CN106939162A - SiO2The synthetic method of@Tb (phen-Si) L nuclear shell structure nano luminescent composites - Google Patents
SiO2The synthetic method of@Tb (phen-Si) L nuclear shell structure nano luminescent composites Download PDFInfo
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Abstract
A kind of SiO2The synthetic method of@Tb (phen-Si) L nuclear shell structure nano luminescent composites.Using particle diameter as 500nm SiO2Microballoon is kernel, is modified with phen-Si.Using sulfoxide and terbium perchlorate organic coordination compound as clad, SiO is synthesized2@Tb (phen-Si) L core-shell type rare earth nano light-emitting composites.The invention belongs to rare earth organic fluorescent materials field.The problem of mainly solving is by conventional SiO2The rare earth luminescent material of doping type makes core-shell rare-earth luminescent material.Specific method is to do " molecular bridge " with silane coupler phen-Si, its one end is connected with silicon ball, double N atoms and the rare earth Tb of the other end3+Coordination, while sulfoxide part can also be with Tb3+Coordination, the SiO as a result modified in phen-Si2Rare earth Sulfoxide coordination compound on microballoon external sheath, obtains two kinds of new SiO2(500)@Tb(Phen-Si) L(20), SiO2(500)@Eu(Phen-Si)L(100)SiO2Nuclear shell structure nano luminescent composite.Material preparation method of the present invention is simple, and rare earth organic complex clad is nanoscale, therefore high-purity rare-earth consumption is few, low cost.Obtain the excellent nuclear shell structure nano luminescent material of luminescent properties simultaneously.
Description
Technical field
The invention belongs to rare earth luminescent material field, it is related to the SiO of core shell structure2@
The synthetic method of Tb (phen-Si) L luminescent materials, due to the SiO using inexpensive safety2Microballoon is kernel, using the method for self assembly by terbium perchlorate, adjacent carboxy phenyl carboxymethyl sulfoxide L（C6H4(COOH)SOCH2COOH）, pass through phen-Si（Molecular formula is (phen)-N- (CONH (CH2)3Si(OCH2CH
3) 3)2）With SiO2Kernel chemistry, which is bonded, to be connected together, and forms SiO2@
Tb (phen-Si) L nuclear shell structure nano luminescent composites.
Background technology
Core-shell type structure nano compound particle be it is a kind of construct novel, the nanoscale as formed by another nano material is coated by a kind of nano material by chemical bond or other interactions ordered fabrication structure, be higher level nano composite structure.Because core-shell type structure nano particle has the peculiar property for being different from any single substance, cause the concern of more and more people.One layer of other materials are coated in particle surface, can make to be wrapped by particle by changing coating structure, size and particle composition has magnetic, light, heat, electricity, photoelectricity and catalysis characteristics.Nucleocapsid structure is mainly to strengthen the advantages such as its fluorescence intensity, raising quantum yield, enhancing stability for the change of luminescent material property.Although each component keeps relative independentability in composite, but the property of core-shell structure copolymer composite be not each component property simple plus and, but on the basis of some features of each component material are kept, with the combination property acted synergistically between generation component, this fully compensate for the shortcoming of homogenous material, the new performance not available for homogenous material is generated, the new situation in terms of design of material is opened.As described above, the characteristics of nano material has many excellent compared with common massive material.So in recent years, with developing rapidly for nanometer rare-earth compound luminescent material, nucleocapsid structure material turns into the important means that synthesizing new fluorescent material is used, by kernel using cheap material so that the cost of product is minimized.By precise control experiment condition, the core/shell structure luminescent material of specific morphology, size and function can be prepared according to demand.This core/shell structure luminescent material is being remained outside the luminosity of original fluorescent material, also many unique properties such as the stability with nucleocapsid, Modulatory character, self assembly, is had a extensive future, thus is widely paid attention to.
