CN105652347A - Preparation method of three-dimensional ordered titanium dioxide photonic crystal microballoons covered by silver nanoparticles - Google Patents
Preparation method of three-dimensional ordered titanium dioxide photonic crystal microballoons covered by silver nanoparticles Download PDFInfo
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Abstract
The invention discloses a preparation method of three-dimensional ordered titanium dioxide photonic crystal microballoons covered by silver nanoparticles, and belongs to the technical field of biomedical research, environmental monitoring and clinical detection. According to the invention, a microfluidic device is adopted to prepare three-dimensional ordered titanium dioxide photonic crystal microballoons, and then a silver nitrate water solution is adopted to generate the silver nanoparticles through high temperature reduction of a hydrothermal reaction, the silver nanoparticles are loaded uniformly on the surfaces of the titanium dioxide photonic crystal microballoons, and three-dimensional ordered titanium dioxide photonic crystal microballoon structure covered by the silver nanoparticles is generated. The prepared product has the advantages that the structure is simple in regulation and control, is good in repeatability, and is uniform in surface hotspot distribution, so that the prepared three-dimensional ordered titanium dioxide photonic crystal microballoon structure covered by the silver nanoparticles is high in detection sensitivity, is simple in operation and is relatively good in signal reproducibility when the structure is used for surface raman enhanced spectrum substrate detection, and the detection limit range of the composite material in the surface raman enhanced detection field is further improved.
Description
Technical field
The present invention relates to the technical field of biomedical research, environmental monitoring and Clinical detection, particularly to the preparation method of a kind of three-dimensional order Nano silver grain cladding titanium dioxide photon crystal micro-ball.
Background technology
Current surface Raman enhancement spectrum has been widely used in biochemistry because of the high sensitivity of its detection property, and chemical molecular detects, iconography, environmental monitoring and sensor application aspect. Substrate as ideal effective surface Raman enhancement spectrum not only to have high sensitivity, in addition it is also necessary to ensures good signal reproducibility.
In order to extensively and fully play periodic arrangement structure and its reproducible advantage of good making of photonic crystal high uniformity, photon crystal material has been widely used in the research of Surface Raman Spectra substrate. And photonic crystal is prepared into microsphere just there is the advantage such as arrangement high-sequential and controllable adjustment, preparation favorable reproducibility, big, the good biocompatibility of specific surface area, it is thus possible to realize quick, easy, cheap biomolecule surface Raman substrate detection. The Electromagnetic enhancement effect of recycling silver nano-grain, silver nano-grain is modified at equably photon crystal micro-ball surface, so its surface hotspot's distribution is homogeneous, when this composite is as Surface Raman Spectra substrate, can not only there is the shortcoming that the advantage such as higher sensitivity, detection limit wider range can also overcome detection signal reproducibility difference.
The photon crystal film of the existing two dimension of current report, three-dimensional photon crystal film and optical fiber are used to the substrate research of Surface Raman Spectra. But, photon crystal film easily comes off from substrate, not easily large area prepare, the application when photon crystal film of most of institutes report is as substrate, its structure is unstable and sensitivity is not high when detection, detection limit is limited in scope, it is crucial that the repeatability of its signal can not be protected. Research is fallen over each other in the high activity substrate of three-dimensional order, and the photonic crystal fiber of three-dimensional can not be widely used due to complex manufacturing technology, cost height.
Summary of the invention
It is an object of the invention to the preparation method proposing three-dimensional order Nano silver grain cladding titanium dioxide photon crystal micro-ball, the substrate that the method is prepared is highly sensitive, favorable reproducibility.
The preparation method of the present invention a kind of three-dimensional order Nano silver grain cladding titanium dioxide photon crystal micro-ball comprises the following steps:
1) prepare the dioxide photon crystal microsphere of three-dimensional order: by titanium dioxide nano-particle solution after ultrasonic disperse by solution inhalation syringe; Draw low viscosity methyl-silicone oil with syringe simultaneously; Syringe is connected on the interface singly pushing away syringe pump apparatus of correspondence, and with impeller driven syringe, separately designs the flow velocity of colloid solution and silicone oil; Produce steady and continuous emulsion droplet by micro fluidic device and form microsphere from sedimentation, dry calcining;
2) prepare the Nano silver grain cladding titanium dioxide photon crystal micro-ball of three-dimensional order: the above-mentioned dioxide photon crystal microsphere preparing three-dimensional order is placed in polymeric kettle, add silver nitrate aqueous solution high-temperature water thermal response, take out nature and dry.
