CN104099098A - Preparation of magnetic long-afterglow light-emitting nano material with magnetic porous material as core - Google Patents
Preparation of magnetic long-afterglow light-emitting nano material with magnetic porous material as core Download PDFInfo
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Abstract
The invention provides a new method of preparation of a magnetic long-afterglow light-emitting nano material. The method can solve a problem of sintering during high-temperature calcination of a long-afterglow light-emitting material in the prior art well. The nano material prepared through the method is uniform in particles, is neat in shape, has an excellent long-afterglow light-emitting performance and an excellent magnetic performance, and has potential applications in the fields of biology and medicine. The method has a wide range of application, can be widely used for preparing various magnetic light-emitting nano materials. The method is mainly characterized by employing magnetic cores, such as ferroferric oxide and gadolinium oxide; wrapping external layers of the magnetic cores with materials such as porous silicon dioxide and aluminium oxide; adsorbing light-emitting substrate ions such as alkaline-earth metals and the like, and light-emitting activating ions such as rare earth metals and the like, or a gel precursor of a long-afterglow light-emitting material with the core-shell-structure magnetic microspheres as a template; and performing a high-temperature calcination process to obtain the magnetic light-emitting nano material such as a light-emitting silicate, a light-emitting aluminate, a light-emitting aluminosilicate, a light-emitting phosphate and the like.
Description
Technical field
The invention belongs to magnetic long after glow luminous material field, relate generally to a kind of novel method of preparing magnetic long after glow luminous material, in more detail, the magnetic nano material of apparatus of the present invention is core, nano material in skin parcel porous, using the nano material of porous of this magnetic as masterplate, utilize specific surface area absorption that magnetic porous nano-form is huge to form metal ion the high-temperature calcination of long after glow luminous material, obtain the good magnetic long-persistence nano of pattern material.
Background technology
Nanometer long after glow luminous material has highly sensitive, without external light source, excites and do not produce the advantages such as organism autofluorescence lamp, in bio-imaging, field of drug delivery, paid attention to, but cause it in application aspect, to be extremely restricted because photoimaging resolving power is lower.Magnetic imaging is a kind of high-resolution imaging mode of generally acknowledging in the world, but magnetic imaging is difficult to realize real time imagery, and because the restriction of instrument aspect is easy to occur illusion, the accuracy of impact diagnosis.The mentioned long-persistence luminous nano material of magnetic of the present invention has excellent long-persistence luminous performance and magnetic simultaneously, so just can there is long-afterglow fluorescent imaging and magnetic imaging simultaneously, realize highly sensitive and high-resolution imaging, be expected to be all widely used and study in fields such as bio-imaging, biological detection, tracking cell, gene order, bioseparation, targeted drug conveyings.In addition, the preparation method of traditional long after glow luminous material has no idea to obtain pattern rule as sol-gel method, solid sintering technology, and the uniform nano particle of size distribution, is not suitable for the preparation of the long-persistence luminous nano material of magnetic.The domestic and international report about the long-persistence luminous nano material of magnetic does not almost have at present.
Summary of the invention
The object of this invention is to provide a kind of novel method of preparing the long-persistence luminous nano material of magnetic.Technique of the present invention is simple, easy to operate, is easy to scale operation.The long-persistence luminous appearance of nano material rule of magnetic of utilizing the present invention to prepare, particle diameter is controlled, and magnetic is good.The present invention uses Fe
3o
4, γ-Fe
2o
3, Gd
2o
3gdS, Fe etc. or contain Gd element, Fe element and to have paramagnetic nano material be core, at porous nanometer materials such as the silicon-dioxide of the skin parcel vesicular structure of magnetic Nano core, aluminum oxide, silicate, aluminate, phosphoric acid salt, form the magnetic porous nano material of nucleocapsid structure, utilize the specific surface area absorption that porous material is huge to form in the metal ion solution or precursor sol of long after glow luminous material, through high-temperature roasting, obtain the long-persistence luminous nano material of magnetic.
