CN108619115B - Multifunctional hollow mesoporous SiO2Process for preparing nano composite material - Google Patents
Multifunctional hollow mesoporous SiO2Process for preparing nano composite material Download PDFInfo
- Publication number
- CN108619115B CN108619115B CN201810712494.4A CN201810712494A CN108619115B CN 108619115 B CN108619115 B CN 108619115B CN 201810712494 A CN201810712494 A CN 201810712494A CN 108619115 B CN108619115 B CN 108619115B
- Authority
- CN
- China
- Prior art keywords
- sio
- ethanol
- water
- mesoporous
- hollow mesoporous
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000000463 material Substances 0.000 title claims abstract description 20
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 41
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 35
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 35
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 35
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 15
- 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
- 239000011248 coating agent Substances 0.000 claims abstract description 7
- 238000000576 coating method Methods 0.000 claims abstract description 7
- 238000000975 co-precipitation Methods 0.000 claims abstract description 5
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims abstract description 5
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000003980 solgel method Methods 0.000 claims abstract description 4
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 4
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 14
- 239000012153 distilled water Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 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 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 238000004090 dissolution Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000003814 drug Substances 0.000 description 7
- 229940079593 drug Drugs 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 239000010410 layer Substances 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- 238000000295 emission spectrum Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000000643 oven drying Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000013268 sustained release Methods 0.000 description 2
- 239000012730 sustained-release form Substances 0.000 description 2
- 229910007156 Si(OH)4 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 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
- 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 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000005283 ground state Effects 0.000 description 1
- 210000000987 immune system Anatomy 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 239000002502 liposome Substances 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000007787 solid 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
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000004736 wide-angle X-ray diffraction Methods 0.000 description 1
Images
Classifications
-
- 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
Landscapes
- 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 multifunctional hollow mesoporous SiO2Process for preparing nanocomposites with Y2O3、Yb2O3And Er2O3Synthesis of Y (OH) CO by coprecipitation method for raw material3Yb, Er, then hydrothermally in Y (OH) CO3Coating a carbon shell on the surface of a Yb and Er core structure, and coating Y (OH) CO by a sol-gel method3Yb, Er @ C surface-coated mesoporousmSiO2Finally synthesizing Y with hollow mesoporous structure2O3:Yb,Er@mSiO2(ii) a The method can be used for preparing the photoluminescent nanocomposite material with the hollow mesoporous structure and larger aperture and specific surface area.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a method for preparing Y2O3:Yb,Er@mSiO2A method of making a nanocomposite.
Background
Controlling drug sustained release is one of the most important and attractive areas of research, and the carrier is most critical for controlling the drug storage capacity and its release rate. This research has been greatly enhanced in the last decade, and a large number of organic systems have been investigated as drug carriers in drug delivery systems, such as micelles, liposomes and polymers. However, these carriers have various limitations such as poor thermal and chemical stability and rapid decomposition in the immune system. CompareIn contrast, mesoporous silica materials have good biocompatibility, stable selectivity and no toxicity. In addition, it is degraded in the body to Si (OH)4,Si(OH)4Can be discharged out of the body through the kidney, so the material can be widely used as an adjuvant in pharmaceutical technology.
The mesoporous material has the characteristics of large specific surface area, ordered mesoporous structure, adjustable pore diameter and pore volume, and modifiable surface groups, which are attractive characteristics. These features facilitate the insertion of bioactive molecules into the pore structure and also provide a pathway for the subsequent diffusion of these molecules. Moreover, the hollow mesoporous silica spheres have high storage capacity due to the structure thereof; in addition, the hollow sphere with the mesoporous layer exhibits great advantages in large-scale diffusion and transportation compared to the conventional solid layer hollow sphere. Therefore, the hollow mesoporous silica attracts more and more attention in the aspect of drug slow release.
SUMMERY OF THE UTILITY MODEL
The invention aims to provide a hollow-structure multifunctional mesoporous Y2O3:Yb,Er@mSiO2 (wherein @ represents a coating layer,mrepresenting mesopores) nanocomposite.
