CN103215037A - Method for synthesizing upconversion fluorescence hollow nanosphere based on sodium polyacrylate microsphere template synthesis - Google Patents
Method for synthesizing upconversion fluorescence hollow nanosphere based on sodium polyacrylate microsphere template synthesis Download PDFInfo
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Abstract
The invention belongs to the field of nanometer composite materials and in particular relates to a preparation method of an upconversion fluorescence hollow nanosphere based on sodium polyacrylate microsphere template synthesis. Sodium polyacrylate microsphere is used as a template for synthesizing multicolor upconversion fluorescence gadolinium trioxide mesoporous hollow nanosphere. The method comprises the following steps of: firstly, adding sodium polyacrylate to a water and isopropanol system to prepare a sodium polyacrylate microsphere; then, enabling rear-earth ions to replace sodium ions for being coordinated with carboxyl of the sodium polyacrylate microsphere to form a polymer precursor shell by using the sodium polyacrylate microsphere as the template through the ion exchange effect of the rear-earth ions and the sodium ions, wherein the polymer precursor shell is repeatedly washed by isopropanol for many times; and finally, roasting the washed polymer precursor for 2 hours at 600 DEG C to obtain the lanthanide series-doped upconversion fluorescence hollow gadolinium trioxide spheres. The method for synthesizing the upconversion fluorescence hollow nanosphere based on sodium polyacrylate microsphere template synthesis is simple and quick, gentle in conditions, green and environment-friendly. Moreover, the method can be used for drug delivering, upconversion fluorescence cell imaging and magnetic resonance imaging. Besides, the method also can be used for catalysts, a chemical reactor, a biological imaging probe and a drug delivery system.
Description
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Technical field
The invention belongs to field of nanocomposite materials, be specifically related to the preparation method of the synthetic up-conversion fluorescence hollow nanospheres of sodium polyacrylate microsphere template.
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Background technology
Up-conversion luminescence is meant that rare earth ion absorbs two or more lower energy photons and the luminescence phenomenon of a high-energy photon of radiation, typically refers near infrared light conversion visible light.Up to now, up-conversion mainly is the solid chemical compound of doped with rare-earth elements, utilizes the metastable level feature of rare earth element, can absorb a plurality of low-energy long-wave radiations, thereby makes infrared light invisible to the human eye become visible light.Compare with traditional fluorescent material, for example organic fluorescent dye molecule and semiconductor-quantum-point, it has demonstrated excellent characteristic, the narrowband emission that the stokes displacement is big, fluorescence lifetime is long, and optical property is stable, low background fluorescence and assorted scattered light, dark light penetration dimension degree, but multi-color marking etc.In recent years, the up-conversion luminescence mark is because of adopting near infrared continuous laser as excitaton source, have darker light penetration depth, lifeless matter background fluorescence disturb, to significant advantages such as biological tissue's not damageds, can with the coupling well of common confocal fluorescent imaging system, can be to of the biological sample imaging of multiple probe with tense marker, can show more details in the complicated biological sample, this imaging technique has broad application prospects in chemistry, Materials science and medical research.Wherein, the up-conversion fluorescence nano material of mesoporous hollow structure receives much concern because of its high-specific surface area, large vol, stronger optical property and widespread use especially.Based on above these advantages, many study group are devoted to the study on the synthesis of up-conversion fluorescence hollow nanospheres.