The present invention mainly comprises following basic step:
(1) prepare magnetic porous nano material
The present invention uses Fe
3o
4, γ-Fe
2o
3, Gd
2o
3gdS, Fe etc. or contain Gd element, Fe element and to have paramagnetic nano material be core, the nano materials such as the silicon-dioxide of porous, aluminum oxide, silicate, aluminate, aluminosilicate, phosphoric acid salt or their mixture obtain magnetic porous nano material as porous shell, by regulating particle diameter, pattern and the magnetic etc. of magnetic porous nano material, can regulate easily particle diameter, pattern and the magnetic etc. of the finished product.It is the microscopic appearance feature that the shape characteristic of magnetic porous material has determined the long-persistence luminous nano material of magnetic of preparation.Used magnetic porous nanometer material, as mature preparation process such as magnetic mesoporous silicon-dioxide, magnetic mesoporous aluminum oxide, has much realized suitability for industrialized production, can prepare voluntarily easily.
(2) preparation forms metal ion solution or the precursor sol of long after glow luminous material
Form the long-persistence luminous nano material metal ion of magnetic and conventionally contain the matrix ion such as Ca, Mg, Sr, Ba, Zn, Cd, the activation ions such as rare earth ion, transition element ion.Form the metal ion solution of long after glow luminous material by the direct lyotropic salt (being often nitrate or hydrochloride) with these elements of water dissolution, can prepare easily the solution that contains these ions.In solution, alternative citric acid, polyoxyethylene glycol, boric acid, the ammonium chloride etc. of adding are to regulate the solubleness of metal ion, the character such as soltion viscosity.The precursor sol that forms long after glow luminous material passes through at organic solvent as ethanol, the metal oxygen-containing acid esters that the dissolvings such as ethylene glycol contain the luminous host element that forms the long-persistence luminous nano material of magnetic, as tetra-n-butyl titanate, isopropyl titanate etc., and lyotropic salt (being often nitrate or hydrochloride) obtains containing the viscosity that can optionally add the increase colloidal sols such as citric acid, polyoxyethylene glycol, EDTA in these element colloidal sol colloidal sols.
(3) metal ion solution or the precursor sol that utilize magnetic porous nano material absorption to form long after glow luminous material join the described magnetic porous nano material of a certain amount of step (1) in the described solution of step (2) or colloidal sol, soak certain hour, the metal ion solution or the precursor sol that form long after glow luminous material are entered in the micropore of magnetic porous nano material by diffusion, absorption.Through centrifugal or filtering separation, dry obtained adsorbing form the metal ion solution of long after glow luminous material or the magnetic porous nano material of precursor sol.
(4) high-temperature calcination
The magnetic porous nano material that to process through step (3), puts into High Temperature Furnaces Heating Apparatus, through high-temperature roasting certain hour, generates long-persistence luminous nano material.Obtain size-grade distribution very evenly with Fe
3o
4, γ-Fe
2o
3, Gd
2o
3, GdS, Fe etc. or contain Gd element, Fe element and to have paramagnetic nano material be core, the long-persistence luminous nano material of magnetic that the long-persistence luminous nano materials such as silicate, aluminate, aluminosilicate, phosphoric acid salt are shell.
Accompanying drawing explanation
Fig. 1 is Gd
2o
3/ Ca
2gd
8(SiO
4)
6o
2: Eu, Dy, the surface sweeping electron micrograph of Mn.
Fig. 2 is Gd
2o
3/ Ca
2gd
8(SiO
4)
6o
2: Eu, Dy, the XRD figure of Mn.
Fig. 3 is Gd
2o
3/ Ca
2gd
8(SiO
4)
6o
2: Eu, Dy, the exciting light spectrogram of Mn.
