CN105385444A - Strontium titanate light-emitting nano-particle coated by silicon dioxide and preparation method thereof - Google Patents
Strontium titanate light-emitting nano-particle coated by silicon dioxide and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a strontium titanate light-emitting nano-particle coated by silicon dioxide and a preparation method thereof, and the strontium titanate light-emitting nano-particle coated by mesoporous silicon dioxide is prepared by adopting a solvothermal and sol-gel method. The prepared material is a core-shell structured nanometer material, a Yb/Er co-doped strontium titanate light-emitting nano-particle is taken as a core, and silicon dioxide is taken as a shell. Rare-earth elements are introduced into the system, and excellent optical monitoring can be realized, the method is simple, and the operability is high. The prepared material is the strontium titanate light-emitting nano-particle coated by silicon dioxide with the particle size of 110-120 nm, and the material is uniform in size, good in monodispersity, good in biocompatibility and high in conversion light-emitting effect. The prepared material has a broad application prospect in the fields of bio-medicine, such as biological probes, tissue or cell imaging, and drug tracing.
Description
Technical field
The invention belongs to applied inorganic advanced technical field of nano material, particularly a kind of strontium titanate luminous nano granule and preparation method thereof of Silica-coated, can be applicable to bioprobe, tissue or the field such as cell imaging and pharmaceutical indications.
Background technology
Nano material has many advantages as pharmaceutical carrier and is widely studied.Nano particle has larger specific surface area, less size, and has good pattern.Studying more has SiO
2nano particle, the biopolymer nanoparticles such as PLGA, also have NaYF
4or NaYF
4with SiO
2the nano particle of compound.In these materials, silicon-dioxide, except having homogeneous size and controllable appearance, outside larger specific surface area, also has good biocompatibility, has become a kind of important pharmaceutical carrier.When silicon-dioxide is as pharmaceutical carrier, by regulating mesoporous formation, loading and the controllable release of medicine can be realized.
But the kinetics of drug release process remains a difficult problem for a clinical application, this just needs to find a kind of method can its change procedure of more intuitive understanding.Rare earth element can realize long-wave band light source activation, continues the light inspiring shorter wavelength.Compare with UV-light with organic dye, rear-earth-doped up-conversion nano material has the premium propertiess such as excitation light source energy is low, tissue injury is little, excellent in optical properties, chemical stability are good, biological tissue's absorption is little, penetrativity is large, therefore gets the attention and studies.Utilize the change of the up-conversion luminescence effect of rare earth element optical signalling in the loading and dispose procedure of medicine, the dynamic monitoring of medicine can well be realized.
Summary of the invention
Problem to be solved by this invention is to provide strontium titanate luminous nano granule of the large mesoporous silicon oxide parcel of a kind of good biocompatibility, luminous efficiency and luminous intensity and preparation method thereof.
The object of the invention is to be achieved through the following technical solutions:
A strontium titanate luminous nano granule for Silica-coated, described nano particle diameter is 110 ~ 120nm, has chemical general formula: Sr
1-x-ytiO
3: xYb
3+, yEr
3+mSiO
2, wherein 0.15≤x≤0.18,0.01≤y≤0.02.
A preparation method for the strontium titanate luminous nano granule of Silica-coated, comprises the following steps:
(1) according to chemical general formula Sr
1-x-ytiO
3: xYb
3+, yEr
3+in stoichiometric ratio (0.15≤x≤0.18 of each element, 0.01≤y≤0.02), get four nitric hydrate strontiums, five nitric hydrate erbiums, five nitric hydrate ytterbiums, join (naoh concentration 17.5mol/L) in 10ml aqueous sodium hydroxide solution, make it dissolve under magnetic stirring, obtain solution A; 4mmol titanous chloride is first dissolved in 10ml ethanol, is then dropwise added drop-wise in A, obtains B solution.
(2) stir after 30 minutes, successively 2ml oleic acid and 1.6g sodium oleate are added in B solution; Then be transferred in 50ml tetrafluoroethylene reactor inner bag, add water to 40ml, continue stirring 2 hours.After mixing, inner bag is put into stainless steel outer sleeve, put into 180 DEG C of baking oven reactions 8 hours; After being cooled to room temperature, after using hexanaphthene, washing with alcohol centrifugal successively white depositions bottom inner bag, 60 DEG C of dry 24h, can obtain rare earth-doped strontium titanate up-conversion luminescence nano particle, be denoted as Sr
1-x-ytiO
3: xYb
3+, yEr
3+.