The technical scheme adopted by the invention for solving the technical problems is as follows: multifunctional hollow mesoporous SiO2Preparation method of nano composite material, core-shell structure and material composition thereof are Y2O3:Yb,Er@mSiO2The steps are as follows
(1) Coprecipitation method for synthesizing Y (OH) CO3:Yb,Er:
Will Y2O3、Yb2O3And Er2O3Respectively dissolved in HNO3To obtain Y (NO)3)3、Yb(NO3)3And Er (NO)3)3Adding the solution into distilled water according to a certain proportion, adding urea, continuously stirring, transferring the mixture into a flask, reacting in a water bath at 90 ℃ for 3 h, and finally centrifuging, washing and drying to obtain Y (OH) CO3:Yb,Er;
(2) By hydrothermal method on Y (OH) CO3Coating a carbon shell on the surface of a Yb and Er core structure:
by reacting Y (OH) CO3Yb and Er are dispersed in distilled water and alcohol, glucose is added, and Y (OH) CO is obtained by centrifugal washing and drying after hydrothermal reaction3:Yb,Er@C;
(3) By sol-gel method on Y (OH) CO3Yb, Er @ C surface-coated mesoporousmSiO2:
Mixing Yb (OH) CO3Yb, Er @ C are dispersed in ethanol and distilled water, CTAB and ammonia water are added, tetraethoxysilane is slowly dripped, the mixture is stirred for 6 hours at room temperature, and Y (OH) CO is obtained by centrifugal washing and drying3:Yb,Er@C@mSiO2;
(4) Synthesis of Yb with hollow mesoporous structure2O3:Yb,Er@mSiO2:
The Y (OH) CO obtained above is reacted3:Yb,Er@C@mSiO2Calcining in a muffle furnace at 800 ℃ for 3 h, removing the carbon shell to obtain Y with a hollow structure2O3:Yb,Er@mSiO2。
The multifunctional hollow mesoporous SiO2A process for producing a nanocomposite, wherein in the step (1), Y is used in a molar ratio of 0.78:0.20:0.022O3,Yb2O3And Er2O3Dissolved in 2mol L-1HNO of (2)3。
The multifunctional hollow mesoporous SiO2Process for the preparation of a nanocomposite, wherein in step (1) Y (NO)3)3、Yb(NO3)3And Er (NO)3)3The solution was added to 200 ml of distilled water, followed by 12.1 g of urea and continued stirring, and after 2 h was transferred to the flask.
The multifunctional hollow mesoporous SiO2The preparation method of the nano composite material comprises the steps of centrifuging, washing and drying the solution in the step (1) at the speed of 4000 r/min, washing the solution with water and ethanol for three times respectively, and drying the solution in an oven at the temperature of 60 ℃ for 24 hours.
The multifunctional hollow mesoporous SiO2Nano composite materialThe preparation method of the material comprises the step (2) of accurately weighing 0.2 g Y (OH) CO3Yb and Er were dispersed in 20 mL of distilled water and 13 mL of ethanol, and 3.2 g of glucose was added, followed by continuous vigorous stirring for 0.5 h.
The multifunctional hollow mesoporous SiO2The hydrothermal reaction in the step (2) is to transfer the reactants into a 50 mL polytetrafluoroethylene reaction kettle and then react for 12 h at 180 ℃.
The multifunctional hollow mesoporous SiO2The preparation method of the nano composite material comprises the steps of centrifuging, washing and drying in the step (2) at the speed of 4000 r/min, washing with water and ethanol for three times respectively, and drying in an oven at the temperature of 60 ℃ for 24 hours.
The multifunctional hollow mesoporous SiO2The preparation method of the nano composite material comprises the step (3) of accurately weighing 0.4 g Y (OH) CO3Yb, Er @ C was dispersed in 100 mL of ethanol and 150 mL of distilled water, followed by addition of 0.5 g of CTAB and 1 mL of 1.0 mol L-1Then 200. mu.L of ethyl orthosilicate was slowly added dropwise.
The multifunctional hollow mesoporous SiO2The preparation method of the nano composite material comprises the steps of centrifuging, washing and drying in the step (3) at the speed of 4000 r/min, washing with water and ethanol for three times respectively, and drying in an oven at the temperature of 60 ℃ for 24 hours.
The invention has the beneficial effects that:
the invention adopts a coprecipitation method, a hydrothermal method and a sol-gel method to prepare Y with a hollow mesoporous structure with uniform particle size and good dispersibility2O3:Yb,Er@mSiO2A nanocomposite; CTAB is adopted as a surfactant to form an ordered mesoporous silicon dioxide layer, so that a large surface area is provided for introducing a large amount of functional molecular groups, and a large aperture is provided for absorbing and encapsulating biomolecules; by changing the quality of the reactants and the crystal growth time, the hollow ordered mesoporous structure nano composite material with different sizes can be synthesized.
