CN104743607A - Preparing method of cube titanium dioxide vacant shell - Google Patents
Preparing method of cube titanium dioxide vacant shell Download PDFInfo
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- CN104743607A CN104743607A CN201310260076.3A CN201310260076A CN104743607A CN 104743607 A CN104743607 A CN 104743607A CN 201310260076 A CN201310260076 A CN 201310260076A CN 104743607 A CN104743607 A CN 104743607A
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Abstract
The invention relates to a cube titanium dioxide vacant shell material and a preparing method thereof. The material comprises uniform cube titanium dioxide shells. The preparing method includes following steps: (1) slowly hydrolyzing titanium sulfate on surfaces of cube silver bromide microcrystals which are adopted as a template agent to obtain silver bromide/titanium dioxide of a core-shell structure; (2) subjecting the obtained silver bromide/titanium dioxide to hydro-thermal treatment; and (3) treating the silver bromide/titanium dioxide with a solution capable of dissolving silver bromide to remove the silver bromide template so as to obtain the cube titanium dioxide vacant shells. The material and the method have advantages of simple preparation processes, controllable morphology, and the like. The prepared material can be used for medical biomacromolecules, slow-release and controlled-release medicine carriers for medicines, and the like.
Description
Technical field
The present invention relates to and a kind ofly can be used for the medically slowly-releasing of biomacromolecule and medicine, the drug carrier material of controlled release and preparation method thereof, belong to biomedical sector.
Background technology
The morphology of material determines the performance of material, as all closely related with its Potamogeton crispus with material etc. in the absorption of material, the numerous characteristics such as separation and catalysis.Design and synthesize the functional materials with specific morphology structure and become one of most active research contents of current Material Field.
In recent years, the preparation of inorganic hollow material, as SiO
2, Ni, Co/B, TiO
2, Pt/Ru/Pd, Co
3o
4, Ni/Fe/P, ferrite, carbon, SnO
2with Calucium Silicate powder etc., more and more receive the concern of people.Because inorganic hollow material has chemistry and Heat stability is good, specific surface area is large, vesicular structure, low-density feature, therefore it has potential application prospect in a lot of fields, such as catalyzer, magnetics, microwave absorbing, lithium ion battery, solar cell, electrocatalysis, storage hydrogen, gas sensor, drug conveying etc.
In these Inorganic Hollow Microspheres materials, because the nano titania/micrometer structure of hollow structure at high temperature has very high toughness, stability and biocompatibility, and its boring structure can be used for drug loading and small molecules, be therefore widely used in the every field such as chemical catalysis, energy storage, sewage disposal and biomedicine.Due to the character of its uniqueness, become the study hotspot of domestic and international scientist.
Hollow structure can utilize its cavity as microenvironment, for the slowly-releasing, controlled release etc. of medically biomacromolecule and medicine.Common administering mode, within for some time that administration starts, the concentration of medicine in blood or in in-vivo tissue is very large, sometimes exceedes the medicine maximum tolerated dose of patient, and may produce larger side effect; On the other hand, the concentration of medicine in human body can only maintain the very short time, and the concentration of medicine in blood or in in-vivo tissue is very fast again lower than effective dose, and does not have due curative effect.Although adopt multiple low dose administration can avoid above-mentioned phenomenon, bring inconvenience to patient, be difficult to carry out.Therefore, preparation the slow-releasing prolonged action drug of slow releasing pharmaceutical cpd can have using value in disease treatment.Prepare slow release long-acting medicine, key to prepare the solid support material of the sustained release that can make carried.
The nano-medicament carrier kind of main development is a lot of both at home and abroad at present, and they possess nano level size (being less than 1mm), various Biodegradable material, the polymer of such as nature or synthetic or lipid, phosphatide or organic double compound etc.Titanium dioxide due to its structure and surface properties clear, there is good biocompatibility, the advantages such as the functional modification on surface can be carried out well, nano material is obtained a wide range of applications in biomedicine, nano-carrier makes it to have higher area/volume ratio due to sub-micro finestructure, improves scatter coefficient.Usually by reticuloendothelial system phagocytic nanoparticulate carriers in body, this phagolysis is usually relevant with the particle diameter of particle and surface properties thereof.