Titania nanoparticles prepared by the present invention is Detitanium-ore-type, and diameter is about 250nm, and size is homogeneous, becomes three-dimensional dioxide photon crystal microsphere with the structure dense accumulation of Hexagonal packing, and its reflection peak position is at about 670nm, it then follows Bragg's equation. The titanium dioxide of Anatase is more beneficial for Surface Raman Spectra to be strengthened.
The photon crystal micro-ball arrangement high-sequential being self-assembled into by micro fluidic device and controllable adjustment, preparation favorable reproducibility, spherical completely, arrangement is neat modifies above silver nano-grain for next step and provides regular substrate. Step 1) in the mass percentage concentration of titanium dioxide nano-particle solution be 5%��15%, the flow velocity of titanium dioxide nano-particle solution is 0.5mL/h��2mL/h, and the flow velocity of silicone oil is 5ml/h��50ml/h. In this flow rates, the reactant size obtained is homogeneous, spherical completely. Drying temperature is 40��60 DEG C, drying time 36��60h. Within the scope of this temperature and time, moisture is removed preferably. Calcining heat is 400��800 DEG C.
Step 2 of the present invention) in silver nitrate aqueous solution concentration be 0.015mol/L��0.22mol/L, hydro-thermal reaction generates silver nano-grain and is uniformly modified at the surface of dioxide photon crystal microsphere preferably. The mass ratio that feeds intake of described silver nitrate aqueous solution and dioxide photon crystal microsphere is 12.5��187.5:1, this quality ratio is in scope, being the Key Quality ratio synthesizing titanium dioxide/silver, the titanium dioxide/silver pattern synthesized is homogeneous, and during as substrate, Raman detection signal is the strongest. Hydrothermal temperature is 100��150 DEG C, and the response time is 20��28h. Within the scope of this temperature and time, silver nano-grain can be modified on titanium dioxide microballoon sphere preferably, plays very strong Raman reinforced effects.
The advantage of present invention process is: adopt dioxide photon crystal arrangement of microspheres high-sequential obtained by microflow control technique, controllable adjustment, reproducible. In its finishing, silver nano-grain is realized by one step hydro thermal method, the method preparation cost simple to operate is cheap, manufacturing cycle is short, and silver nano-grain can be uniformly distributed in dioxide photon crystal microsphere surface, it is possible to form homogeneous hotspot's distribution thus improving sensitivity when Surface Raman Spectra detects. The arrangement architecture of obtained dioxide photon crystal microsphere high-sequential modifies upper silver nano-grain as substrate not only due to the hotspot's distribution of its uniform surface makes detection limit wider range, easy and simple to handle when detecting as surface Raman enhancement spectrum substrate simultaneously. It is highly sensitive that the present invention is that surface Raman enhancement spectrum provides, the base material of favorable reproducibility.
Accompanying drawing explanation
Fig. 1 is for adopting the inventive method in step 1) the SEM figure of the dioxide photon crystal microsphere of three-dimensional order for preparing.Figure (a) is overall for microsphere; Figure (b) is microsphere local.
Fig. 2 adopts the inventive method in step 2) the SEM figure and EDS of the three-dimensional order Nano silver grain cladding titanium dioxide photon crystal micro-ball prepared. Figure (a) schemes for SEM; Figure (b) is EDS.
Fig. 3 is that the SERS of mercaptobenzoic acid is schemed by end product of the present invention detection. Figure (a) is that the SERS of mercaptobenzoic acid is schemed by detection variable concentrations; Figure (b) is with 1340cm-1The canonical plotting of the SERS Strength Changes that peak is the concentration dependant that reference peak obtains at place.
Detailed description of the invention
One, in order to make the purpose of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is described in detail.
