CN110484236B - Preparation method for growing bismuth quantum dot material in mesoporous silica nanoparticles - Google Patents
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- CN110484236B CN110484236B CN201910709960.8A CN201910709960A CN110484236B CN 110484236 B CN110484236 B CN 110484236B CN 201910709960 A CN201910709960 A CN 201910709960A CN 110484236 B CN110484236 B CN 110484236B
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Abstract
The invention discloses a preparation method of a bismuth quantum dot material growing in mesoporous silica nanoparticles, and belongs to the field of preparation research of nanomaterials. The method utilizes an organic template to prepare mesoporous silica, and reduces and grows bismuth quantum dots in situ, so that the prepared mesoporous silica has the particle size of about 150nm, the pore size of about 10nm and the particle size of about 1-2nm of the bismuth quantum dots. The mesoporous silica prepared by the method has excellent adsorption performance, has good protection effect on bismuth, improves the photothermal conversion efficiency of bismuth, and has wide application prospect in the fields of electronic devices, sensors, drug carriers and the like. Bismuth quantum dots (Bi @ SiO) grown in mesoporous silicon oxide nanoparticles prepared by adopting method2) Has excellent photo-thermal conversion performance and has great potential in the field of tumor photo-thermal treatment. The preparation method provided by the invention has the advantages of simple equipment, easy control of process conditions, low cost and the like.
Description
Technical Field
The invention belongs to the technical field of inorganic nano-particle materials, and particularly relates to a method for growing bismuth quantum dots (Bi @ SiO) in mesoporous silicon oxide nano-particles2) A method for preparing the material.
Background
The porous material has the advantages of large specific surface area, large pore volume, low density and the like, and is widely applied to the fields of adsorption separation, catalysis, electrochemistry, biomedicine, optics, electronic devices and the like. Compared with other porous materials, the mesoporous silica has more excellent performances, such as adjustable morphology and size, highly ordered pore structure, uniform distribution of pore size, high porosity and large specific surface area, easy surface modification, no toxicity, stability, cheapness and the like, so that the mesoporous silica has good application prospects in the fields of catalysis, sensors and drug carriers.
When the silicon dioxide is used as a drug carrier, the drug loading capacity and the morphology of the silicon dioxide are closely related to the structure. Among the various morphologies, mesoporous silica nanoparticle materials exhibit significant characteristics superior to other morphologies, such as: (1) the high specific surface area makes it possible to adsorb large amounts of chemical substances; (2) the large pore structure makes it possible to load more drug; (3) the surface groups are abundant, and the modification is easy to carry out.
The organic template method is widely used for preparing mesoporous silica, but it has several disadvantages: (1) the preparation process is complicated (2) the controllable size nano-particles smaller than 200nm can not be prepared (3) the aperture is more than 5 nm. The invention adopts ethyl acetate as a pore-enlarging agent, and can synthesize the silica nano-particles with controllable pore diameter and particle size. And the method has the advantages of simple equipment, simple operation and low cost, so the method has good prospect when being used for preparing the mesoporous silica nano particles.
Bismuth is a green metal and is widely applied to the field of tumor photothermal therapy. Photothermal therapy is a treatment mode based on a photothermal agent, and the photothermal agent can generate higher temperature locally under the excitation of a proper external field light source, so that the apoptosis and even the necrosis of tumor cells are realized. The ideal selection principle of the photo-thermal agent is based on the advantages of no toxicity, high photo-thermal conversion efficiency, low cost, simple preparation and the like. Bismuth has strong absorption to near infrared light, so bismuth is a good photo-thermal agent, and can be used as a contrast agent for CT imaging due to high atomic number. However, bismuth is easily oxidized, and effective protection cannot be achieved by the existing preparation method. The invention adopts the in-situ reduction method in the mesoporous silica pore channel to prepare the Bi @ SiO which can well protect the bismuth quantum dots and is synthesized2Has high photo-thermal conversion efficiency and has great application prospect in the field of tumor photo-thermal treatment.