The prepared nano composite material has the following characteristics:
the material has a cavity structure inside, and can be used for storing a large number of drug molecules; the surface of the material is provided with a mesoporous silica layer, so that an internal cavity of the material can be communicated with the external environment through a mesoporous pore canal, the exchange of internal and external substances can be realized, and in addition, the mesoporous silica pore canal can also store a large amount of drug molecules, so that the mesoporous silica material is a good drug sustained-release carrier material; the composite material emits strong up-conversion fluorescence under 980nm exciting light, and can be used for detecting the slow release process and the curative effect of the drug; toxic products are not generated in the experimental process, the environmental protection is realized, the experimental raw materials are low in price, the experimental process is simple and easy to implement, and the production and popularization of the experimental method are easy.
Drawings
FIG. 1 shows Y (OH) CO3:Yb,Er@C@mSiO2And Y2O3:Yb,Er@mSiO2@mSiO2X-ray diffraction pattern of (a);
FIG. 2 is Y2O3:Yb,Er@mSiO2Transmission electron microscope photograph of (1);
FIG. 3 is Y2O3Yb, Er and Y2O3:Yb,Er@mSiO2The upconversion emission spectrum of the sample.
Detailed Description
The technical solution and effects of the present invention will be further described with reference to the following examples. However, the specific methods, formulations and descriptions used are not intended to be limiting.
The implementation process comprises the following steps:
(1) coprecipitation method for synthesizing Y (OH) CO3:Yb,Er。
Y in a molar ratio of 0.78:0.20:0.022O3,Yb2O3And Er2O3Dissolved in 2mol L-1HNO of (2)3In (1). Obtained Y (NO)3)3、Yb(NO3)3And Er (NO)3)3The solution was added to 200 ml of distilled water. 12.1 g of urea are subsequently added and stirring is continued. After 2 h, the mixture was transferred to a flask and reacted in a water bath at 90 ℃ for 3 h. Finally, the reacted solution is centrifuged at 4000 r/min, washed with water and ethanol three times respectively, and dried in an oven at 60 ℃ for 24 hoursTo obtain Y (OH) CO3:Yb,Er。
(2) By hydrothermal method on Y (OH) CO3The surface of Yb and Er is coated with a carbon shell.
Accurately weigh 0.2 g of above Y (OH) CO3Yb and Er are dispersed in 20 mL of distilled water and 13 mL of ethanol, a certain amount of glucose is added, the mixture is continuously stirred vigorously for 0.5 h, and then the reactants are transferred into a 50 mL polytetrafluoroethylene reaction kettle and reacted for 12 h at 180 ℃. Finally, centrifuging at 4000 r/min, washing with water and ethanol for three times respectively, and oven-drying at 60 deg.C for 24 hr to obtain Y (OH) CO3:Yb,Er@C。
(3) Synthesis of Y (OH) CO3:Yb,Er@C@SiO2。
Accurately weighing 0.4 g Y (OH) CO3Yb, Er @ C was dispersed in 100 mL of ethanol and 150 mL of distilled water. 0.5 g CTAB and 1 mL of 1.0 mol L‒1200 mu.L of ethyl orthosilicate is slowly dropped into the ammonia water, and the mixture is stirred for 6 hours at room temperature. Finally, centrifuging at 4000 r/min, washing with water and ethanol for three times respectively, and oven-drying at 60 deg.C for 24 hr to obtain Y (OH) CO3:Yb,Er@C@mSiO2。
(4) Synthetic hollow structure Y2O3:Yb,Er@mSiO2。
Y (OH) CO obtained by the above reaction3:Yb,Er@C@mSiO2Calcining in a muffle furnace at 800 ℃ for 3 h, burning off the carbon shell to obtain Y with a hollow structure2O3:Yb,Er@mSiO2。
FIG. 1 is a wide angle X-ray diffraction pattern of a sample, JCPDS 25-1011 being a standard card; from the figure, it can be confirmed that the phases before firing are all amorphous phases. And for Y2O3:Yb,Er@mSiO2We can see four sharp peaks at 2 θ =29.2 °, 33.4 °, 48.5 ° and 57 °, being Y2O3Characteristic peak of (2), and Y2O3The relative intensity position and diffraction position of the standard X-ray diffraction card (JCPDS No.25-1011) are consistent, so that the powder calcined at 800 ℃ does not generate impurity phase, and can be classified as amorphous SiO at 2 theta =22 DEG2Characteristic peak of (JCPDS 29-0085). ByThis can explain SiO2The coating to the powder surface has been successful, and four sharp peaks of 2 theta =29.2 °, 33.4 °, 48.5 ° and 57 ° indicate SiO2The coating of (2) has no influence on the crystal structure of the powder.