Embodiment 1
(1) the dioxide photon crystal microsphere of three-dimensional order is prepared: be blended in there-necked flask by the acetonitrile of the dehydrated alcohol of 75mL and 50mL, it is subsequently added the ammonia of 190uL and the water of 455uL, 1.25mL butyl titanate is rapidly joined when being stirred vigorously, 30 degree of constant temperature are stirred vigorously 6h, and reaction terminates rear centrifuge washing and obtains titanium dioxide nano-particle solution. solution is sucked by the certain density titanium dioxide nano-particle solution of preparation after ultrasonic disperse half an hour in the syringe of 1mL, draw low viscosity methyl-silicone oil about 25ml with 25mL syringe simultaneously, syringe is connected on the interface singly pushing away syringe pump apparatus of correspondence, and with impeller driven syringe, the flow velocity of design colloid solution is 0.5ml/h, and the flow velocity of silicone oil is 10ml/h. emulsion is dripped into microsphere in the catcher equipped with full-bodied methyl-silicone oil by micro fluidic device, after all drops all settlement stabilities, slowly mobile container of collecting is statically placed in 36h in the baking oven of 60 DEG C, the water treated in drop evaporates completely, until completing the crystallization of colloidal crystal microsphere, after forming the colloidal crystal microsphere of close-packed structure, take out container, after to be cooled, gradually dilute remaining methyl-silicone oil again with normal hexane after silicone oil is poured out a part, after repeatedly washing (to remove the silicone oil in microsphere surface residual), after colloidal crystal microsphere being taken out natural drying with pipet, it is placed in Muffle furnace again in 600 DEG C of calcinings,
(2) three-dimensional order Nano silver grain cladding titanium dioxide photon crystal micro-ball is prepared: the dioxide photon crystal microsphere 0.004g taking above-mentioned three-dimensional order is placed in 50mL politef reactor, add the silver nitrate aqueous solution (0.074mol/L) of 20mL, hydro-thermal reaction 24h at 130 DEG C, takes out nature by product and dries.
Embodiment 2
(1) the dioxide photon crystal microsphere of three-dimensional order is prepared: be blended in there-necked flask by the acetonitrile of the dehydrated alcohol of 75mL and 50mL, it is subsequently added the ammonia of 190uL and the water of 455uL, 1.25mL butyl titanate is rapidly joined when being stirred vigorously, 30 degree of constant temperature are stirred vigorously 6h, and reaction terminates rear centrifuge washing and obtains titanium dioxide nano-particle solution. solution is sucked by the certain density titanium dioxide nano-particle solution of preparation after ultrasonic disperse half an hour in the syringe of 1mL, draw low viscosity methyl-silicone oil about 25ml with 25mL syringe simultaneously, syringe is connected on the interface singly pushing away syringe pump apparatus of correspondence, and with impeller driven syringe, the flow velocity of design colloid solution is 1ml/h, and the flow velocity of silicone oil is 5ml/h. emulsion is dripped into microsphere in the catcher equipped with full-bodied methyl-silicone oil by micro fluidic device, after all drops all settlement stabilities, slowly mobile container of collecting is statically placed in 60h in the baking oven of 40 DEG C, the water treated in drop evaporates completely, until completing the crystallization of colloidal crystal microsphere, after forming the colloidal crystal microsphere of close-packed structure, take out container, after to be cooled, gradually dilute remaining methyl-silicone oil again with normal hexane after silicone oil is poured out a part, after repeatedly washing (to remove the silicone oil in microsphere surface residual), after colloidal crystal microsphere being taken out natural drying with pipet, it is placed in Muffle furnace again in 400 DEG C of calcinings,
(2) three-dimensional order Nano silver grain cladding titanium dioxide photon crystal micro-ball is prepared: the dioxide photon crystal microsphere 0.004g taking above-mentioned three-dimensional order is placed in 50mL politef reactor, add the silver nitrate aqueous solution (0.015mol/L) of 20mL, hydro-thermal reaction 20h at 150 DEG C, takes out nature by product and dries.