Therefore, stablize in development structure, good biocompatibility, drug loading efficiency high and can the nanoparticle of target controllable release as on pharmaceutical carrier, titanium dioxide has good Research Prospects.
Summary of the invention
The present invention for template, carries out external sheath with titanium dioxide to it with cubes AgBr crystallite, finally processes bromination silver/titanium dioxide with the solution of solubilized Silver monobromide, and removing Silver monobromide template, obtains cubes titanium dioxide ghost.Prepared titanium dioxide shell can with its cavity as pharmaceutical carrier.
The preparation of cubic silver bromide crystallite adopts double-jet method, and its concrete preparation process is shown in the CatalysisCommunications such as Dong, 2013,38,16-20.The preparation of titanium dioxide ghost is with cubic silver bromide crystallite for template, and its concrete preparation process comprises the following steps:
(1) under gelatin, polyvinylpyrrolidone or polyvinyl alcohol exist, titanium sulfate is joined Silver monobromide crystallite mutually in, control the add-on of titanium sulfate, hydrolysis temperature and hydrothermal temperature, nucleocapsid structure Silver monobromide/titanium dioxide granule can be obtained;
(2) obtained nucleocapsid structure Silver monobromide/titanium dioxide granule is carried out hydrothermal treatment consists;
(3) process nucleocapsid structure Silver monobromide/titanium dioxide granule with the solution of solubilized Silver monobromide, removing Silver monobromide template, obtains cubes titanium dioxide ghost.
In step (1), the add-on of titanium sulfate calculates by coated by titanium dioxide layer thickness, and be generally 0.05 ~ 0.2 μm, the hydrolysis temperature of titanium sulfate is 30 DEG C ~ 80 DEG C;
In step (2), hydrothermal temperature is 100 ~ 150 DEG C;
In step (3), comprise in thiosulfate ion, thiocyanate ion, cryanide ion or fewrricyanic acid radical ion in the solution of removing Silver monobromide template one or both.
Accompanying drawing explanation
Fig. 1 is that embodiment 1 obtains cubes TiO
2transmission electron microscope figure.
Fig. 2 is that embodiment 1 obtains cubes TiO
2x-ray diffraction pattern.
Embodiment
Below in conjunction with example, the present invention is further described in detail.
Embodiment 1
Take a certain amount of Silver monobromide gelatin solution, add titanium sulfate (be 0.1 μm calculating by coated by titanium dioxide layer thickness), be warming up to 80 DEG C gradually from 30 DEG C and first titanium sulfate be hydrolyzed, then carry out hydro-thermal at 120 DEG C, improve titanium dioxide crystal degree.Then, carry out centrifuge washing 6 times with the bromination silver/titanium dioxide composite semiconductor of the warm water of 45 DEG C to preparation, to remove saltpetre, sulfuric acid that gelatin protective material, excessive Potassium Bromide and reaction generate.80 DEG C of dryings 3 hours, obtain Silver monobromide/titania powder.Above-mentioned powder is joined in hypo solution, stirs 30 minutes, removing Silver monobromide template, then wash 4 times with water, can TiO be obtained
2ghost.
The transmission microscopy picture of the cubes titanium dioxide ghost of example 1 gained as shown in Figure 1.As can be seen from the figure, find out that cubes titanium dioxide is cubes shell structures, the length of side is about 0.8 μm, and thickness of the shell is about 0.1 μm.The X-ray crystallography of embodiment 1 gained titanium dioxide sample as shown in Figure 2, as can be seen from the figure, the diffraction peak of products obtained therefrom and the standard diffraction collection of illustrative plates (JCPDS:21-1272) of anatase titania completely the same.
Embodiment 2
Take a certain amount of Silver monobromide, add polyvinylpyrrolidone, add titanium sulfate (be 0.1 μm calculating by coated by titanium dioxide layer thickness), be warming up to 80 DEG C gradually from 30 DEG C and first titanium sulfate be hydrolyzed, carry out hydro-thermal at 120 DEG C again, improve titanium dioxide crystal degree.Then, carry out centrifuge washing 6 times with the bromination silver/titanium dioxide composite semiconductor of the warm water of 45 DEG C to preparation, to remove saltpetre, sulfuric acid that polyvinylpyrrolidone protective material, excessive Potassium Bromide and reaction generate.80 DEG C of dryings 3 hours, obtain Silver monobromide/titania powder.Above-mentioned powder is joined in hypo solution, stirs 30 minutes, removing Silver monobromide template, then wash 4 times with water, can TiO be obtained
2ghost.
