CN108619115A - A kind of multi-functional hollow mesoporous SiO2The preparation method of nanocomposite - Google Patents
A kind of multi-functional hollow mesoporous SiO2The preparation method of nanocomposite Download PDFInfo
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- 239000002114 nanocomposite Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 28
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 26
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 26
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 26
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 26
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims abstract description 6
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 4
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 4
- 239000011248 coating agent Substances 0.000 claims abstract description 3
- 238000000576 coating method Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 235000019441 ethanol Nutrition 0.000 claims description 19
- 238000005406 washing Methods 0.000 claims description 15
- 239000012153 distilled water Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000000643 oven drying Methods 0.000 claims description 9
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 239000000908 ammonium hydroxide Substances 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000008103 glucose Substances 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 238000004821 distillation Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000004020 luminiscence type Methods 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 12
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 9
- 239000003814 drug Substances 0.000 description 8
- 229940079593 drug Drugs 0.000 description 5
- 238000005119 centrifugation Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000295 emission spectrum Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- JKGITWJSGDFJKO-UHFFFAOYSA-N ethoxy(trihydroxy)silane Chemical class CCO[Si](O)(O)O JKGITWJSGDFJKO-UHFFFAOYSA-N 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 229910009253 Y(NO3)3 Inorganic materials 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000013270 controlled release Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000005283 ground state Effects 0.000 description 1
- 210000000987 immune system Anatomy 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 239000002502 liposome Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000004736 wide-angle X-ray diffraction Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- BXJPTTGFESFXJU-UHFFFAOYSA-N yttrium(3+);trinitrate Chemical compound [Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O BXJPTTGFESFXJU-UHFFFAOYSA-N 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/51—Nanocapsules; Nanoparticles
- A61K9/5107—Excipients; Inactive ingredients
- A61K9/5115—Inorganic compounds
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K49/00—Preparations for testing in vivo
- A61K49/001—Preparation for luminescence or biological staining
- A61K49/0013—Luminescence
- A61K49/0017—Fluorescence in vivo
- A61K49/0019—Fluorescence in vivo characterised by the fluorescent group, e.g. oligomeric, polymeric or dendritic molecules
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K49/00—Preparations for testing in vivo
- A61K49/001—Preparation for luminescence or biological staining
- A61K49/0063—Preparation for luminescence or biological staining characterised by a special physical or galenical form, e.g. emulsions, microspheres
- A61K49/0069—Preparation for luminescence or biological staining characterised by a special physical or galenical form, e.g. emulsions, microspheres the agent being in a particular physical galenical form
- A61K49/0089—Particulate, powder, adsorbate, bead, sphere
- A61K49/0091—Microparticle, microcapsule, microbubble, microsphere, microbead, i.e. having a size or diameter higher or equal to 1 micrometer
- A61K49/0093—Nanoparticle, nanocapsule, nanobubble, nanosphere, nanobead, i.e. having a size or diameter smaller than 1 micrometer, e.g. polymeric nanoparticle
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- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Veterinary Medicine (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Biomedical Technology (AREA)
- Public Health (AREA)
- Nanotechnology (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Silicon Compounds (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses a kind of multi-functional hollow mesoporous SiO2The preparation method of nanocomposite, with Y2O3、Yb2O3And Er2O3Pass through Co deposited synthesis Y (OH) CO for raw material3:Then Yb, Er use hydro-thermal method in Y (OH) CO3:Yb, Er nuclear structure coated with carbon shell, then using sol-gal process in Y (OH) CO3:Yb, Er@C Surfaces are coating mesoporousmSiO2, it is finally synthesizing the Yb of hollow meso-hole structure2O3:Yb,Er@mSiO2；The hollow meso-hole structure luminescence generated by light nanocomposite with larger aperture and specific surface area can be prepared using this method.
Description
Technical field
The present invention relates to technical field of nano material, and in particular to a kind of to prepare Y2O3:Yb,Er@mSiO2Nano combined material
The method of material.
Background technology
Control medicament slow release is most important and has one of the research field of most attraction, for control drug storage volume and
Its release rate, carrier are most criticals.Last decade, this research has been obtained for great raising, in drug controlled release system
In, a large amount of organic system has been studied as pharmaceutical carrier, such as micelle, liposomes and polymer.However, these carriers
There are various limitations, such as poor thermal stability and chemical stability and the fast decoupled in immune system.Phase
Than under, Metaporous silicon dioxide material but has good biocompatibility, stable selectivity and no toxicity.In addition, it
Si (OH) can also be degraded in body4, Si (OH)4It can be excreted by kidney, therefore such material can be in pharmaceutical technology
It is widely used as adjuvant.