Embodiment 3
(1) three-dimensional order Nano silver grain cladding titanium dioxide photon crystal micro-ball is prepared: be blended in there-necked flask by the acetonitrile of the dehydrated alcohol of 75mL and 50mL, it is subsequently added the ammonia of 190uL and the water of 455uL, 1.25mL butyl titanate is rapidly joined when being stirred vigorously, 30 degree of constant temperature are stirred vigorously 6h, and reaction terminates rear centrifuge washing and obtains titanium dioxide nano-particle solution. solution is sucked by the certain density titanium dioxide nano-particle solution of preparation after ultrasonic disperse half an hour in the syringe of 1mL, draw low viscosity methyl-silicone oil about 25ml with 25mL syringe simultaneously, syringe is connected on the interface singly pushing away syringe pump apparatus of correspondence, and with impeller driven syringe, the flow velocity of design colloid solution is 2ml/h, and the flow velocity of silicone oil is 50ml/h. emulsion is dripped into microsphere in the catcher equipped with full-bodied methyl-silicone oil by micro fluidic device, after all drops all settlement stabilities, slowly mobile container of collecting is statically placed in 48h in the baking oven of 50 DEG C, the water treated in drop evaporates completely, until completing the crystallization of colloidal crystal microsphere, after forming the colloidal crystal microsphere of close-packed structure, take out container, after to be cooled, gradually dilute remaining methyl-silicone oil again with normal hexane after silicone oil is poured out a part, after repeatedly washing (to remove the silicone oil in microsphere surface residual), after colloidal crystal microsphere being taken out natural drying with pipet, it is placed in Muffle furnace again in 800 DEG C of calcinings,
(2) three-dimensional order Nano silver grain cladding titanium dioxide photon crystal micro-ball is prepared: take above-mentioned three-dimensional order Nano silver grain cladding titanium dioxide photon crystal micro-ball 0.004g and be placed in 50mL politef reactor, add the silver nitrate aqueous solution (0.22mol/L) of 20mL, hydro-thermal reaction 28h at 100 DEG C, takes out nature by product and dries.
Two, product property:
Fig. 1 adopts the inventive method in step 1) the SEM figure of the dioxide photon crystal microsphere of three-dimensional order for preparing. It is good spherical that figure (a) shows that microsphere entirety has, and (b) shows that microsphere local becomes three-dimensional dioxide photon crystal microsphere with the structure dense accumulation of Hexagonal packing, and the homogeneous arrangement of size is regular.
Fig. 2 adopts the inventive method in step 2) the SEM figure and EDS of the three-dimensional order Nano silver grain cladding titanium dioxide photon crystal micro-ball prepared. After modifying upper silver nano-grain as Suo Shi (a) figure, microsphere local remains in that the structure of Hexagonal packing, compound with regular structure. Can significantly find out that from (b) figure power spectrum modified by silver nanoparticles is at dioxide photon crystal microsphere surface.
Fig. 3 is that the SERS of mercaptobenzoic acid is schemed by end product of the present invention detection. 2 �� 10 can be reached using Monitoring lower-cut during to mercaptobenzoic acid as probe molecule-16M, its enhancer is 4.8 �� 105. Being adsorbed on the three-dimensional order Nano silver grain cladding titanium dioxide photon crystal micro-ball of preparation when can be seen that mercaptobenzoic acid as probe molecule as shown in (a) figure detection range is 2 �� 10-6M��2 �� 10-16M, Monitoring lower-cut has reached 2 �� 10-16M, and baseline stationary nature peak is obvious;B () figure is with 1340cm-1The canonical plotting of the SERS Strength Changes that peak is the concentration dependant that reference peak obtains at place, detection limit wider range when the material that as seen from the figure prepared by the present invention is as Raman detection substrate, linear fit relation is good.
Claims (8)
1. the preparation method of a three-dimensional order Nano silver grain cladding titanium dioxide photon crystal micro-ball, it is characterised in that comprise the steps of
1) prepare the dioxide photon crystal microsphere of three-dimensional order: by titanium dioxide nano-particle solution after ultrasonic disperse by solution inhalation syringe; Draw low viscosity methyl-silicone oil with syringe simultaneously; Syringe is connected on the interface singly pushing away syringe pump apparatus of correspondence, and with impeller driven syringe, separately designs the flow velocity of colloid solution and silicone oil; Produce steady and continuous emulsion droplet by micro fluidic device and form microsphere from sedimentation, dry calcining;
2) prepare the Nano silver grain cladding titanium dioxide photon crystal micro-ball of three-dimensional order: the above-mentioned dioxide photon crystal microsphere preparing three-dimensional order is placed in polymeric kettle, add silver nitrate aqueous solution high-temperature water thermal response, take out nature and dry.
2. preparation method according to claim 1, it is characterised in that described step 1) in prepare three-dimensional order the mass percentage concentration of titanium dioxide nano-particle solution of dioxide photon crystal microsphere be 5%��15%.
3. preparation method according to claim 1, it is characterized in that described step 1) in prepare three-dimensional order the flow velocity of titanium dioxide nano-particle solution of dioxide photon crystal microsphere be 0.5mL/h��2mL/h, the flow velocity of silicone oil is 5ml/h��50ml/h.
4. preparation method according to claim 1, it is characterised in that the temperature conditions of described drying is 40��60 DEG C, drying time 36��60h.
5. preparation method according to claim 1, it is characterised in that the temperature conditions of described calcining is 400��800 DEG C.
6. preparation method according to claim 1, it is characterised in that described step 2) in the mass ratio that feeds intake of silver nitrate aqueous solution and the dioxide photon crystal microsphere of three-dimensional order be 12.5��187.5:1.
7. preparation method according to claim 1 or 6, it is characterised in that the concentration of described silver nitrate aqueous solution is 0.015mol/L��0.22mol/L.
8. preparation method according to claim 1, it is characterised in that described step 2) in hydrothermal temperature be 100��150 DEG C, the response time is 20��28h.
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Cited By (9)
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| CN106179141A (en) * | 2016-07-25 | 2016-12-07 | 华南师范大学 | A kind of microsphere with Raman active and preparation method thereof |
| CN106290303A (en) * | 2016-08-11 | 2017-01-04 | 扬州大学 | A kind of multicomponent Raman spectrum method for detecting surface reinforcement based on composite photonic crystal microsphere |
| CN108896530A (en) * | 2018-06-29 | 2018-11-27 | 上海交通大学 | A kind of preparation method of Raman spectrum detection substrate |
| CN108893777A (en) * | 2018-06-27 | 2018-11-27 | 武汉理工大学 | A kind of preparation method and application of the titanium dioxide inverse opal photonic crystal microballoon of three-dimensional order |
| CN110441284A (en) * | 2019-07-23 | 2019-11-12 | 海南大学 | The preparation method and products obtained therefrom of a kind of Surface enhanced Raman scattering chip can be used for trace detection and application |
| CN110465317A (en) * | 2018-10-18 | 2019-11-19 | 黑龙江大学 | A kind of photochemical catalyst g-C3N4/ GO/ magnetic particle and preparation method thereof |
| CN112289871A (en) * | 2020-10-27 | 2021-01-29 | 山西大学 | Laminated photonic crystal with optical performance regulation and control function and preparation method thereof |
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| CN113737281A (en) * | 2021-08-31 | 2021-12-03 | 武汉理工大学 | Oxide spherical photonic crystal with inverse opal structure, simple preparation method and application thereof |
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| CN106179141B (en) * | 2016-07-25 | 2019-04-30 | 华南师范大学 | A kind of microballoon and preparation method thereof with Raman active |
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| CN108893777A (en) * | 2018-06-27 | 2018-11-27 | 武汉理工大学 | A kind of preparation method and application of the titanium dioxide inverse opal photonic crystal microballoon of three-dimensional order |
| CN108896530A (en) * | 2018-06-29 | 2018-11-27 | 上海交通大学 | A kind of preparation method of Raman spectrum detection substrate |
| CN110465317A (en) * | 2018-10-18 | 2019-11-19 | 黑龙江大学 | A kind of photochemical catalyst g-C3N4/ GO/ magnetic particle and preparation method thereof |
| CN110441284A (en) * | 2019-07-23 | 2019-11-12 | 海南大学 | The preparation method and products obtained therefrom of a kind of Surface enhanced Raman scattering chip can be used for trace detection and application |
| CN110441284B (en) * | 2019-07-23 | 2022-02-15 | 海南大学 | Preparation method of surface-enhanced Raman scattering chip for trace detection, obtained product and application |
| CN112289871A (en) * | 2020-10-27 | 2021-01-29 | 山西大学 | Laminated photonic crystal with optical performance regulation and control function and preparation method thereof |
| CN113237867A (en) * | 2021-06-02 | 2021-08-10 | 江南大学 | Device and method for preparing surface enhanced Raman substrate by coupling micro-fluidic technology and plasma technology |
| CN113737281A (en) * | 2021-08-31 | 2021-12-03 | 武汉理工大学 | Oxide spherical photonic crystal with inverse opal structure, simple preparation method and application thereof |
| CN113737281B (en) * | 2021-08-31 | 2024-04-26 | 武汉理工大学 | Oxide spherical photonic crystal with inverse opal structure, simple preparation method and application thereof |
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