Present stage, conventional synthetic method has template and ion exchange method etc.Template is a template with the nanometer ball of finishing, and the up-conversion fluorescence layer is grown at template surface, subsequently template etching or calcining is removed, and obtains product.People such as Yuliang Zhao are by the method for template, adopt hydro-thermal carbon ball as sacrificing template, success prepared rear-earth-doped Gadolinium trioxide hollow nanospheres on a large scale.People such as Hongjie Zhang are template with the melamino-formaldehyde microballoon, remove template by heat treated mode subsequently, successfully synthesize the Gadolinium trioxide microballoon (reference: (a) G. Tian of hollow structure, Z. Gu, X. Liu, L. Zhou, W. Yin, L. Yan, S. Jin, W. Ren, G. Xing, S. Li and Y. Zhao, J. Phys. Chem. C, 2011,115,23790; (b) Z. R. Shen, J. G. Wang, P. C. Sun, D. T. Ding and T. H. Chen, Chem. Commun., 2009,13,1742; (c) J. U. Park, H. J. Lee, W. Cho, C. Jo and M. Oh, Adv. Mater., 2011,23,3161.).Ion exchange method has also obtained the concern of a lot of study group, and people such as Jun Lin are by being incorporated into vanadium ion Gd (OH) CO
3: Ln
3+In the presoma, obtain lanthanide doped hollow GdVO after calcining 10 h through 180 ° of C
4Ball (reference: X. Kang, D. Yang, Y. Dai, M. Shang, Z. Cheng, X. Zhang, H. Lian, P. Ma and J. Lin,
Nanoscale, 2013,5,253.).People such as Fan Zhang are by HF and Y
2O
3Ion exchange reaction between the nanoparticle has obtained α-NaYF
4Hollow ball (reference: F. Zhang, Y. Shi, X. Sun, D. Zhao and G. D. Stucky,
Chem. Mater., 2009,21,5237.).
Yet these prepare the method synthesis step complexity of up-conversion fluorescence hollow ball, need higher temperature of reaction, the long reaction times.It is gentle, green inadequately to react required reagent, mostly is the HF or the NaOH solution that have volatile organic reagent and have severe corrosive, based on the as above shortcoming of existing method, it is a kind of simple to need exploitation badly, green, economical and effective, on a large scale, the universal method of reaction conditions gentleness.
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Summary of the invention
The purpose of this invention is to provide a kind of general preparation method based on the synthetic up-conversion fluorescence hollow nanospheres of sodium polyacrylate microsphere template, the synthetic method is simple, and is easy to operate, and the Nano capsule function that obtains is many.
The present invention is a template with the sodium polyacrylate microballoon, the synthetic mesoporous hollow nanospheres of polychrome up-conversion fluorescence Gadolinium trioxide.
The solution of the present invention is: at first, add sodium polyacrylate in water and Virahol system, preparation sodium polyacrylate microballoon.Be template with the sodium polyacrylate microballoon then,, make rare earth ion replace sodium ion, carry out coordination, form polymerization precursor shell, clean repeatedly for several times with Virahol with the carboxyl of sodium polyacrylate microballoon by the ion exchange between rare earth ion and sodium ion.Afterwards, after calcining 2 h, 600 ° of C obtain lanthanide doped up-conversion fluorescence hollow Gadolinium trioxide ball.
Purpose of the present invention realizes by following proposal: a kind of general preparation method based on the synthetic mesoporous hollow nanospheres of up-conversion fluorescence of sodium polyacrylate microsphere template comprises the steps:
One, the preparation method of sodium polyacrylate (PAAS) microballoon: get 0.5-1 mL 0.2 g mL
-1The PAAS aqueous solution, 5-15 mL deionized water and stirring is even to wherein adding, and then to this mixed solution and dripping 40-200 mL Virahol (IPA), continues to stir 20-40 min, and it is standby to obtain the PAAS microspheres solution;
Two, the preparation method of lanthanide-doped polymerization precursor (PAA-Ln):
(1) gets above-mentioned PAAS microspheres solution 2-4 mL, add the GdCl of 0.1 M
3: YbCl
3: ErCl
3The ultrasonic 10-50 min of deionized water-IPA mixing solutions, after reaction is finished, clean 5-7 time with IPA, remove unreacted matters fully, at last the PAA-Ln precursor for preparing is put into 50 ° of C oven for drying;
(2) be the synthetic mesoporous hollow nanospheres of polychrome up-conversion fluorescence, can regulate the molar ratio of rare earth element, the mesoporous hollow nanospheres of preparation polychrome up-conversion fluorescence by adding different rare earth elements.Gd
3+: Yb
3+(Y
3+)/Er
3+(Tm
3+, Ho
3+) at Gd
2O
3: Yb
3+/ Er
3+, Gd
2O
3: Yb
3+/ Tm
3+, Gd
2O
3: Y
3+/ Er
3+, Gd
2O
3: Yb
3+/ Ho
3+And Gd
2O
3: Y
3+/ Ho
3+Molar ratio in the system is respectively: 80:18:2,79.8:20:0.2,80:18:2,79.6:20:0.4 and 79.6:20:0.4.
Three, the preparation method who synthesizes the mesoporous hollow nanospheres of polychrome up-conversion fluorescence based on the sodium polyacrylate microsphere template: product 400-600 ° of C calcining 2 ~ 4 h with step 2 obtain the synthetic mesoporous hollow nanospheres of up-conversion fluorescence of sodium polyacrylate microsphere template.
Obtain polychrome up-conversion fluorescence hollow Gadolinium trioxide ball by method for preparing.Compare the present invention with traditional method and have following advantage:
1, the present invention has proposed the method for synthetic sodium polyacrylate microballoon in water-Virahol system, method simple and fast, mild condition, environmental protection first.
2, the carboxyl functional group of the sodium polyacrylate microsphere surface of the present invention preparation can carry out coordination with rare earth ion, therefore can be used as functional template applications in the synthesizing of last conversion nano hollow ball.
3, the present invention is in the process of the synthetic mesoporous hollow nanospheres of polychrome up-conversion fluorescence, avoided the use of complicated treating processes and harmful reagent.
4, the present invention does not need template is modified or particular processing in the process of the synthetic mesoporous hollow nanospheres of up-conversion fluorescence, so this method is simple, convenient.
5, the polychrome up-conversion fluorescence hollow Gadolinium trioxide ball that obtains of the present invention has dispersed preferably and bigger hollow structure, therefore can be used for drug conveying, up-conversion fluorescence cell imaging and nuclear magnetic resonance.
6, condition of the present invention is simple, gentleness, and natural environmental protection can be extended to the synthetic of other hollow nano materials, and this class material can be with being catalyzer, chemical reactor, bio-imaging probe and delivery system.
The invention provides the preparation method of the mesoporous hollow nanospheres of novel polychrome up-conversion fluorescence, use the sodium polyacrylate microballoon as template, the method environmental protection, mild condition, easy handling, method is general, and the nanoparticulate dispersed that obtains is better, has wide practical use in a plurality of fields such as biotherapy and clinical medicine.
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Description of drawings
The transmission electron microscope picture of accompanying drawing 1, the sodium polyacrylate microballoon for preparing for the present invention;
The transmission electron microscope picture of accompanying drawing 2, the lanthanide-doped polymerization precursor for preparing for the present invention;
Accompanying drawing 3, the red up-conversion fluorescence hollow Gd for preparing for the present invention
2O
3: Yb
3+/ Er
3+The transmission electron microscope picture of nanometer ball;
Accompanying drawing 4, the red up-conversion fluorescence hollow Gd for preparing for the present invention
2O
3: Yb
3+/ Er
3+The nitrogen adsorption figure of nanometer ball and graph of pore diameter distribution;
Accompanying drawing 5, the red up-conversion fluorescence hollow Gd for preparing for the present invention
2O
3: Yb
3+/ Er
3+The up-conversion fluorescence spectrogram of nanometer ball;
Accompanying drawing 6, the blue up-conversion fluorescence hollow Gd for preparing for the present invention
2O
3: Yb
3+/ Tm
3+The transmission electron microscope picture of nanometer ball; Accompanying drawing 7, the green up-conversion fluorescence hollow Gd for preparing for the present invention
2O
3: Y
3+/ Er
3+The transmission electron microscope picture of nanometer ball;
Accompanying drawing 8, the red up-conversion fluorescence hollow Gd for preparing for the present invention
2O
3: Yb
3+/ Ho
3+The transmission electron microscope picture of nanometer ball;
Accompanying drawing 9, the deep green look up-conversion fluorescence hollow Gd for preparing for the present invention
2O
3: Y
3+/ Ho
3+The transmission electron microscope picture of nanometer ball.
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Embodiment
Embodiment 1:
Based on the synthetic mesoporous Gd of red up-conversion fluorescence of sodium polyacrylate microsphere template
2O
3: Yb
3+/ Er
3+And Gd
2O
3: Yb
3+/ Ho
3+The preparation of hollow nanospheres:
(1) synthetic sodium polyacrylate (PAAS) microballoon: under the room temperature, get 0.5 mL, 0.2 g mL
-1The PAAS aqueous solution, 10 mL deionized water and stirring are even to wherein adding, in this mixing solutions, dropwise drip 40 mL Virahols (IPA) then, continue to stir 20 min, obtain dispersiveness PAAS microspheres solution standby (volume ratio of water and Virahol is 1:4) preferably;
(2) get above-mentioned PAAS microspheres solution 4 mL, add the GdCl of 320 μ L, 0.1 M
3: YbCl
3: ErCl
3(Gd
3+: Yb
3+/ Er
3+=80:18:2) or GdCl
3: YbCl
3: HoCl
3(Gd
3+: Yb
3+/ Ho
3+=79.6:20:0.4) ultrasonic 20 min of deionized water-IPA mixing solutions after reaction is finished, clean 5 times with IPA, and the centrifugal unreacted matters of removing is fully put into 50 ° of C oven for drying with the precursor of preparation at last;
(3) white powder that oven dry in the step (2) is obtained is calcined 2 h at 600 ° of C (heat up in argon gas atmosphere before 600 ° of C, heat-up rate is 2 ° of C min
-1, after temperature reaches 600 ° of C, calcining 2 h in air atmosphere), in the process that forms the rare earth oxide shell, template is decomposed and is removed synchronously, treat that nature is cooled to room temperature after, obtain the mesoporous Gd of red up-conversion fluorescence
2O
3: Yb
3+/ Er
3+And Gd
2O
3: Yb
3+/ Ho
3+Hollow nanospheres.
Embodiment 2:
Based on the synthetic mesoporous Gd of green up-conversion fluorescence of sodium polyacrylate microsphere template
2O
3: Y
3+/ Er
3+The preparation of hollow nanospheres:
(1) with embodiment 1;
(2) get above-mentioned PAAS microspheres solution 4 mL, add the GdCl of 320 μ L, 0.1 M
3: YCl
3: ErCl
3(Gd
3+: Y
3+/ Er
3+=80:18:2) ultrasonic 20 min of deionized water-IPA mixing solutions, other are with embodiment 1;
(3) with embodiment 1.
Embodiment 3:
Based on the mesoporous Gd of sodium polyacrylate microsphere template synthesizing blue up-conversion fluorescence
2O
3: Yb
3+/ Tm
3+The preparation of hollow nanospheres:
(1) with embodiment 1;
(2) get above-mentioned PAAS microspheres solution 4 mL, add the GdCl of 320 μ L, 0.1 M
3: YbCl
3: TmCl
3(Gd
3+: Yb
3+/ Tm
3+=79.8:20:0.2) ultrasonic 20 min of deionized water-IPA mixing solutions, other are with embodiment 1;
(3) with embodiment 1.
Embodiment 4:
Based on the synthetic mesoporous Gd of deep green up-conversion fluorescence of sodium polyacrylate microsphere template
2O
3: Y
3+/ Ho
3+The preparation of hollow nanospheres:
(1) with embodiment 1;
(2) get above-mentioned PAAS microspheres solution 4 mL, add the GdCl of 320 μ L, 0.1 M
3: YCl
3: HoCl
3(Gd
3+: Y
3+/ Ho
3+=79.6:20:0.4) ultrasonic 20 min of deionized water-IPA mixing solutions, other are with embodiment 1;
(3) with embodiment 1.
Claims (1)
1. the method for the synthetic up-conversion fluorescence hollow nanospheres of sodium polyacrylate microsphere template is characterized in that comprising the steps:
One, the preparation method of sodium polyacrylate PAAS microballoon: get 0.5-1 mL 0.2 g mL
-1The PAAS aqueous solution, 5-15 mL deionized water and stirring is even to wherein adding, and then to this mixed solution and dripping 40-200 mL Virahol IPA, continues to stir 20-40 min, and it is standby to obtain the PAAS microspheres solution;
Two, the preparation method of lanthanide-doped polymerization precursor PAA-Ln:
(1) gets above-mentioned PAAS microspheres solution 2-4 mL, add the GdCl of 0.1 M
3: YbCl
3: ErCl
3The ultrasonic 10-50 min of deionized water-IPA mixing solutions, after reaction is finished, clean 5-7 time with IPA, remove unreacted matters fully, at last the PAA-Ln precursor for preparing is put into 50 ° of C oven for drying;
(2) be synthetic up-conversion fluorescence hollow nanospheres,, regulate the molar ratio of rare earth element, preparation polychrome up-conversion fluorescence hollow nanospheres, Gd by adding different rare earth elements
3+: Yb
3+(Y
3+): Er
3+(Tm
3+, Ho
3+) at Gd
2O
3: Yb
3+/ Er
3+, Gd
2O
3: Yb
3+/ Tm
3+, Gd
2O
3: Y
3+/ Er
3+, Gd
2O
3: Yb
3+/ Ho
3+And Gd
2O
3: Y
3+/ Ho
3+Molar ratio in the system is respectively: 80:18:2,79.8:20:0.2,80:18:2,79.6:20:0.4 and 79.6:20:0.4;
Three, the preparation method who synthesizes polychrome up-conversion fluorescence hollow nanospheres based on the sodium polyacrylate microsphere template: product 400-600 ° of C calcining 2 ~ 4 h with step 2 obtain the synthetic up-conversion fluorescence hollow nanospheres of sodium polyacrylate microsphere template.