With larger specific surface area, ordered mesopore structure, adjustable aperture and pore volume, and the surface base that may modify
Group is all the more attractive feature of mesoporous material.These features are conducive to bioactive molecule and are embedded into pore structure,
Channel is provided for the diffusion after these molecules.Moreover, hollow mesoporous silica spheres possess high deposit due to its structure
Store up capacity；In addition, the hollow ball with mesoporous layer compared with traditional solid layer hollow ball, is opened up in extensive diffusion and transport
Good advantage is showed.Therefore hollow mesoporous silicon oxide has attracted more and more concerns in terms of medicament slow release.
Invention content
The purpose of the present invention is to provide a kind of multi-functional mesoporous Y of hollow-core construction2O3:Yb,Er@mSiO2 (wherein@is represented
Cladding,mRepresent mesoporous) preparation method of nanocomposite.
The technical solution adopted by the present invention to solve the technical problems is：A kind of multi-functional hollow mesoporous SiO2It is nano combined
The preparation method of material, nucleocapsid and material are configured to Y2O3:Yb,Er@mSiO2, step is
（1）Co deposited synthesis Y (OH) CO3:Yb,Er：
By Y2O3、Yb2O3And Er2O3It is dissolved in HNO respectively3Obtain Y (NO3)3、Yb(NO3)3With Er (NO3)3Solution, by the above solution
It is added in distilled water by a certain percentage, urea is then added and persistently stirs, then, said mixture is transferred in flask,
90 DEG C of 3 h of water-bath, finally, centrifuge washing are dried to obtain Y (OH) CO3:Yb,Er；
（2）Using hydro-thermal method in Y (OH) CO3:Yb, Er nuclear structure coated with carbon shell：
By Y (OH) CO3:Yb, Er are scattered in distilled water and ethyl alcohol, glucose is added, and centrifuge washing is dry after hydro-thermal reaction
To Y (OH) CO3:Yb,Er@C；
（3）Using sol-gal process in Y (OH) CO3:Yb, Er@C Surfaces are coating mesoporousmSiO2：
By Yb (OH) CO3:Yb, Er@C are scattered in ethyl alcohol and distilled water, and CTAB and ammonium hydroxide is added, positive silicic acid second is slowly added dropwise
Ester, stirs 6 h at room temperature, and centrifuge washing is dried to obtain Y (OH) CO3:Yb,Er@C@mSiO2；
（4）Synthesize the Yb of hollow meso-hole structure2O3:Yb,Er@mSiO2：
By Y obtained above (OH) CO3:Yb,Er@C@mSiO23 h are calcined in 800 DEG C of Muffle furnace, are removed carbon shell, are obtained
The Yb of hollow structure2O3:Yb,Er@mSiO2。
The multi-functional hollow mesoporous SiO of one kind2The preparation method of nanocomposite, step（1）In be mole
Than being 0.78:0.20:0.02 Y2O3,Yb2O3And Er2O3It is dissolved in a concentration of 2 mol L-1HNO3。
The multi-functional hollow mesoporous SiO of one kind2The preparation method of nanocomposite, step（1）Middle Y (NO3)3、
Yb(NO3)3With Er (NO3)3Solution is added in 200 ml distilled water, and 12.1 g urea are then added and continue to stir, after 2 h
It is then transferred in flask.
The multi-functional hollow mesoporous SiO of one kind2The preparation method of nanocomposite, step（1）In centrifugation
Dry washing is that solution is centrifuged with the speed of 4000 r/min, water and each washing of ethyl alcohol is used in combination three times, 60 DEG C of oven dryings 24
h。
The multi-functional hollow mesoporous SiO of one kind2The preparation method of nanocomposite, step（2）It is accurately to claim
Measure 0.2 g Y (OH) CO3:Yb, Er are scattered in 20 mL distilled water and 13 mL ethyl alcohol, are added 3.2 g glucose, are then held
It is continuous to be vigorously stirred 0.5 h.
The multi-functional hollow mesoporous SiO of one kind2The preparation method of nanocomposite, step（2）In hydro-thermal
Reaction is that reactant is transferred in 50 mL ptfe autoclaves, then 180 DEG C of 12 h of reaction.