Embodiment 3
Take a certain amount of Silver monobromide, add polyvinyl alcohol, add titanium sulfate (be 0.1 μm calculating by coated by titanium dioxide layer thickness), be warming up to 80 DEG C gradually from 30 DEG C and first titanium sulfate be hydrolyzed, carry out hydro-thermal at 120 DEG C again, improve titanium dioxide crystal degree.Then, carry out centrifuge washing 6 times with the bromination silver/titanium dioxide composite semiconductor of the warm water of 45 DEG C to preparation, to remove saltpetre, sulfuric acid that polyvinyl alcohol protective material, excessive Potassium Bromide and reaction generate.80 DEG C of dryings 3 hours, obtain Silver monobromide/titania powder.Above-mentioned powder is joined in hypo solution, stirs 30 minutes, removing Silver monobromide template, then wash 4 times with water, can TiO be obtained
2ghost.
Embodiment 4
Take a certain amount of Silver monobromide gelatin solution, add titanium sulfate (be 0.05 μm calculating by coated by titanium dioxide layer thickness), be warming up to 80 DEG C gradually from 30 DEG C and first titanium sulfate be hydrolyzed, then carry out hydro-thermal at 120 DEG C, improve titanium dioxide crystal degree.Then, carry out centrifuge washing 6 times with the bromination silver/titanium dioxide composite semiconductor of the warm water of 45 DEG C to preparation, to remove saltpetre, sulfuric acid that gelatin protective material, excessive Potassium Bromide and reaction generate.80 DEG C of dryings 3 hours, obtain Silver monobromide/titania powder.Above-mentioned powder is joined in hypo solution, stirs 30 minutes, removing Silver monobromide template, then wash 4 times with water, can TiO be obtained
2ghost.
Embodiment 5
Take a certain amount of Silver monobromide gelatin solution, add titanium sulfate (be 0.15 μm calculating by coated by titanium dioxide layer thickness), be warming up to 80 DEG C gradually from 30 DEG C and first titanium sulfate be hydrolyzed, then carry out hydro-thermal at 120 DEG C, improve titanium dioxide crystal degree.Then, carry out centrifuge washing 6 times with the bromination silver/titanium dioxide composite semiconductor of the warm water of 45 DEG C to preparation, to remove saltpetre, sulfuric acid that gelatin protective material, excessive Potassium Bromide and reaction generate.80 DEG C of dryings 3 hours, obtain Silver monobromide/titania powder.Above-mentioned powder is joined in hypo solution, stirs 30 minutes, removing Silver monobromide template, then wash 4 times with water, can TiO be obtained
2ghost.
Embodiment 6
Take a certain amount of Silver monobromide gelatin solution, add titanium sulfate (be 0.2 μm calculating by coated by titanium dioxide layer thickness), be warming up to 80 DEG C gradually from 30 DEG C and first titanium sulfate be hydrolyzed, then carry out hydro-thermal at 120 DEG C, improve titanium dioxide crystal degree.Then, carry out centrifuge washing 6 times with the bromination silver/titanium dioxide composite semiconductor of the warm water of 45 DEG C to preparation, to remove saltpetre, sulfuric acid that gelatin protective material, excessive Potassium Bromide and reaction generate.80 DEG C of dryings 3 hours, obtain Silver monobromide/titania powder.Above-mentioned powder is joined in hypo solution, stirs 30 minutes, removing Silver monobromide template, then wash 4 times with water, can TiO be obtained
2ghost.