Fig. 4 is Gd
2o
3/ Ca
2gd
8(SiO
4)
6o
2: Eu, Dy, the twilight sunset utilizing emitted light spectrogram of Mn.
Fig. 5 is Gd
2o
3/ Ca
2gd
8(SiO
4)
6o
2: Eu, Dy, the Magnetic resonance imaging figure of Mn.
Fig. 6 is relaxation rate and 1/T
1graph of a relation.
Fig. 7 is Gd
2o
3/ CaTiO
3: the stereoscan photograph of Pr.
Fig. 8 is Gd
2o
3/ CaTiO
3: the XRD figure of Pr.
Fig. 9 is Gd
2o
3/ CaTiO
3: the excitation and emission spectra figure of Pr.
Figure 10 is Gd
2o
3/ CaTiO
3: the T1 Magnetic resonance imaging figure of Prr.
Figure 11 is relaxation rate and 1/T
1graph of a relation.
Embodiment
Example 1: we introduce a kind of with Gd
2o
3for core, the magnetic porous nano material of mesoporous silicon oxide porous shell is that the metal ion solution of raw material absorption formation long after glow luminous material is prepared the long-persistence luminous nano material Gd of magnetic yellow
2o
3the specific implementation method of/Ca2Gd8 (SiO4) 6O2.Get 0.3g Gd (OH)
3, be dispersed in ultrasonic dispersion 20 min in 160 mL ethanol 40 mL water, add wherein the ammoniacal liquor of 2 mL 28 wt%, solution is 20
oc stirred in water bath 30 min, add 50 uL TEOS, continue to stir 6 h at this temperature.The Gd obtaining (OH)
3@nSiO
2the centrifugal collection of nano particle, water and ethanol are respectively washed three times, are dispersed in 120 mL ethanol, in 160 mL water, add wherein the ammoniacal liquor of 2 mL 28wt%, 20
oc stirred in water bath 30 min, add 2 mL TEOS, continue to stir 6 h at this temperature.The centrifugal collection of product, water and ethanol are respectively washed three times, and 60
oc vacuum-drying 2 h.550
oc calcines 5 h, obtains the Gd of 200 ~ 400nm
2o
3@mSiO
2.By magnetic porous nano material Gd
2o
3@mSiO
20.3 g is immersed in 30 mL and contains Ca (NO
3)
2, Eu (NO
3)
3, Dy (NO
3)
3, Mn (NO
3)
2metal ion solution in, its ion concentration is 100:(1 ~ 10) (1 ~ 10): (1 ~ 10), stir 0.5 hour ~ 24 hours, centrifugation has obtained adsorbing the magnetic porous silicon-dioxide of metal ion, then containing 3% ~ 10%H
2argon gas atmosphere in, through 800 ℃ ~ 1200 ℃ calcinings, within 2 hours ~ 24 hours, can obtain the long-persistence luminous nano material of magnetic that particle diameter is 200 nm.Its chemical structure can be expressed as Gd
2o
3/ Ca
2gd
8(SiO
4)
6o
2: Eu, Dy, Mn.Obtain the electron scanning micrograph of product referring to accompanying drawing 1.By accompanying drawing 1, can see the long-persistence luminous nano material Gd of magnetic preparing by the present invention
2o
3/ Ca
2gd
8(SiO
4)
6o
2: Eu, Dy, Mn size distribution is very narrow, pattern rule.By X-ray diffraction analysis (Fig. 2), can confirm that products therefrom contains Ca
2gd
8(SiO
4)
6o
2crystalline phase.Known by measuring twilight sunset transmitting and excitation spectrum (Fig. 3 and Fig. 4), the twilight sunset emission peak of the long-persistence luminous nano material of magnetic of preparation is 580 nm, is typical Ca
2gd
8(SiO
4)
6o
2twilight sunset emission peak, the main excitation peak of this material is positioned at UV-light wave band, but can be by the excited by visible light of 450 nm ~ 470 nm.This material irradiates through fluorescent lamp, can send bright yellow twilight sunset, and under dark surrounds, naked eyes reach 2 h visible time of persistence.The magnetic of this material has carried out characterizing (Fig. 5 and Fig. 6) by T1 Magnetic resonance imaging, has obtained obvious NMR (Nuclear Magnetic Resonance) imaging photo, and the relaxation rate of this material (r1) is 4.13 mM s
-1.