(3) the rare earth-doped strontium titanate up-conversion luminescence nano particle of step 2 gained is dissolved in cyclohexane solution with 10mg/mL, then the cyclohexane solution of 2ml rare earth-doped strontium titanate nano particle is joined (CTAB concentration is 0.0275-0.0825M) in cetyl trimethylammonium bromide (CTAB) aqueous solution of 5ml, ultrasonic vibration 30 minutes.Then mixing solutions is heated 5 minutes, with evaporating cyclohexane at 70 DEG C.
(4) 45ml deionized water, 0.3ml sodium hydroxide solution (2M) and 2.2mmol tetraethyl orthosilicate is then added successively, stir after 3 hours, centrifugal and use water, ethanol purge successively, gained white depositions puts into the dry 12h of baking oven, finally put into retort furnace 550 DEG C sintering 2h, the strontium titanate luminous nano granule of Silica-coated can be obtained.
Beneficial effect of the present invention is:
(1) the luminous strontium titanate nanoparticles particle diameter synthesized by is little, and luminous intensity is large, can well be used as optical signalling and follow the trail of material.
(2) the strontium titanate luminous nano granule stable performance of this preparation method's gained mesoporous silicon oxide parcel, controllability is strong, and solvent for use is second alcohol and water, green non-pollution.
(3) the strontium titanate luminous nano granule luminous efficiency of gained mesoporous silicon oxide parcel of the present invention is high, and luminous intensity is large, can realize good fluorescent mark effect.Important application prospect is had in organizational project, imaging in biological tissues and pharmaceutical indications field.
Accompanying drawing explanation
Fig. 1 is the two X-ray diffractogram mixing the strontium titanate luminous nano granule of strontium titanate nanoparticles and Silica-coated of ytterbium erbium prepared by embodiment 1.Sharp peak represents strontium titanate crystals, and steamed bun peak is SiO
2sign.
Fig. 2 is the transmission electron microscope photo of the strontium titanate luminous nano granule of Silica-coated prepared by embodiment 1.
Fig. 3 is the up-conversion fluorescence spectrogram of the strontium titanate luminous nano granule material of Silica-coated prepared by embodiment 1 and embodiment 2.
Embodiment
The strontium titanate luminous nano granule of a kind of mesoporous silicon oxide parcel of the present invention, described nano particle diameter is 110 ~ 120nm, has chemical general formula: Sr
1-x-ytiO
3: xYb
3+, yEr
3+mSiO
2, wherein 0.15≤x≤0.18,0.01≤y≤0.02.The nano particle diameter prepared due to the present invention is little, Surface coating has mesoporous silicon oxide shell, has larger specific surface area, is conducive to adsorption activity group, drug molecule etc., more realize medicine to load and controllable release, also can be used for fluorescent mark and bio-imaging.It is infrared ray excited that the strontium titanate luminous nano granule that this mesoporous silicon oxide wraps up can realize 980nm, launches the green glow of 550-560nm wave band and the ruddiness of 660-670nm wave band.Up-conversion luminescence efficiency is high, and luminous intensity is large, and can regulate intensity and the color of light.Concrete preparation method is as follows:
(1) according to chemical general formula Sr
1-x-ytiO
3: xYb
3+, yEr
3+in stoichiometric ratio (0.15≤x≤0.18 of each element, 0.01≤y≤0.02), get four nitric hydrate strontiums, five nitric hydrate erbiums, five nitric hydrate ytterbiums, join (naoh concentration 17.5mol/L) in 10ml aqueous sodium hydroxide solution, make it dissolve under magnetic stirring, obtain solution A; 4mmol titanous chloride is first dissolved in 10ml ethanol, is then dropwise added drop-wise in A, obtains B solution.In this step, utilize titanous chloride as titanium source, more stable than titanium tetrachloride chemical property, and can be easy to be converted into titanic in high-temperature water thermal process.
(2) stir after 30 minutes, successively 2ml oleic acid and 1.6g sodium oleate are added in B solution, effectively to control the grain nucleation and growth process of strontium titanate nanoparticles; Then be transferred in 50ml tetrafluoroethylene reactor inner bag, add water to 40ml, continue stirring 2 hours.After mixing, inner bag is put into stainless steel outer sleeve, put into 180 DEG C of baking oven reactions 8 hours; After being cooled to room temperature, after using hexanaphthene, washing with alcohol centrifugal successively white depositions bottom inner bag, 60 DEG C of dry 24h, can obtain rare earth-doped strontium titanate up-conversion luminescence nano particle, be denoted as Sr
1-x-ytiO3:xYb3+, yEr3+.Gained nano particle median size is 100nm, and luminescent effect is strong.