Embodiment 7
Take a certain amount of Silver monobromide gelatin solution, add titanium sulfate (be 0.1 μm calculating by coated by titanium dioxide layer thickness), 40 DEG C are hydrolyzed to titanium sulfate, then carry out hydro-thermal at 120 DEG C, improve titanium dioxide crystal degree.Then, carry out centrifuge washing 6 times with the bromination silver/titanium dioxide composite semiconductor of the warm water of 45 DEG C to preparation, to remove saltpetre, sulfuric acid that gelatin protective material, excessive Potassium Bromide and reaction generate.80 DEG C of dryings 3 hours, obtain Silver monobromide/titania powder.Above-mentioned powder is joined in hypo solution, stirs 30 minutes, removing Silver monobromide template, then wash 4 times with water, can TiO be obtained
2ghost.
Embodiment 8
Take a certain amount of Silver monobromide gelatin solution, add titanium sulfate (be 0.1 μm calculating by coated by titanium dioxide layer thickness), 70 DEG C are hydrolyzed to titanium sulfate, then carry out hydro-thermal at 120 DEG C, improve titanium dioxide crystal degree.Then, carry out centrifuge washing 6 times with the bromination silver/titanium dioxide composite semiconductor of the warm water of 45 DEG C to preparation, to remove saltpetre, sulfuric acid that gelatin protective material, excessive Potassium Bromide and reaction generate.80 DEG C of dryings 3 hours, obtain Silver monobromide/titania powder.Above-mentioned powder is joined in hypo solution, stirs 30 minutes, removing Silver monobromide template, then wash 4 times with water, can TiO be obtained
2ghost.
Embodiment 9
Take a certain amount of Silver monobromide gelatin solution, add titanium sulfate (be 0.1 μm calculating by coated by titanium dioxide layer thickness), be warming up to 80 DEG C gradually from 30 DEG C and first titanium sulfate be hydrolyzed, then carry out hydro-thermal at 100 DEG C, improve titanium dioxide crystal degree.Then, carry out centrifuge washing 6 times with the bromination silver/titanium dioxide composite semiconductor of the warm water of 45 DEG C to preparation, to remove saltpetre, sulfuric acid that gelatin protective material, excessive Potassium Bromide and reaction generate.80 DEG C of dryings 3 hours, obtain Silver monobromide/titania powder.Above-mentioned powder is joined in hypo solution, stirs 30 minutes, removing Silver monobromide template, then wash 4 times with water, can TiO be obtained
2ghost.
Embodiment 10
Take a certain amount of Silver monobromide gelatin solution, add titanium sulfate (be 0.1 μm calculating by coated by titanium dioxide layer thickness), be warming up to 80 DEG C gradually from 30 DEG C and first titanium sulfate be hydrolyzed, then carry out hydro-thermal at 150 DEG C, improve titanium dioxide crystal degree.Then, carry out centrifuge washing 6 times with the bromination silver/titanium dioxide composite semiconductor of the warm water of 45 DEG C to preparation, to remove saltpetre, sulfuric acid that gelatin protective material, excessive Potassium Bromide and reaction generate.80 DEG C of dryings 3 hours, obtain Silver monobromide/titania powder.Above-mentioned powder is joined in hypo solution, stirs 30 minutes, removing Silver monobromide template, then wash 4 times with water, can TiO be obtained
2ghost.
Embodiment 11
Take a certain amount of Silver monobromide gelatin solution, add titanium sulfate (be 0.1 μm calculating by coated by titanium dioxide layer thickness), be warming up to 80 DEG C gradually from 30 DEG C and first titanium sulfate be hydrolyzed, then carry out hydro-thermal at 120 DEG C, improve titanium dioxide crystal degree.Then, carry out centrifuge washing 6 times with the bromination silver/titanium dioxide composite semiconductor of the warm water of 45 DEG C to preparation, to remove saltpetre, sulfuric acid that gelatin protective material, excessive Potassium Bromide and reaction generate.80 DEG C of dryings 3 hours, obtain Silver monobromide/titania powder.Above-mentioned powder is joined in rhodan ammonium solution, stir 30 minutes, removing Silver monobromide template, then wash 4 times with water, can TiO be obtained
2ghost.