Example 2: we introduce a kind of with Gd
2o
3for core, the magnetic porous nano material of mesoporous silicon oxide porous shell is that the sol precursor of raw material absorption formation long after glow luminous material is prepared magnetic red long-afterglow Illuminant nanometer material Gd
2o
3/ CaTiO
3: the implementation method that Pr is concrete.Take 0.3g Gd (OH)
3, be dispersed in ultrasonic dispersion 20 min in 160 mL ethanol 40 mL water, add wherein the ammoniacal liquor of 2 mL 28wt%, solution is 20
oc stirred in water bath 30 min, add 50 uL TEOS, continue to stir 6h at this temperature.The Gd obtaining (OH)
3@nSiO
2the centrifugal collection of nano particle, water and ethanol are respectively washed three times, are dispersed in 120 mL ethanol, in 160 mL water, add wherein the ammoniacal liquor of 2 mL 28 wt%, 20
oc stirred in water bath 30min, adds 2 mL TEOS, continues to stir 6 h at this temperature.The centrifugal collection of product, water and ethanol are respectively washed three times, and 60
oc vacuum-drying 2h.550
oc calcines 5 h, obtains Gd
2o
3@mSiO
2.Get 2.361 g Ca (NO
3)
2, 2.1014 g monohydrate potassiums, 1 g polyoxyethylene glycol 10,000 is dissolved in 50 mL ethanol, adds wherein 2 mL 0.001mol/L Pr (NO
3)
3ethanolic soln, use HNO
3regulate pH=1, in oxytropism solution, add after stirring for some time under 3.5mL tetra-n-butyl titanate room temperature and occur white opacity, in solution, add 0.5 mL HNO
3, continuing to stir for some time, white opacity disappears, and solution becomes clarification, by the CaTiO of clarification
3: Pr colloidal sol is put in uncovered stirring volatilization ethanol in stink cupboard, is reduced to 20mL. regulator solution pH extremely neutral to solution.By magnetic porous nano material Gd
2o
3@mSiO
20.2g is dispersed in CaTiO prepared by 30 mL
3: in Pr colloidal sol, stir 2 hours ~ 5 hours, centrifugation has obtained adsorbing the magnetic porous silicon-dioxide of sol precursor ion, and under air atmosphere, 500 ℃ ~ 900 ℃ roastings obtain the long-persistence luminous nanometer material of magnetic, and its chemical structure can be expressed as Gd
2o
3/ CaTiO
3: Pr.Obtain the electron scanning micrograph of product referring to accompanying drawing 7, can be to from accompanying drawing 7, the long-persistence luminous nano material Gd of magnetic preparing by the present invention
2o
3/ CaTiO
3: Pr size distribution is even, pattern rule.By X-ray diffraction analysis (Fig. 8), can confirm that products therefrom contains CaTiO
3crystalline phase.Known by measuring twilight sunset transmitting and excitation spectrum (Fig. 9), the twilight sunset emission peak of the long-persistence luminous nano material of magnetic of preparation is 613 nm, is typical CaTiO
3: Pr twilight sunset emission peak, the main excitation peak of this material is positioned at UV-light wave band, with the ultra violet lamp of 365 nm, can send bright red twilight sunset, and under dark surrounds, naked eyes reach 1 h visible time of persistence.The magnetic of this material is passed through T
1magnetic resonance imaging has carried out characterizing (Figure 10 and Figure 11), has obtained obvious NMR (Nuclear Magnetic Resonance) imaging photo, the relaxation rate (r of this material
1) be 6.43 mM s
-1.