Because with being easy to be made into spherical monodisperse nano-particle particle, particle diameter is easily controlled, the advantages, SiO such as with low cost and hypotoxicity are synthesized2It is one of nano-particle of current most widely used core shell structure, based on Nano-meter SiO_22Very special spheroidal particle structure, when as nuclear material, because its particle diameter distribution is narrow, the Si-OH groups on surface and outside hydrogen bond have very strong reactivity, thus easily it is combined with multiple material by chemical bond and electrostatic interaction, shows the properties such as excellent light, electricity, magnetic.Simultaneously because spherical SiO2It is used as a significant advantage of core, you can by adjusting SiO2The size and shape of core simply and easily controls the size and pattern of resulting composite.Last decade is used as the popular direction of field of nanometer material technology, SiO2It is also more and more as the research of nuclear structure, but most research is all to lay particular emphasis on rare earth phosphor as clad, such as rare earth oxide, rare-earth vanadate, phosphate, other salts.And it is then few as the research of shell for rare earth organic fluorescent materials, yellow shake of University Of Qingdao et al. is by rare earth compounding Eu (TTA)3Phen·H2O is coated on SiO as shell2Outside, has obtained core-shell structure copolymer nano-complex enhanced compared with pure rare earth complex fluorescent；Xianmin Guo and Jean-Louis Canet et al. regard obtained DPAE-Si of DPA (clupanodonic acid) the derivative DPAE methane after silated as connection synthesis SiO2@Ln(DPAE–Si)3 (Ln= Eu3+
, Tb3+) core shell composite nano materials, it is modified by the surface for realizing amino, it can be applied in terms of biological nano mark.
Preparation for core-shell material has mainly have two methods at present, one is Direct precipitation, certain thickness shell is formed by the way that functional material is deposited directly into silicon dioxide microsphere surface, although this method can prepare core-shell material, but its reaction time is long, thickness is difficult to control, and the core-shell material prepared may disintegrate under ul-trasonic irradiation.Other method is to be connected silica kernel by the effect of chemical bond with outer layer functional material by silane coupler, and the core-shell material shell thickness being prepared out is easy to control, and chemical bond is not easy to break, Stability Analysis of Structures.Silane coupler is that (formula is RSiX to a kind of chemical organic compounds with double reactive functionalities3), R is carboxyl, dinitrogen etc. in molecular formula, can be with rare earth ion formation coordinate bond；X is the organic group that can be hydrolyzed, by the activity hydroxy hydrolytic condensation with nanoparticle surface, forms silicon oxygen bond and is connected to nanoparticle surface, such as methoxyl group, ethyoxyl.Generally speaking, silane coupler is during nanoparticle surface modified, can as bridge by two kinds of nature differences very big material securely it is continuous together, erected between kernel and outer layer functional material one " molecular bridge ".Silane coupler used herein is the phenanthroline of amino silane functionalization, it is one of current most widely used silane coupler, its advantage is that can be acted on by the dinitrogen in phenanthroline group and rare earth ion, prepare the rare earth compounding of good luminescence property, simultaneously because it has the part of amino silane, it can be hydrolyzed with the hydroxyl of silica surface, so as to reach the purpose of rare earth compounding cladding.In recent years, its application is focused primarily upon and synthesizes glass gels with TEOS reactions.Koen Binnemans and Philip Lenaerts in 2003 et al., which publishes an article, introduces phen-Si Eu-tta two-element match, adds after TEOS, synthesizes vitreous rare earth doped hybridized nanometer compound；Beta-diketon class rare earth compounding is synthesized rare-earth hybridized material by Jing Feng and Jiang-Bo Yu et al. using phen-Si characteristic, the problem of successfully solving chemically and thermally mechanical stability and mechanical strength.And the research that rare earth organic complex is coated on to the core-shell material of silicon ball outer layer for the modification by phen-Si is less.The work for summarizing forefathers is understood：Sulfoxide type complex has that fluorescence property is strong concurrently and preferable etc. the advantage of dissolubility, is a class application performance very high rare earth luminous complex, there is very much theoretical research value.