Disclosure of Invention
The invention aims to provide a method for growing bismuth quantum dots (Bi @ SiO) by using mesoporous silica nanoparticles2) The preparation method of the material adopts an organic template method to successfully synthesize the nano-particles with controllable pore diameter (10nm) and particle size (150 nm). And (3) successfully growing 1-2nm bismuth quantum dots in the silicon dioxide pore channel by adopting an in-situ reduction method.
The purpose of the invention is realized by the following technical scheme: mesoporous silica nanoparticle grown bismuth quantum dot (Bi @ SiO)2) The preparation method of the material comprises the following steps:
(1) 200mg of cetyltrimethylammonium bromide was weighed and dissolved in 10ml of deionized water, and magnetically stirred until dissolved to obtain a first solution.
(2) To 95ml of deionized water were added 20ml of ethyl acetate, 5ml of methanol and 3ml of ammonia water in this order to obtain a second solution.
(3) And dropwise adding the first solution into the second solution under the stirring state to obtain a third solution.
(4) And dropwise adding 0.5ml of tetraethyl orthosilicate into the third solution under the stirring state, and then stirring at room temperature for 12 hours to obtain the mesoporous silica solution.
(5) And (3) mixing the mesoporous silica solution obtained in the step (4) with more than 100ml of ethanol, centrifuging at the speed of 10000rpm for 6 minutes, and then re-dispersing the mesoporous silica particles in water to obtain the mesoporous silica solution.
(6) And (3) annealing the mesoporous silica solution obtained in the step (5) in air at 550 ℃ for 3 hours to obtain the mesoporous silica nanoparticles.
(7) 30mg of mesoporous silica particles are dissolved in 15ml of deionized water to obtain a mesoporous silica solution for later use.
(8) 300mg of polyvinylpyrrolidone (PVP) and 100mg of bismuth nitrate (Bi (NO) were weighed out3)3·5H2O) was dissolved in 10ml of ethanol and dissolved at 55 ℃ with stirring to obtain a fourth solution.
(9) Adding the solution 4 into the mesoporous silica solution obtained in the step (7), performing ultrasonic treatment to enable the fourth solution to enter a pore channel of the mesoporous silica, and adding 10mM NaBH410ml, stirred for 1min to obtain Bi @ SiO2And (3) solution.
(10) Bi @ SiO obtained in the step (9)2Centrifuging the solution at a speed of 10000rpm for 3 minutes, and washing to obtain Bi @ SiO2。
Further, the Bi @ SiO2The mesoporous silica is of a mesoporous structure and wraps the bismuth quantum dots, the particle size of the mesoporous silica is 150nm, the pore diameter of the mesoporous silica is 10nm, and the bismuth quantum dots are 1-2 nm.
Compared with the prior art, the invention has the beneficial effects that: the invention adopts an organic template method to prepare mesoporous silica nano-particles with controllable aperture (10nm) and particle size (150 nm). By in-situ reductionAccording to the original method, 1-2nm bismuth quantum dots are successfully grown in the silicon dioxide pore channel. The process involves the hydrolytic condensation of tetraethylorthosilicate to form silica. The preparation process used ethyl acetate as a pore-expanding agent and cetyltrimethylammonium bromide as a surfactant. Firstly, tetraethyl orthosilicate is hydrolyzed into silicate, then silicate micelles are self-assembled between the silicate with negative electricity and cationic surfactant CTAB in the system through electrostatic interaction, and the mesoporous silica nanospheres can be obtained in the environment of ammonia water. The pore diameter of the silica can be enlarged by adding ethyl acetate. The invention adopts a simple organic template method to prepare uniform mesoporous silica nanoparticles with stable structure. The mesoporous silica nanoparticle has excellent adsorption performance and has wide application prospect in the fields of electronic devices, sensors, drug carriers and the like. Bismuth quantum dots (Bi @ SiO) grow in mesoporous silicon oxide nanoparticles prepared by adopting the method2) The bismuth-doped silicon dioxide has excellent photo-thermal conversion performance, has a great application prospect in the field of tumor photo-thermal treatment, has a good protection effect on bismuth by silicon dioxide, and improves the photo-thermal conversion efficiency of bismuth. The method has the advantages of simple equipment, simple operation, easy control and low cost.