The multi-functional hollow mesoporous SiO of one kind2The preparation method of nanocomposite, step（2）In centrifugation
Washing drying is centrifuged with the speed of 4000 r/min, is used in combination water and ethyl alcohol respectively to wash three times, then 60 DEG C of oven dryings 24
h。
The multi-functional hollow mesoporous SiO of one kind2The preparation method of nanocomposite, step（3）It is accurately to claim
Take 0.4 g Y (OH) CO3:Yb, Er@C are scattered in 100 mL ethyl alcohol and 150 mL distilled water, be then added 0.5 g CTAB and
A concentration of 1.0 mol L of 1 mL-1Ammonium hydroxide, then 200 μ L ethyl orthosilicates are slowly added dropwise.
The multi-functional hollow mesoporous SiO of one kind2The preparation method of nanocomposite, step（3）In centrifugation
Washing drying is centrifuged with the speed of 4000 r/min, is used in combination water and ethyl alcohol respectively to wash three times, then 60 DEG C of oven dryings 24
h。
The beneficial effects of the invention are as follows：
The present invention uses the hollow mesoporous knot of coprecipitation, hydro-thermal method and sol-gal process preparation uniform particle sizes, favorable dispersibility
The Y of structure2O3:Yb,Er@mSiO2Nanocomposite；Orderly mesoporous dioxy can be formed as surfactant using CTAB
SiClx layer is not only to introduce a large amount of functional molecular group to provide larger surface area, is also carried to absorb and encapsulating biomolecule
Larger aperture is supplied；By changing reactant quality and crystal growth time, can synthesize that size differs hollow has
Ordered meso-porous structure nanocomposite.
The nanocomposite of preparation has the characteristics that：
Material internal has cavity structure, can be used for storing high amount of drug molecule；Material surface has one layer of mesoporous silicon oxide
Layer can make the internal cavities of material pass through mesopore orbit with external environment and communicate with one another, it can be achieved that inside and outside mass exchange, is situated between in addition
Hole silica duct itself can also store high amount of drug molecule, be a kind of good slow releasing carrier of medication material；The composite wood
Material sends out strong up-conversion fluorescence under 980 nm exciting lights, can be used for the detection of medicament slow release process and curative effect；In experimentation
It is environmentally protective toxic products are not will produce, and experiment raw material are cheap, experimentation is simple and practicable, is easy to the life of experimental method
Production and popularization.
Description of the drawings
Fig. 1 is Y (OH) CO3:Yb,Er@C@mSiO2And Y2O3:Yb,Er@mSiO2@mSiO2X-ray diffraction spectrogram；
Fig. 2 is Y2O3:Yb,Er@mSiO2Transmission electron microscope photo；
Fig. 3 is Y2O3:Yb, Er and Y2O3:Yb,Er@mSiO2The up-conversion emission spectra of sample.
Specific implementation mode
Technical scheme of the present invention and effect are further described with reference to embodiment.But it is used specific
Method, formula and explanation are not limitation of the present invention.
Implementation process：
（1）Co deposited synthesis Y (OH) CO3:Yb,Er。
Molar ratio 0.78:0.20:0.02 Y2O3,Yb2O3And Er2O3It is dissolved in a concentration of 2mol L-1HNO3In.It obtains
Y(NO3)3、Yb(NO3)3With Er (NO3)3Solution is added in 200 ml distilled water.The urea of 12.1 g is then added and persistently stirs
It mixes.Said mixture is transferred in flask after 2 h, 90 DEG C of 3 h of water-bath.Finally, 4000 r/min of solution after reaction from
The heart, water and ethyl alcohol is used in combination, and respectively three times, 60 DEG C of 24 h of oven drying obtain Y (OH) CO for washing3:Yb,Er。
（2）Using hydro-thermal method in Y (OH) CO3:Yb, Er coated with carbon shell.
Y (OH) CO on 0.2 g of precise3:Yb, Er are scattered in 20 mL distilled water and 13 mL ethyl alcohol, are added certain
The glucose of amount, continuing vigorous stir 0.5 h, then above-mentioned reactant are transferred in 50 mL ptfe autoclaves,
180 DEG C of 12 h of reaction.Finally, 4000 r/min are centrifuged, and water and ethyl alcohol is used in combination respectively to wash three times, 60 DEG C of 24 h of oven drying,
Obtain Y (OH) CO3:Yb,Er@C。
（3）Synthesize Y (OH) CO3:Yb,Er@C@SiO2。
Accurately weigh 0.4 g Y (OH) CO3:Yb, Er@C are scattered in 100 mL ethyl alcohol and 150 mL distilled water.It is added
A concentration of 1.0 molL of 0.5 g CTAB and 1 mL‒1Ammonium hydroxide, 200 μ L ethyl orthosilicates are slowly added dropwise, stir 6 h at room temperature.