Plurality of advantages based on phen-Si and sulfoxide, the present invention uses SiO2Microballoon is kernel, using the method for self assembly by terbium perchlorate, adjacent carboxy phenyl carboxymethyl sulfoxide L, passes through phen-Si and SiO2Kernel chemistry, which is bonded, to be connected together, and prepares the SiO of different cladding thickness2@
Tb (phen-Si) L nuclear shell structure nano luminescent composites, and the test for the transmission electron microscope and luminescent properties for passing through each core-shell structure copolymer nano-complex, as a result show that core-shell material has good luminescent properties.And because the thickness of clad is in nanometer scale, reduce the consumption of rare earth, the cost reduction of material.It is significant for the excellent and with low cost rare earth organic fluorescent materials of following synthesis performance.
The content of the invention
The SiO with core shell structure is prepared it is an object of the invention to provide a kind of2@
The method of Tb (phen-Si) L rare earth organic fluorescent materialses.
The silicon dioxide microsphere of about 500nm particle diameters is prepared in the method that the mixed solvent of second alcohol and water is hydrolyzed with TEOS.
SiO2The method of modifying of microballoon：Using phen-Si as silane coupler, to SiO2Microballoon is modified, in phen-Si molecules-Si (OC2H5)
3Occur hydrolysis with the active silicone hydroxyl of silicon dioxide microsphere outer layer, then connect phen-Si with silicon ball chemical bond, make phen-Si modifications in silicon ball surface.By adjusting the ratio of silicon ball and phen-Si, the thickness of decorative layer can be readily adjusted.
Experimentation is as follows：With phen-Si, SiO2The ratio of core and ethanol is about 500nm silicon balls for 1g/1g/10ml ratio modification particle diameter.1.0g phen-Si are dissolved in 5ml absolute ethyl alcohols, separately by 1.0g SiO2Microballoon excusing from death is scattered in 5ml absolute ethyl alcohols, adds 5ml deionized waters, and phen-Si ethanol solution is slowly dropped into, magnetic agitation 2h by ammoniacal liquor regulation pH about 9 ~ 10.Centrifugation, is washed, and is dried, and is obtained the silicon ball that decorative layer thickness is 15nm, is expressed as SiO2(500)@
(Phen-Si) (15).With phen-Si, SiO2The ratio modification particle diameter that the ratio of core and ethanol is 0.1g/0.1g/10ml is about 500nm silicon balls.0.1g phen-Si are dissolved in 5ml absolute ethyl alcohols, separately by 0.1g SiO2Microballoon excusing from death is scattered in 5ml absolute ethyl alcohols, adds 5ml deionized waters, and phen-Si ethanol solution is slowly dropped into, magnetic agitation 2.5h by ammoniacal liquor regulation pH about 9 ~ 10.Centrifugation, washing obtains the silicon ball that decorative layer thickness is 65nm；It is expressed as SiO2(500)@(Phen-Si)(65)。
Two kinds of modification structures can clearly be seen that the decorative layer of outer layer amino silane.And the silicon ball smooth in appearance after modification, decorative layer size uniform, microballoon is spherical regular.
SiO2(500)@ (Phen-Si)
(20)And SiO2(500)@
(Phen-Si) (100)The preparation of nuclear shell structure nano luminescent composite：Silicon ball is modified by two kinds of certain mass（SiO2(500)@(Phen-Si)
(15)And SiO2(500)@
(Phen-Si) (65)）It is scattered in 20ml absolute ethyl alcohols, according to the amount of the material containing phen-Si, with phen-Si：Sulfoxide：The mol ratio of rare earth ion is 1:2:1 ratio, sulfoxide is slightly excessive, is first well mixed sulfoxide part with the silicon ball modified, and is heated to 80 DEG C, instills the ethanol solution of terbium perchlorate, reacts 0.5h, is cooled to after room temperature and centrifuges, wash, dries.Prepare two kinds of new SiO2(500)@
Tb(phen-Si)L(20)And SiO2(500)@ Tb(phen-Si)L(100)Nuclear shell structure nano luminescent composite.