As shown in FIG. 2, the material was uniform in size and no agglomeration occurred. We can observe that there is a layer of darker shell around the sphere, which is an obvious hollow shell-core structure.
FIG. 3 is Y2O3Yb, Er and Y2O3:Yb,Er@mSiO2The upconversion emission spectrum of the sample. Under excitation of a 980nm laser, the sample showed strong green and red light emission. From FIG. A, it can be seen thatH-Y2O3Yb, Er samples present three different Er3+Characteristic emission peaks, generated in Er at green emission between 520nm and 538nm and between 540nm and 560nm3+Is/are as follows2H11/2To4I15/2And4S3/2to4I15/2The red light emission between 640nm and 680nm is due to4F9/2To4I15/2And (4) transition. I.e. Er under excitation of 980nm3+Is excited to the ground state electron by absorbing a photon4I11/2Energy level, further excited upon absorption of a second photon4F7/2Energy level in the visible region, Er3+Non-radiative relaxation by rapid phonon decay processes to2H11/2And4S3/2energy level, generation2H11/2To4I15/2And4S3/2to4I115/2Green emission, electrons can be further relaxed and arranged to4F9/2Energy level, generation4F9/2To4I15/2Red light emission of (a). FIG. B isH-Y2O3:Yb,Er@mSiO2The up-conversion emission spectrum of the sample, from which we can see that there is no change in the pattern except for the significant decrease in the intensity of the emission peak, which is the coating SiO2The result is.
The above-described embodiments are merely illustrative of the principles and effects of the present invention, and some embodiments may be applied, and it will be apparent to those skilled in the art that various changes and modifications may be made without departing from the inventive concept of the present invention, and these embodiments are within the scope of the present invention.
Claims (1)
1. Multifunctional hollow mesoporous SiO2The preparation method of the nano composite material is characterized by comprising the following steps: comprises the steps of
(1) Coprecipitation method for synthesizing Y (OH) CO3:Yb,Er:
Mixing Y with the molar ratio of 0.78:0.20:0.022O3,Yb2O3And Er2O3The dissolution concentration is 2 mol.L-1HNO of (2)3To obtain Y (NO)3)3、Yb(NO3)3And Er (NO)3)3Adding the solution into 200 ml of distilled water according to a certain proportion, then adding 12.1 g of urea and continuously stirring, transferring into a flask after 2 h, carrying out water bath reaction at 90 ℃ for 3 h, and finally, centrifuging, washing and drying to obtain Y (OH) CO3Yb, Er; the centrifugal washing and drying is that the solution is centrifuged at the speed of 4000 r/min, and is washed by water and ethanol for three times respectively, and is dried in an oven at the temperature of 60 ℃ for 24 hours;
(2) by hydrothermal method on Y (OH) CO3Coating a carbon shell on the surface of a Yb and Er core structure:
accurately weigh 0.2 g Y (OH) CO3Yb and Er are dispersed in 20 mL of distilled water and 13 mL of ethanol, then 3.2 g of glucose is added, then the mixture is continuously and vigorously stirred for 0.5 h, the reactant is transferred into a 50 mL of polytetrafluoroethylene reaction kettle, then the reaction is carried out for 12 h at 180 ℃, then the reaction is centrifuged at the speed of 4000 r/min and is respectively washed with water and ethanol for three times, and then the reaction product is dried in an oven at 60 ℃ for 24 h to obtain Y (OH) CO3:Yb,Er@C;
(3) By sol-gel method on Y (OH) CO3Yb, Er @ C surface-coated mesoporousmSiO2:
Accurately weighing 0.4 g Y (OH) CO3Yb, Er @ C was dispersed in 100 mL of ethanol and 150 mL of distilled water, followed by addition of 0.5 g of CTAB and 1 mL of 1.0 mol · L-1Slowly dropwise adding 200 mu L of tetraethoxysilane, stirring at room temperature for 6 h, centrifuging at the speed of 4000 r/min, washing with water and ethanol for three times respectively, and drying in an oven at 60 ℃ for 24 h to obtain Y (OH) CO3:Yb,Er@C@mSiO2;
(4) Synthesis of Yb with hollow mesoporous structure2O3:Yb,Er@mSiO2:
The Y (OH) CO obtained above is reacted3:Yb,Er@C@mSiO2Calcining in a muffle furnace at 800 ℃ for 3 h, removing the carbon shell to obtain Y with a hollow structure2O3:Yb,Er@mSiO2。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810712494.4A CN108619115B (en) | 2018-06-29 | 2018-06-29 | Multifunctional hollow mesoporous SiO2Process for preparing nano composite material |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810712494.4A CN108619115B (en) | 2018-06-29 | 2018-06-29 | Multifunctional hollow mesoporous SiO2Process for preparing nano composite material |