(3) the rare earth-doped strontium titanate up-conversion luminescence nano particle of step 2 gained is dissolved in cyclohexane solution with 10mg/mL, then the cyclohexane solution of 2ml rare earth-doped strontium titanate nano particle is joined (CTAB concentration is 0.0275-0.0825M) in cetyl trimethylammonium bromide (CTAB) aqueous solution of 5ml, ultrasonic vibration 30 minutes.Then mixing solutions is heated 5 minutes, with evaporating cyclohexane at 70 DEG C.In this step, it is mesoporous to produce to add cetyl trimethylammonium bromide, and the number of throughput carrys out the structure of adjustment kit covering layer.
(4) then add 45ml deionized water, 0.3ml sodium hydroxide solution (2M) and 2.2mmol tetraethyl orthosilicate successively, wherein, sodium hydroxide can promote the polymerization of tetraethyl orthosilicate hydrolyzate, obtains uniform mesoporous silicon oxide integument.Stir after 3 hours, centrifugal and use water, ethanol purge successively, gained white depositions puts into the dry 12h of baking oven, finally puts into retort furnace 550 DEG C sintering 2h, can obtain the strontium titanate luminous nano granule of Silica-coated.
Describe technical scheme of the present invention in detail below in conjunction with the drawings and specific embodiments, but the present invention is not limited to embodiment, those skilled in the art can adjust according to practical situation.
embodiment 1
(1) 3.2mmol tetra-nitric hydrate strontium, 0.08mmol five nitric hydrate erbium and 0.72mmol five nitric hydrate ytterbium are joined in 10 milliliters of aqueous sodium hydroxide solutions (17.5mol/L), make it dissolve under magnetic stirring, obtain solution A.4mmol titanous chloride is first dissolved in 10ml ethanol, is then slowly added drop-wise in A, obtains B solution.
(2) stir after 30 minutes, in turn 2ml oleic acid and 1.6g sodium oleate are added in B solution.Proceed in 50ml tetrafluoroethylene reactor inner bag, add water to 40ml, continue stirring 2 hours.After mixing, inner bag is put into stainless steel outer sleeve, reaction 8 hours at 180 DEG C in an oven.After being cooled to room temperature, white depositions hexanaphthene bottom inner bag, ethanol repetitive scrubbing is centrifugal to go out the impurity such as oleic acid.The white depositions that obtains, in air, 60 DEG C of dry 24h can obtain rare earth-doped strontium titanate up-conversion luminescence nano particle.
(3) cyclohexane solution of 2ml rare earth-doped strontium titanate nano particle joins (CTAB concentration is 0.025M) in cetyl trimethylammonium bromide (CTAB) aqueous solution of 5ml, ultrasonic vibration 30 minutes.Then mixing solutions is heated to 70 DEG C, continues hexanaphthene to be evaporated in 5 minutes.
(4) 45ml deionized water, 0.3ml sodium hydroxide solution (2M) and 2.2mmol tetraethyl orthosilicate is then added in turn, stir after 3 hours, centrifugal and with water and ethanol purge, gained white depositions puts into the dry 12h of baking oven, finally put into retort furnace 550 DEG C sintering 2h, the strontium titanate luminous nano granule of Silica-coated can be obtained, called after S
0.8tO:0.18Yb
3+, 0.02Er
3+0.5mSiO
2.
The chemical general formula STO:Yb of the product that the present embodiment obtains
3+, Er
3+1.0mSiO
2.As can be seen from Figure 1, gained nano particle is except SrTiO
3crystalline phase and SiO
2, there is no other impurity phases outward, illustrate that Er and Yb successfully adulterates with the crystalline structure of strontium titanate.As can be seen from Figure 2, gained nano grain surface silica shell layer thickness is about 6nm, and parcel evenly.As can be seen from Figure 3, the luminous intensity of gained nano particle is large.
embodiment 2
(1) 3.36mmol tetra-nitric hydrate strontium, 0.04mmol five nitric hydrate erbium and 0.6mmol five nitric hydrate ytterbium are joined in 10 milliliters of aqueous sodium hydroxide solutions (17.5mol/L), make it dissolve under magnetic stirring, obtain solution A.4mmol titanous chloride is first dissolved in 10ml ethanol, is then slowly added drop-wise in A, obtains B solution.