Drawings
Fig. 1 is an SEM image of the prepared mesoporous silica nanoparticles;
FIG. 2 is a TEM image of the prepared mesoporous silica nanoparticles;
FIG. 3 shows the growth of bismuth quantum dots (Bi @ SiO) in the prepared mesoporous silica nanoparticles2) SEM picture of (1);
FIG. 4 shows the growth of bismuth quantum dots (Bi @ SiO) in the prepared mesoporous silica nanoparticles2) A TEM image of (B);
FIG. 5 shows mesoporous silica nanoparticles and bismuth quantum dots (Bi @ SiO) grown in the mesoporous silica nanoparticles2) BET analysis result of (a);
FIG. 6 shows the growth of bismuth quantum dots (Bi @ SiO) in mesoporous silica nanoparticles2) And XRD patterns of PVP-Bi quantum dots placed in water for 0 and 4 days;
FIG. 7 shows different illuminationsRecording the temperature change condition by using a thermal infrared imager under the time: (a) is Bi @ SiO of different concentrations2Laser (1W/cm) of nanoparticles at 808nm2) A plot of temperature under irradiation versus time; (b) is Bi @ SiO of different concentrations2Laser (1W/cm) of nanoparticles at 808nm2) A thermal image under illumination; (c) bi @ SiO in an amount of 400. mu.g/ml2Laser (1W/cm) of nanoparticles at 808nm2) A heating curve of lower irradiation for 900s and a cooling curve of natural cooling; (d) is a linear fit of time to-ln theta.
Detailed Description
The invention is further illustrated below with reference to the figures and examples.
The invention provides a method for growing bismuth quantum dots (Bi @ SiO) by using mesoporous silica nanoparticles2) The preparation method of the material adopts an organic template method to prepare the mesoporous silica nano-particles with controllable aperture and particle size, and specifically comprises the following steps:
(1) 200mg of cetyltrimethylammonium bromide was weighed and dissolved in 10ml of deionized water, and magnetically stirred until dissolved to obtain a first solution.
(2) To 95ml of deionized water were added 20ml of ethyl acetate, 5ml of methanol and 3ml of aqueous ammonia in this order to obtain a second solution.
(3) And dropwise adding the first solution into the second solution under the stirring state to obtain a third solution.
(4) And dropwise adding 0.5ml of tetraethyl orthosilicate into the third solution under the stirring state, and then stirring at room temperature for 12 hours to obtain the mesoporous silica solution.
(5) And (3) centrifuging the mesoporous silica solution obtained in the step (4) by using more than 11ml of ethanol at the speed of 10000rpm for 6 minutes, and then re-dispersing the mesoporous silica particles in water to obtain the mesoporous silica solution.
(6) And (3) annealing the mesoporous silica solution obtained in the step (5) in air at 550 ℃ for 3 hours to obtain the mesoporous silica nanoparticles.
The mesoporous silica nanoparticles prepared by the method are shown in figure 1. As can be seen from the figure, the mesoporous silica nanoparticles have a particle size of about 150nm, a pore size of about 10nm, and a uniform particle size, as shown in FIGS. 1 and 2.
Fig. 3 and 4 show bismuth quantum dots grown on mesoporous silica nanoparticles obtained by the preparation method provided by the invention. The preparation process specifically comprises the following steps:
(7) 30mg of mesoporous silica particles are dissolved in 15ml of deionized water to obtain a mesoporous silica solution for later use.