Publications (2)
Publication Number | Publication Date |
---|---|
CN108619115A CN108619115A (en) | 2018-10-09 |
CN108619115B true CN108619115B (en) | 2021-04-23 |
Family
ID=63689398
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201810712494.4A Active CN108619115B (en) | 2018-06-29 | 2018-06-29 | Multifunctional hollow mesoporous SiO2Process for preparing nano composite material |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN108619115B (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN116002620A (en) * | 2023-01-13 | 2023-04-25 | 中国核动力研究设计院 | Erbium-containing yttrium hydride material and preparation method thereof |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0747034B1 (en) * | 1995-06-08 | 2001-08-16 | 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 |
CN105271266B (en) * | 2015-10-21 | 2017-09-08 | 哈尔滨工程大学 | The preparation method of the multi-functional mesoporous nano composite materials of Gd Si Ce6 of core shell structure |
CN108054387B (en) * | 2017-12-04 | 2020-03-24 | 五行科技股份有限公司 | Preparation method of palladium-mesoporous silica hollow multi-core nano catalytic material |
-
2018
- 2018-06-29 CN CN201810712494.4A patent/CN108619115B/en active Active
Also Published As
Publication number | Publication date |
---|---|
CN108619115A (en) | 2018-10-09 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Yang et al. | Uniform hollow Lu2O3: Ln (Ln= Eu3+, Tb3+) spheres: facile synthesis and luminescent properties | |
CN107151029B (en) | A kind of sol-gel self-combustion synthesis preparation process of tetra phase barium titanate powder | |
CN102350281A (en) | Preparation method of fluorescent mesoporous silica-based core-shell nanoscale capsule | |
CN102728848A (en) | Method of producing silver nanowires in large quantities | |
CN104587471A (en) | Functional hollow mesoporous SiO2 nanometer composite material and preparation method thereof | |
CN102874823A (en) | Method for preparing silicon dioxide hollow microspheres with uniform shape by taking pollen grains as biological template | |
CN105623663A (en) | Red up-conversion luminous nano-carrier and preparation method | |
CN106811832A (en) | A kind of pearl-decorated curtain shape BiFeO3The preparation method and products obtained therefrom of micro nanometer fiber | |
CN112391167A (en) | Rare earth doped ternary metal fluoride NaCaLnF6And preparation method of heterogeneous isomorphic material thereof | |
JP4759661B2 (en) | Silica nanofiber / metal oxide nanocrystal composite and production method thereof | |
Choma et al. | Carbon–gold core–shell structures: Formation of shells consisting of gold nanoparticles | |
CN108619115B (en) | Multifunctional hollow mesoporous SiO2Process for preparing nano composite material | |
JP2007290887A (en) | Bismuth titanate-based nanoparticle, piezoelectric ceramic using the same, and methods for producing them | |
Liu et al. | Large-scale fabrication of H2 (H2O) Nb2O6 and Nb2O5 hollow microspheres | |
CN102134105B (en) | Method for accessorily preparing nanometer cobaltosic oxide granules at room temperature by utilizing amino acids | |
CN107603623A (en) | A kind of small size β NaREF4The preparation method of fluorescent material | |
CN107416843B (en) | A kind of silica yolk-eggshell structural material of the flower-shaped kernel containing big spacing and preparation method thereof | |
CN105948117A (en) | Hydrothermal method for preparing HfO2 nano-particles | |
CN111151242B (en) | Preparation method of cerium-manganese metal ion modified aluminate photocatalyst | |
RU2323876C1 (en) | METHOD FOR MANUFACTURING METAL-CARBON NANOSTRUCTURES BY REACTING ORGANIC COMPOUNDS WITH SALTS OF d-METALS | |
KR100488100B1 (en) | Mesoporous transition metal oxide thin film and powder and preparation thereof | |
CN112194178B (en) | Titanium dioxide and Prussian blue ordered assembly state mesomorphic nano material and preparation method thereof | |
CN113980677A (en) | g-C3N4Quantum dot and preparation method thereof | |
CN107381591A (en) | A kind of preparation method of the sodalite of petal-shaped at room temperature | |
CN109266349B (en) | Preparation method and application of water-soluble rare earth up-conversion nanoparticles |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |