing bowknot-shaped terbium-mixed Teflon gadolinium sodium green luminous nanometer materials |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101787284A (en) * | 2010-02-10 | 2010-07-28 | 长春理工大学 | Upconversion luminescent hollow sphere using yttrium fluoride as ground substance and preparation method thereof |
| CN102618283A (en) * | 2012-02-24 | 2012-08-01 | 长春理工大学 | Method for preparing bowknot-shaped terbium-mixed Teflon gadolinium sodium green luminous nanometer materials |
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| 空壳及介孔结构稀土氟化物的制备及其光学性能的研究;王刘振;《哈尔滨大学硕士学位论文》;20140430;第4章第33-34页，46页 * |
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