(8) 300mg of polyvinylpyrrolidone (PVP) and 100mg of bismuth nitrate (Bi (NO) were weighed out3)3·5H2O) was dissolved in 10ml of ethanol and dissolved at 55 ℃ with stirring to obtain a fourth solution.
(9) Adding the fourth solution into the mesoporous silica solution obtained in the step (7), performing ultrasonic treatment to enable the fourth solution to enter a pore channel of the mesoporous silica, and adding 10mM NaBH410ml, vigorously stirred for 1min to obtain Bi @ SiO2And (3) solution.
(10) Bi @ SiO obtained in the step (9)2Centrifuging the solution at a speed of 10000rpm for 3 minutes, and washing to obtain Bi @ SiO2。
As can be seen from fig. 3 and 4, the size of the silica particle on which the bismuth quantum dot grows is almost unchanged, but the surface becomes rough, the pore size becomes large, and probably because the bismuth quantum dot grows in the pore channel of the silica, the pore channel of the silica is damaged to some extent; it is also possible that the aqueous sodium borohydride solution is alkaline and has a corrosive effect on the silicon dioxide.
FIG. 5 shows mesoporous silica nanoparticles and bismuth quantum dots (Bi @ SiO) grown in the mesoporous silica nanoparticles2) The BET result of (1). From the same figure, it is also understood that the pore diameter of the silica becomes large and the specific surface area becomes small after bismuth is grown.
Growing bismuth quantum dots (Bi @ SiO) in mesoporous silica nanoparticles2) And the XRD patterns of the PVP-Bi quantum dots when placed in water for 0 day and 4 days are shown in figure 6, from which it can be seen that the bismuth quantum dots protected by silica, when placed in water for four days, are not oxidized, whereas the PVP-Bi quantum dots have been oxidized to Bi for 4 days2O2CO3. Therefore, the mesoporous silica nano particle provided by the invention grows bismuth quantum dots (Bi @ SiO)2) The material performance is more stable.
Adding Bi @ SiO2The nanoparticles were prepared as aqueous solutions of varying concentrations in a 24-well plate with a concentration gradient of 25, 50, 100, 200, 400. mu.g/m L, deionized water as a control, using a 808nm laser (power density of 1W/cm)2) And (3) irradiating the aqueous solutions of different samples, and recording the temperature change condition by using a thermal infrared imager under different irradiation time. FIG. 7(a) shows Bi @ SiO in different concentrations2Laser (1W/cm) of nanoparticles at 808nm2) The curve (b) of the temperature under irradiation as a function of time is Bi @ SiO at different concentrations2Laser (1W/cm) of nanoparticles at 808nm2) Photo of thermal imaging under illumination. Using a 808nm laser (power density 1W/cm)2) Irradiation of 400. mu.g/m L of Bi @ SiO2Then stopping irradiation, naturally cooling, and recording the temperature change by an infrared thermal imaging camera. FIG. 7(c) is a representation of Bi @ SiO at 400. mu.g/ml2Laser (1W/cm) of nanoparticles at 808nm2) The temperature rise curve of the lower irradiation time is 900s and the temperature drop curve of the natural cooling is carried out.
As can be seen from FIG. 7(a), the temperature rise of water under the irradiation of 808nm laser for 10min is only 1.3 ℃, which is negligible, and the Bi @ SiO of 400 mug/m L2The nanoparticle solutions can be raised by 31.5 ℃ respectively, indicating that Bi @ SiO2The nanoparticles have good photo-thermal conversion performance and show strong photo-thermal effect. From FIG. 7(c), Bi @ SiO can be calculated2Photothermal conversion efficiency η was obtained from FIG. 7 (d). The Bi @ SiO2The photo-thermal conversion efficiency of the nanoparticles was 43%. This compares the photo-thermal conversion efficiency (30%) of PVP-Bi quantum dots in the literature with many common photo-thermal materials (such as gold nanorods (21%), gold nanoparticles (11%), MoS)2Nanoparticles (27.6%), etc.) are high in light-to-heat conversion efficiency. Bi @ SiO due to its excellent photothermal properties2The nano-particles have great prospect in the aspect of photothermal treatment of tumors.
Claims (1)
1. ABismuth quantum dot Bi @ SiO grown in mesoporous silica nanoparticles2The preparation method of the material is characterized by comprising the following steps:
(1) 200mg of cetyltrimethylammonium bromide was weighed and dissolved in 10ml of deionized water, and magnetically stirred until dissolved to obtain a first solution.
(2) To 95ml of deionized water were added 20ml of ethyl acetate, 5ml of methanol and 3ml of ammonia water in this order to obtain a second solution.
(3) And dropwise adding the first solution into the second solution under the stirring state to obtain a third solution.
(4) And dropwise adding 0.5ml of tetraethyl orthosilicate into the third solution under the stirring state, and then stirring at room temperature for 12 hours to obtain the mesoporous silica solution.
(5) And (3) mixing the mesoporous silica solution obtained in the step (4) with more than 100ml of ethanol, centrifuging at the speed of 10000rpm for 6 minutes, and then re-dispersing the mesoporous silica particles in water to obtain the mesoporous silica solution.
(6) And (3) annealing the mesoporous silica solution obtained in the step (5) in air at 550 ℃ for 3 hours to obtain the mesoporous silica nanoparticles.
(7) 30mg of mesoporous silica particles are dissolved in 15ml of deionized water to obtain a mesoporous silica solution for later use.
(8) 300mg polyvinylpyrrolidone PVP and 100mg bismuth nitrate Bi (NO) were weighed3)3·5H2O is dissolved in 10ml of ethanol and stirred at 55 ℃ to obtain a fourth solution.
(9) Adding the solution 4 into the mesoporous silica solution obtained in the step (7), performing ultrasonic treatment to enable the fourth solution to enter a pore channel of the mesoporous silica, and adding 10mM NaBH410ml, stirred for 1min to obtain Bi @ SiO2And (3) solution.
(10) Bi @ SiO obtained in the step (9)2Centrifuging the solution at a speed of 10000rpm for 3 minutes, and washing to obtain Bi @ SiO2。
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| CN110898234B (en) * | 2019-12-25 | 2020-12-22 | 河南大学 | Two-dimensional bismuth nano composite material and preparation method and application thereof |
| CN111317825B (en) * | 2020-03-06 | 2021-08-24 | 南京市江宁医院 | Regularly folded ultra-small-size large-pore inorganic silicon macromolecular drug carrier, and preparation method and application thereof |
| CN112316140B (en) * | 2020-11-10 | 2022-10-28 | 哈尔滨工程大学 | Preparation method of Bi-DMSNs @ PCM multifunctional nano composite material |
| CN115532220B (en) * | 2021-06-29 | 2023-12-01 | 香港大学深圳研究院 | Mesoporous silica-based deoxidizer and preparation method and application thereof |
| CN113768899B (en) * | 2021-09-29 | 2023-06-27 | 广东彼迪药业有限公司 | Colloidal bismuth pectin capsule and preparation method thereof |
| CN113955961B (en) * | 2021-10-18 | 2023-03-17 | 东南大学 | Preparation method of solid waste surface in-situ growth C-S-H gel |
| CN113998730B (en) * | 2021-11-01 | 2023-09-19 | 哈尔滨工程大学 | Preparation method of hollow mesoporous tin dioxide applied to tumor diagnosis and treatment oxygen vacancy |
| CN115007207B (en) * | 2022-06-04 | 2023-11-21 | 哈尔滨理工大学 | Preparation of BiNPs/TpBpy composite material and photocatalytic carbon dioxide reduction |
| CN116139284B (en) * | 2023-04-23 | 2023-10-24 | 成都中医药大学 | Degradable bismuth-based inorganic nano material, preparation method and application thereof, and degradable drug-carrying delivery system mediated by degradable bismuth-based inorganic nano material |
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