Material preparation method of the present invention is simple, and equipment is simple, and low in raw material price, high-purity rare-earth consumption is few；The solvent used be water and ethanol, it is free from environmental pollution, be a kind of preferable friendly process the features such as save the energy, be easy to industrialized production, it is reproducible.
Brief description of the drawings：
Fig. 1 is SiO2@
The preparating mechanism of Tb (phen-Si) L nuclear shell structure nano luminescent composites
Fig. 2 is the scanning electron microscope (SEM) photograph of silicon dioxide microsphere：The particle diameter of silicon dioxide microsphere is 500nm, and the size uniform of silicon dioxide microsphere, smooth in appearance as seen from the figure.
Fig. 3 is the SiO that phen-Si is modified2The TEM figures of microballoon：As phen-Si, SiO2The ratio of core and ethanol be 1g/1g/10ml under conditions of, 500 nm SiO2The thickness that core is modified by phen-Si is 15 nanometers, is expressed as SiO2(500)@(Phen-Si)(15)。
Fig. 4 is the SiO that phen-Si is modified2The TEM figures of microballoon：As phen-Si, SiO2The ratio of core and ethanol be 0.1g/0.1g/10ml under conditions of, 500 nm SiO2The thickness that core is modified by phen-Si is expressed as SiO for 65 nanometers2(,500)@(
phen-Si) (65)。
Fig. 5 is SiO2(500)@Tb
(phen-Si) L(20)TEM figure.This it appears that the form of clad has obvious difference with Fig. 3 from figure, also, the thickness of clad has obvious increase compared with Fig. 3, illustrates that rare earth Sulfoxide coordination compound is connected to SiO by phen-Si2The surface of microballoon, forms the nuclear shell structure nano light-emitting composite using rare earth organic complex as clad.
Fig. 6 is SiO2(500)@ Tb
(phen-Si)L(100)TEM figure.This it appears that the form of clad has obvious difference with Fig. 4 from figure, also, the thickness of clad has obvious increase compared with Fig. 4, illustrates that rare earth Sulfoxide coordination compound is connected to SiO by phen-Si2The surface of microballoon, forms the nuclear shell structure nano light-emitting composite using rare earth organic complex as clad.
Fig. 7 is Tb (phen-Si)2·(ClO4)3·5H2O fluorescence emission spectrums：Test condition is that incident light and transmitting optical slits width are 2.0nm, excitation wavelength lambdaEXUnder conditions of 310nm, the launching light spectrogram of the sample of measure, as can be seen from the figure the sample is with stronger fluorescence property.
Fig. 8 is SiO2(500)@
Tb-Phen-Si-L(20)The fluorescence emission spectrogram of compound of nuclear shell structure nano light-emitting composite：Test condition is that incident light and transmitting optical slits width are 2.0nm, excitation wavelength lambdaEXUnder conditions of 310nm, the launching light spectrogram of the sample of measure, as can be seen from the figure complex of the fluorescent emission intensity of the sample much larger than Fig. 7, illustrates that the formation of core shell structure has and is beneficial to improve fluorescent emission intensity.
Embodiment：
Embodiment one
SiO2(500)@Tb(Phen-Si)L(20)
The preparation of nuclear shell structure nano light-emitting composite：With TEOS：Ethanol：Water：Ammoniacal liquor=0.5ml:5ml:2ml:0.65ml, mixes four kinds of solution, and the reaction time is 2 hours.Obtain 500nmSiO2Microballoon.1.0g.phen-Si is dissolved in 5ml absolute ethyl alcohols.The another 500nm by 1.0g. SiO2Microballoon excusing from death is scattered in 5ml absolute ethyl alcohols, adds 5ml deionized waters, and pH about 9 ~ 10 is adjusted with ammoniacal liquor.Phen-Si ethanol solution is slowly dropped into, magnetic agitation 2h.Centrifugation, is washed, and is dried, and it is the SiO that 15nm phen-Si are modified to prepare decorative layer thickness2Microballoon SiO2(500)@Phen-Si(15)；Above-mentioned modification silicon ball is dissolved in 5ml ethanol with phen-Si：Sulfoxide：Tb3+Mol ratio be 1:2:Sulfoxide part, is first well mixed by 1 ratio with the silicon ball modified, and is heated to 80 DEG C, instills the ethanol solution of terbium perchlorate, reacts 0.5h, is cooled to after room temperature and centrifuges, wash, dries.Prepare SiO2(500)@Tb(Phen-Si)
L(20)Nuclear shell structure nano light-emitting composite.