Finally, 4000 r/min are centrifuged, and water and ethyl alcohol is used in combination, and respectively three times, 60 DEG C of 24 h of oven drying obtain Y (OH) CO for washing3:Yb,
Er@C@mSiO2。
（4）Synthesize hollow structure Y2O3:Yb,Er@mSiO2。
By above-mentioned Y (OH) CO obtained by the reaction3:Yb,Er@C@mSiO23 h are calcined in 800 DEG C of Muffle furnace, are burnt
Carbon shell obtains the Y of hollow structure2O3:Yb,Er@mSiO2。
Fig. 1 is the Wide angle X-ray diffraction figure of sample, and JCPDS 25-1011 is standard card；Before roasting being determined by figure
Be mutually unformed phase.And for Y2O3:Yb,Er@mSiO2It may be seen that in 2 θ=29.2 °, 33.4 °, 48.5 ° and 57 °
There are four sharp peaks at place, are Y2O3Characteristic peak and Y2O3Standard X-ray diffraction card (JCPDS No.25-1011) is compared
Their relative intensity position and diffraction locations are consistent, it can be seen that there is no miscellaneous for the powder roasted under the conditions of 800 DEG C
It mutually generates, at 2 θ=22 °, unformed SiO can be attributed to herein2Characteristic peak（JCPDS 29–0085）.It can be said that
Bright SiO2It is successfully coated to powder surface, and 2 θ=29.2 °, 33.4 °, 48.5 ° and 57 ° four sharp peaks show SiO2
Cladding the crystal structure of powder is not influenced.
As shown in Fig. 2, the material size is uniform, agglomeration does not occur.We can observe that being in the outer of ball
One layer of color is than dark shell, for apparent hollow core-shell structure.
Fig. 3 is respectively Y2O3:Yb, Er and Y2O3:Yb,Er@mSiO2The up-conversion emission spectra of sample.In 980nm laser
Under the excitation of device, sample shows stronger green light and red emission.It can see from figure AH-Y2O3:There are three for Yb, Er sample
A different Er3+Characteristic emission peak results between 520nm to 538nm when green emission between 540nm and 560nm
Er3+'s2H11/2It arrives4I15/2With4S3/2It arrives4I15/2Transition, the red emission between 640nm to 680nm be due to4F9/2It arrives4I15/2Transition.I.e. under 980nm excitations, Er3+Ground state electron by absorb a photon be excited to4I11/2Energy level is being inhaled
Second photon is received further to be energized into4F7/2Energy level, the energy level are located at visible light region, Er3+Pass through quick phonon damping mistake
Journey nonradiative relaxation arrives2H11/2With4S3/2Energy level generates2H11/2It arrives4I15/2With4S3/2It arrives4I115/2Green emission, electronics can be into
One step relaxation, layout arrive4F9/2Energy level generates4F9/2It arrives4I15/2Red emission.Scheming B isH-Y2O3:Yb,Er@mSiO2Sample
Upper conversion emission spectrum, from figure it may be seen that in addition to the intensity of emission peak does not have any change by significantly reducing outer figure
Change, this is coated Si O2It is caused.
The above-described embodiments merely illustrate the principles and effects of the present invention, and the embodiment that part uses, for
For those skilled in the art, without departing from the concept of the premise of the invention, can also make it is several deformation and
It improves, these are all within the scope of protection of the present invention.
Claims (9)
1. a kind of multi-functional hollow mesoporous SiO2The preparation method of nanocomposite, it is characterised in that：Step is
（1）Co deposited synthesis Y (OH) CO3:Yb,Er：
By Y2O3、Yb2O3And Er2O3It is dissolved in HNO respectively3Obtain Y (NO3)3、Yb(NO3)3With Er (NO3)3Solution presses the above solution
Certain proportion is added in distilled water, and urea is then added and persistently stirs, then, said mixture is transferred in flask, 90
DEG C 3 h of water-bath, finally, centrifuge washing is dried to obtain Y (OH) CO3:Yb,Er；
（2）Using hydro-thermal method in Y (OH) CO3:Yb, Er nuclear structure coated with carbon shell：
By Y (OH) CO3:Yb, Er are scattered in distilled water and ethyl alcohol, and glucose is added, and centrifuge washing is dried to obtain after hydro-thermal reaction
Y(OH)CO3:Yb,Er@C；
（3）Using sol-gal process in Y (OH) CO3:Yb, Er@C Surfaces are coating mesoporousmSiO2：
By Yb (OH) CO3:Yb, Er@C are scattered in ethyl alcohol and distilled water, and CTAB and ammonium hydroxide is added, positive silicic acid second is slowly added dropwise
Ester, stirs 6 h at room temperature, and centrifuge washing is dried to obtain Y (OH) CO3:Yb,Er@C@mSiO2；
（4）Synthesize the Yb of hollow meso-hole structure2O3:Yb,Er@mSiO2：
By Y obtained above (OH) CO3:Yb,Er@C@mSiO23 h are calcined in 800 DEG C of Muffle furnace, are removed carbon shell, are obtained
The Yb of hollow structure2O3:Yb,Er@mSiO2。
2. the multi-functional hollow mesoporous SiO of one kind according to claim 12The preparation method of nanocomposite, feature exist
In the step（1）In be molar ratio be 0.78:0.20:0.02 Y2O3,Yb2O3And Er2O3It is dissolved in a concentration of 2 mol L-1
HNO3。
3. the multi-functional hollow mesoporous SiO of one kind according to claim 22The preparation method of nanocomposite, feature exist
In the step（1）Middle Y (NO3)3、Yb(NO3)3With Er (NO3)3Solution is added in 200 ml distilled water, is then added
12.1 g urea simultaneously continue to stir, and are then transferred in flask after 2 h.