Embodiment 12
Take a certain amount of Silver monobromide gelatin solution, add titanium sulfate (be 0.1 μm calculating by coated by titanium dioxide layer thickness), be warming up to 80 DEG C gradually from 30 DEG C and first titanium sulfate be hydrolyzed, then carry out hydro-thermal at 120 DEG C, improve titanium dioxide crystal degree.Then, carry out centrifuge washing 6 times with the bromination silver/titanium dioxide composite semiconductor of the warm water of 45 DEG C to preparation, to remove saltpetre, sulfuric acid that gelatin protective material, excessive Potassium Bromide and reaction generate.80 DEG C of dryings 3 hours, obtain Silver monobromide/titania powder.Above-mentioned powder is joined in potassium ferricyanide solution, stirs 30 minutes, removing Silver monobromide template, then wash 4 times with water, can TiO be obtained
2ghost.
Claims (5)
1. a preparation method for cubes titanium dioxide ghost pharmaceutical carrier, is characterized in that, described cubes titanium dioxide ghost is prepared by the method being template with cubic silver bromide crystallite, and concrete preparation process comprises the following steps:
(1) under gelatin, polyvinylpyrrolidone or polyvinyl alcohol exist, titanium sulfate is joined Silver monobromide crystallite mutually in, control the add-on of titanium sulfate, hydrolysis temperature and hydrothermal temperature, nucleocapsid structure Silver monobromide/titanium dioxide granule can be obtained;
(2) obtained nucleocapsid structure Silver monobromide/titanium dioxide granule is carried out hydrothermal treatment consists;
(3) process nucleocapsid structure Silver monobromide/titanium dioxide granule with the solution of solubilized Silver monobromide, removing Silver monobromide template, obtains cubes titanium dioxide ghost.
2. the preparation method of cubes titanium dioxide ghost pharmaceutical carrier according to claim 1, is characterized in that, the add-on of titanium sulfate calculates by coated by titanium dioxide layer thickness, and coating thickness is 0.05 ~ 0.2 μm.
3. the preparation method of cubes titanium dioxide ghost pharmaceutical carrier according to claim 1, is characterized in that, the hydrolysis temperature of titanium sulfate is 30 DEG C ~ 80 DEG C.
4. the preparation method of cubes titanium dioxide ghost pharmaceutical carrier according to claim 1, it is characterized in that, hydrothermal temperature is 100 ~ 150 DEG C.
5. the preparation method of cubes titanium dioxide ghost pharmaceutical carrier according to claim 1, it is characterized in that, comprise in thiosulfate ion, thiocyanate ion, cryanide ion or fewrricyanic acid radical ion in the solution of removing Silver monobromide template one or both.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105078879A (en) * | 2015-09-06 | 2015-11-25 | 江苏大学 | Preparation method for tegafur slow-release agent |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1593748A (en) * | 2004-07-05 | 2005-03-16 | 华东理工大学 | Process for preparing titanium dioxide membrane photocatalyst |
| CN1594102A (en) * | 2004-07-05 | 2005-03-16 | 华东理工大学 | Method for preparing titanium dioxide mesoporous material |
| CN103101971A (en) * | 2011-11-11 | 2013-05-15 | 新疆大学 | Green biomimetic preparation method of titanium dioxide nano material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1593748A (en) * | 2004-07-05 | 2005-03-16 | 华东理工大学 | Process for preparing titanium dioxide membrane photocatalyst |
| CN1594102A (en) * | 2004-07-05 | 2005-03-16 | 华东理工大学 | Method for preparing titanium dioxide mesoporous material |
| CN103101971A (en) * | 2011-11-11 | 2013-05-15 | 新疆大学 | Green biomimetic preparation method of titanium dioxide nano material |
Non-Patent Citations (1)
| Title |
|---|
| RONGFANG DONG等: "AgBr@Ag/TiO2 core–shell composite with excellent visible light photocatalytic activity and hydrothermal stability", 《CATALYSIS COMMUNICATIONS》, 17 April 2013 (2013-04-17), pages 16 - 20 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105078879A (en) * | 2015-09-06 | 2015-11-25 | 江苏大学 | Preparation method for tegafur slow-release agent |
| CN105078879B (en) * | 2015-09-06 | 2017-10-27 | 江苏大学 | A kind of preparation method of Tegafur sustained release agent |
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