Embodiment two
SiO2(500)@
Tb(Phen-Si)L(100)The preparation of nuclear shell structure nano light-emitting composite：With TEOS：Ethanol：Water：Ammoniacal liquor=0.5ml:5ml:2ml:0.65ml, mixes four kinds of solution, and the reaction time is 2 hours.Obtain 500nmSiO2Microballoon.0.1g phen-Si are dissolved in 5ml absolute ethyl alcohols.The another 500nm by 0.1g SiO2Microballoon excusing from death is scattered in 5ml absolute ethyl alcohols, adds 5ml deionized waters, and pH about 9 ~ 10 is adjusted with ammoniacal liquor.Phen-Si ethanol solution is slowly dropped into, magnetic agitation 2.5h.Centrifugation, is washed, and is dried, and it is the SiO that 60nm phen-Si are modified to prepare decorative layer thickness2Microballoon SiO2(500)@Phen-Si(65)；Above-mentioned modification silicon ball is dissolved in 5ml ethanol with phen-Si：Sulfoxide：Tb3+Mol ratio be 1:2:Sulfoxide part, is first well mixed by 1 ratio with the silicon ball modified, and is heated to 75 DEG C, instills the ethanol solution of terbium perchlorate, reacts 1.0h, is cooled to after room temperature and centrifuges, wash, dries.Prepare SiO2(500)@Tb(Phen-Si)
L(100)Nuclear shell structure nano light-emitting composite.
Claims (3)
1. a kind of SiO2The synthetic method of@Tb (phen-Si) L nuclear shell structure nano luminescent composites, it is characterized in that with 500 nanometers of SiO2Microballoon is kernel, with phen-Si（Molecular formula is (phen)-N- (CONH (CH2)3Si(OCH2CH
3) 3)2）With adjacent carboxy phenyl carboxymethyl sulfoxide L（C6H4(COOH)SOCH2COOH）And the organic coordination compound of terbium perchlorate is clad, using first modifying SiO2The kernel method that self assembly coats rare earth compounding again, synthesizes SiO2(500)@
Tb(phen-Si)L (20)And SiO2(500)@ Tb(phen-Si)L (100)Core-shell type rare earth nano compound.