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| CN105385447A (en) * | 2015-09-19 | 2016-03-09 | 江西理工大学 | Low-cost method for preparing NaREF4 type upconversion light-emitting porous microspheres in large quantities |
| CN105482804A (en) * | 2016-01-11 | 2016-04-13 | 东北师范大学 | Latent fingerprint detection probe and a preparation method thereof |
| CN105646789A (en) * | 2016-03-15 | 2016-06-08 | 大连理工大学 | Method for preparing fluorescent polymer rare earth complex nano-microsphere |
| CN105713603A (en) * | 2016-03-23 | 2016-06-29 | 江西理工大学 | Method for preparing MF2 type water-soluble mesoporous light-emitting nanospheres in efficient and green mode |
| CN105950148A (en) * | 2016-04-29 | 2016-09-21 | 中国计量大学 | Preparation method for preparing ferroferric oxide hollow ball-based fluorescent magnetic composite material |
| CN108485649A (en) * | 2018-04-25 | 2018-09-04 | 深圳市裕同包装科技股份有限公司 | A kind of fast preparation method of rare earth down-conversion fluorescent microballoon |
| CN110643365A (en) * | 2019-10-25 | 2020-01-03 | 无锡威孚环保催化剂有限公司 | Synthesis method of cubic spherical yttrium oxide particles doped with rare earth ytterbium and thulium |
| CN115381968A (en) * | 2022-08-23 | 2022-11-25 | 中山大学 | Rare earth-organic composite optical nano probe and preparation method and application thereof |
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|---|---|---|---|---|
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| CN105482804B (en) * | 2016-01-11 | 2018-03-09 | 东北师范大学 | A kind of latent fingerprint detection probe and preparation method thereof |
| CN105646789A (en) * | 2016-03-15 | 2016-06-08 | 大连理工大学 | Method for preparing fluorescent polymer rare earth complex nano-microsphere |
| CN105713603A (en) * | 2016-03-23 | 2016-06-29 | 江西理工大学 | Method for preparing MF2 type water-soluble mesoporous light-emitting nanospheres in efficient and green mode |
| CN105950148A (en) * | 2016-04-29 | 2016-09-21 | 中国计量大学 | Preparation method for preparing ferroferric oxide hollow ball-based fluorescent magnetic composite material |
| CN108485649A (en) * | 2018-04-25 | 2018-09-04 | 深圳市裕同包装科技股份有限公司 | A kind of fast preparation method of rare earth down-conversion fluorescent microballoon |
| CN110643365A (en) * | 2019-10-25 | 2020-01-03 | 无锡威孚环保催化剂有限公司 | Synthesis method of cubic spherical yttrium oxide particles doped with rare earth ytterbium and thulium |
| CN115381968A (en) * | 2022-08-23 | 2022-11-25 | 中山大学 | Rare earth-organic composite optical nano probe and preparation method and application thereof |
| CN115381968B (en) * | 2022-08-23 | 2023-09-26 | 中山大学 | Rare earth-organic composite optical nano probe and preparation method and application thereof |
| CN116265568A (en) * | 2022-09-09 | 2023-06-20 | 南京市第一医院 | Green fluorescent infrared up-conversion mesoporous nanomaterial and preparation method thereof |
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Application publication date: 20130724 |