(2) stir after 30 minutes, in turn 2ml oleic acid and 1.6g sodium oleate are added in B solution.Proceed in 50ml tetrafluoroethylene reactor inner bag, add water to 40ml, continue stirring 2 hours.After mixing, inner bag is put into stainless steel outer sleeve, reaction 8 hours at 180 DEG C in an oven.After being cooled to room temperature, white depositions hexanaphthene bottom inner bag, ethanol repetitive scrubbing is centrifugal to go out the impurity such as oleic acid.The white depositions that obtains, in air, 60 DEG C of dry 24h can obtain rare earth-doped strontium titanate up-conversion luminescence nano particle.
(3) cyclohexane solution of 2ml rare earth-doped strontium titanate nano particle joins (CTAB concentration is 0.0825M) in cetyl trimethylammonium bromide (CTAB) aqueous solution of 5ml, ultrasonic vibration 30 minutes.Then mixing solutions is heated to 70 DEG C, continues hexanaphthene to be evaporated in 5 minutes.
(4) 45ml deionized water, 0.3ml sodium hydroxide solution (2M) and 2.2mmol tetraethyl orthosilicate is then added in turn, stir after 3 hours, centrifugal and with water and ethanol purge, gained white depositions puts into the dry 12h of baking oven, finally put into retort furnace 550 DEG C sintering 2h, the strontium titanate luminous nano granule of Silica-coated can be obtained, called after S
0.84tO:0.15Yb
3+, 0.01Er
3+1.5mSiO
2.
The chemical general formula S of the product that the present embodiment obtains
0.84tO:0.15Yb
3+, 0.01Er
3+1.5mSiO
2.As can be seen from the above table, the specific surface area of gained nano particle and pore volume increase all to some extent.It can thus be appreciated that method of the present invention can carry out the structure of reconciliation statement bread covering layer by the add-on of cetyl trimethylammonium bromide.
Claims (2)
1. the strontium titanate luminous nano granule of kind of Silica-coated, is characterized in that, described nano particle diameter is 110 ~ 120nm, has chemical general formula: Sr
1-x-ytiO
3: xYb
3+, yEr
3+mSiO
2, wherein 0.15≤x≤0.18,0.01≤y≤0.02.
2. a preparation method for the strontium titanate luminous nano granule of Silica-coated described in claim 1, is characterized in that, comprise the following steps:
(1) according to chemical general formula Sr
1-x-ytiO
3: xYb
3+, yEr
3+in stoichiometric ratio (0.15≤x≤0.18 of each element, 0.01≤y≤0.02), get four nitric hydrate strontiums, five nitric hydrate erbiums, five nitric hydrate ytterbiums, join (naoh concentration 17.5mol/L) in 10ml aqueous sodium hydroxide solution, make it dissolve under magnetic stirring, obtain solution A; 4mmol titanous chloride is first dissolved in 10ml ethanol, is then dropwise added drop-wise in A, obtains B solution;
(2) stir after 30 minutes, successively 2ml oleic acid and 1.6g sodium oleate are added in B solution; Then be transferred in 50ml tetrafluoroethylene reactor inner bag, add water to 40ml, continue stirring 2 hours; After mixing, inner bag is put into stainless steel outer sleeve, put into 180 DEG C of baking oven reactions 8 hours; After being cooled to room temperature, after using hexanaphthene, washing with alcohol centrifugal successively white depositions bottom inner bag, 60 DEG C of dry 24h, can obtain rare earth-doped strontium titanate up-conversion luminescence nano particle, be denoted as Sr
1-x-ytiO
3: xYb
3+, yEr
3+;
(3) the rare earth-doped strontium titanate up-conversion luminescence nano particle of step 2 gained is dissolved in cyclohexane solution with 10mg/mL, then the cyclohexane solution of 2ml rare earth-doped strontium titanate nano particle is joined (CTAB concentration is 0.0275-0.0825M) in cetyl trimethylammonium bromide (CTAB) aqueous solution of 5ml, ultrasonic vibration 30 minutes; Then mixing solutions is heated 5 minutes, with evaporating cyclohexane at 70 DEG C;
(4) 45ml deionized water, 0.3ml sodium hydroxide solution (2M) and 2.2mmol tetraethyl orthosilicate is then added successively, stir after 3 hours, centrifugal and use water, ethanol purge successively, gained white depositions puts into the dry 12h of baking oven, finally put into retort furnace 550 DEG C sintering 2h, the strontium titanate luminous nano granule of Silica-coated can be obtained.
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| CN113008878A (en) * | 2021-02-24 | 2021-06-22 | 杭州可靠护理用品股份有限公司 | Color developing agent for excrement detection and application of color developing agent to paper diapers |
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| CN113789169B (en) * | 2021-10-29 | 2024-01-26 | 重庆文理学院 | Fluorescent powder and preparation method thereof |
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Application publication date: 20160309 |