2.500 nanometers of SiO2The preparation of microballoon and method of modifying：TEOS adjusts basicity in the mixed solvent of second alcohol and water with ammoniacal liquor, and the silicon dioxide microsphere of hydrolytic condensation formation 500nm particle diameters, the specific consumption of reactant is as shown in the table：
Table 1 prepares the reaction condition of 500nm particle diameter silica
SiO2The method of modifying of microballoon：Using phen-Si, as silane coupler, to SiO2Microballoon is modified, in phen-Si molecules-Si (OC2H5)
3Occur hydrolysis with the active silicone hydroxyl of silicon dioxide microsphere outer layer, then connect phen-Si with silicon ball chemical bond, make phen-Si modifications in silicon ball surface, by adjusting the ratio of silicon ball and phen-Si, the thickness of decorative layer can be readily adjusted；Experimentation is as follows：With phen-Si, SiO2The ratio of core and ethanol is about 500nm silicon balls for 1g/1g/10ml ratio modification particle diameter；1.0g phen-Si are dissolved in 5ml absolute ethyl alcohols, separately by 1.0g
SiO2Microballoon excusing from death is scattered in 5ml absolute ethyl alcohols, adds 5ml deionized waters, and phen-Si ethanol solution is slowly dropped into, magnetic agitation 2h by ammoniacal liquor regulation pH about 9 ~ 10；Centrifugation, is washed, and is dried, standby, is prepared into the silicon ball that decorative layer thickness is 15nm, is expressed as SiO2(500)@（Phen-Si）(15)；With phen-Si, SiO2The ratio modification particle diameter that the ratio of core and ethanol is 0.1g/0.1g/10ml is about 500nm silicon balls；0.1g phen-Si are dissolved in 5ml absolute ethyl alcohols, separately by 0.1g SiO2Microballoon excusing from death is scattered in 5ml absolute ethyl alcohols, adds 5ml deionized waters, and phen-Si ethanol solution is slowly dropped into, magnetic agitation 2.5h by ammoniacal liquor regulation pH about 9 ~ 10；Centrifugation, is washed, and is dried, standby, is prepared into the silicon ball that decorative layer thickness is 65nm, is expressed as SiO2(500)@（Phen-Si）(65)。
3.SiO2(500)@
Tb(phen-Si)L (20)And SiO2(500)@ Tb(phen-Si)L (100)The preparation of nuclear shell structure nano luminescent composite：Silicon ball is modified by two kinds of certain mass（SiO2(500)@（Phen-Si）(15)And SiO2(500)@（Phen-Si）(65)）It is scattered in 20ml absolute ethyl alcohols, according to the amount of the material containing phen-Si, with phen-Si：Adjacent carboxy phenyl carboxymethyl sulfoxide L（(COOH)C6H4SOCH2COOH）：The mol ratio of rare earth ion is 1:2:1 ratio, sulfoxide is slightly excessive, is first well mixed sulfoxide part with the silicon ball modified, and is heated to 80 DEG C, instills the ethanol solution of terbium perchlorate, reacts 0.5h, is cooled to after room temperature and centrifuges, wash, dries, prepare two kinds of new SiO2(500)@
Tb(phen-Si)L(20)And SiO2(500)@ Tb(phen-Si)L(100)Nuclear shell structure nano luminescent composite.
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| CN107619661A (en) * | 2017-09-18 | 2018-01-23 | 复旦大学 | Interface self assembly rare earth compounding supermolecule fluorescence/chiral nano composite material and preparation method thereof |
| CN110642550A (en) * | 2019-10-10 | 2020-01-03 | 中国铁道科学研究院集团有限公司铁道建筑研究所 | Composite microsphere for improving early performance of cement-based material |
| CN112341502A (en) * | 2020-10-14 | 2021-02-09 | 内蒙古大学 | Preparation method of core-shell type rare earth complex |
| CN115181568A (en) * | 2022-06-21 | 2022-10-14 | 内蒙古大学 | Synthesis of multilayer core-shell structure composite nano dual-mode luminescent material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107619661A (en) * | 2017-09-18 | 2018-01-23 | 复旦大学 | Interface self assembly rare earth compounding supermolecule fluorescence/chiral nano composite material and preparation method thereof |
| CN110642550A (en) * | 2019-10-10 | 2020-01-03 | 中国铁道科学研究院集团有限公司铁道建筑研究所 | Composite microsphere for improving early performance of cement-based material |
| CN110642550B (en) * | 2019-10-10 | 2023-06-09 | 中国铁道科学研究院集团有限公司铁道建筑研究所 | Composite microsphere for improving early performance of cement-based material |
| CN112341502A (en) * | 2020-10-14 | 2021-02-09 | 内蒙古大学 | Preparation method of core-shell type rare earth complex |
| CN112341502B (en) * | 2020-10-14 | 2023-10-24 | 内蒙古大学 | Preparation method of core-shell rare earth complex |
| CN115181568A (en) * | 2022-06-21 | 2022-10-14 | 内蒙古大学 | Synthesis of multilayer core-shell structure composite nano dual-mode luminescent material |
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