4. the multi-functional hollow mesoporous SiO of one kind according to claim 32The preparation method of nanocomposite, feature exist
In the step（1）In centrifuge washing drying be that solution is centrifuged with the speed of 4000 r/min, be used in combination water and ethyl alcohol respectively to wash
It washs three times, 60 DEG C of 24 h of oven drying.
5. the multi-functional hollow mesoporous SiO of one kind according to claim 12The preparation method of nanocomposite, feature exist
In the step（2）It is precise 0.2 g Y (OH) CO3:Yb, Er are scattered in 20 mL distilled water and 13 mL ethyl alcohol,
3.2 g glucose are added, then continuing vigorous stirs 0.5 h.
6. the multi-functional hollow mesoporous SiO of one kind according to claim 52The preparation method of nanocomposite, feature exist
In the step（2）In hydro-thermal reaction be that reactant is transferred in 50 mL ptfe autoclaves, then 180
DEG C reaction 12 h.
7. the multi-functional hollow mesoporous SiO of one kind according to claim 62The preparation method of nanocomposite, feature exist
In the step（2）In centrifuge washing drying be to be centrifuged with the speed of 4000 r/min, be used in combination water and ethyl alcohol respectively to wash three
It is secondary, then 60 DEG C of 24 h of oven drying.
8. the multi-functional hollow mesoporous SiO of one kind according to claim 12The preparation method of nanocomposite, feature exist
In the step（3）It is accurately to weigh 0.4 g Y (OH) CO3:Yb, Er@C are scattered in 100 mL ethyl alcohol and 150 mL distillations
In water, a concentration of 1.0 mol L of 0.5 g CTAB and 1 mL are then added-1Ammonium hydroxide, then the positive silicic acid second of 200 μ L is slowly added dropwise
Ester.
9. the multi-functional hollow mesoporous SiO of one kind according to claim 82The preparation method of nanocomposite, feature exist
In the step（3）In centrifuge washing drying be to be centrifuged with the speed of 4000 r/min, be used in combination water and ethyl alcohol respectively to wash three
It is secondary, then 60 DEG C of 24 h of oven drying.
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| CN104587471A (en) * | 2014-12-25 | 2015-05-06 | 哈尔滨工程大学 | Functional hollow mesoporous SiO2 nanometer composite material and preparation method thereof |
| CN105271266A (en) * | 2015-10-21 | 2016-01-27 | 哈尔滨工程大学 | Preparation method of multifunctional mesoporous Gd-Si-Ce6 nanocomposite with core-shell structure |
| CN108054387A (en) * | 2017-12-04 | 2018-05-18 | 五行科技股份有限公司 | A kind of preparation method of the hollow multinuclear nano catalytic material of palladium-mesopore silicon oxide |
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| EP0747034A1 (en) * | 1995-06-08 | 1996-12-11 | Vita Zahnfabrik H. Rauter GmbH & Co. KG | Powder mixture for the preparation of a paste of opaque material |
| CN104587471A (en) * | 2014-12-25 | 2015-05-06 | 哈尔滨工程大学 | Functional hollow mesoporous SiO2 nanometer composite material and preparation method thereof |
| CN105271266A (en) * | 2015-10-21 | 2016-01-27 | 哈尔滨工程大学 | Preparation method of multifunctional mesoporous Gd-Si-Ce6 nanocomposite with core-shell structure |
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