Although the present invention is set forth with reference to specific embodiments, but skilled person will easily recognize suitable alternative magnetic porous material, metal ion solution or sol precursor and preparation method in this area, the present invention simultaneously also can be applied to prepare other magnetic Illuminant nanometer material.These magnetic porous materials, metal ion solution or sol precursor, preparation method and the application in other magnetic Illuminant nanometer material of preparation also will comprise in the present invention, and the present invention is limited by appended claims only.
Claims (7)
1. the magnetic core in this patent is Fe
3o
4, γ-Fe
2o
3, Gd
2o
3, GdS, Fe etc. contain Gd element, Fe element and have paramagnetic material; Porous outer layer shell structure in this patent is to comprise silicon-dioxide, aluminum oxide silicon-dioxide, aluminum oxide, silicate, aluminate, aluminosilicate, phosphoric acid salt etc. or their mixture, form magnetic porous masterplate used in this patent by the material with above-mentioned two specific characters.
2. magnetic porous masterplate according to claim 1, the present invention is that to utilize the magnetic porous material described in claim 1 be raw material, be immersed in the metal ion solution or precursor sol that forms long after glow luminous material, utilize the duct adsorptive power of magnetic porous material, adsorbing metal ions or precursor sol ion, through calcining after a while, obtain the long-persistence luminous nano material of magnetic that pattern is good.
3. method according to claim 2, metal ion solution wherein and precursor sol ion comprise matrix metal ion and activation ion two classes.
4. according to claim 3, wherein said machine-processed metal ion mainly comprises alkaline-earth metal ions Mg
2+, Ca
2+, Sr
2+, Ba
2+and Zn
2+, Cd
2+, Pb
2+, Al
3+, Ga
3+, Sn
5+deng, precursor sol ion mainly comprises SO
4 2-, TiO
4 4-, VO
4 -, WO
4 2-, PO
4 3-, HPO
4 2-, H
2pO
4 -, P
2o
7 4-, AsO
4 3-, GeO
4 4-, GaO
4 5-, AlO
4 5-, SnO
4 3-deng oxygen acid radical ion and S
2-, F
-, Cl
-, Br
-, I
-deng negatively charged ion.
5. according to claim 3, wherein said activation ion refers to rare earth ion and transition metal ion, and rare earth ion refers to Eu, Dy, and Nd, Ho, Ce, Tb, Tm, Er, Pr etc., transition metal ion refers to Mn, Co, Al, Cu, Ti etc.
6. according to claim 2, wherein said long-persistence luminous nano material matrix can be expressed as AMgSi
2o
6; A
2mgSi
2o
7; A
3mgSi
2o
8; AAl
2o
4; A
xal
ysiO
z; A
2p
2o
7; A
3p
2o
8; A
xp
yo
z; ATiO
3; AWO
4; BVO
4; A
2b
8(SiO
4)
6o
2deng, wherein A is Ca, Sr, and Mg, Ba, Zn, Cd, Pb etc. or their combination, B is rare earth ion Eu, Dy, Nd, Ho, Ce, Tb, Gd, Y, La etc.
7. according to claim 6, with the different rare earth ion of above-mentioned host doped, transition metal ion, nonmetallic ion is as F, Cl, and Br, I etc. can obtain the long-persistence luminous nano material of magnetic that light emitting region can regulate and control.
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| CN115282296A (en) * | 2022-08-09 | 2022-11-04 | 中国科学院赣江创新研究院 | Superparamagnetic near-infrared long-lasting nanoparticle, and preparation method and application thereof |
| CN116925763A (en) * | 2023-07-28 | 2023-10-24 | 中国科学院赣江创新研究院 | Near infrared long afterglow nano probe for imaging atherosclerosis plaque, and preparation method and application thereof |
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Application publication date: 20141015 |