CN110484236A - The preparation method of bismuth quanta point material is grown in a kind of mesoporous silica nano-particle - Google Patents
The preparation method of bismuth quanta point material is grown in a kind of mesoporous silica nano-particle Download PDFInfo
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- CN110484236A CN110484236A CN201910709960.8A CN201910709960A CN110484236A CN 110484236 A CN110484236 A CN 110484236A CN 201910709960 A CN201910709960 A CN 201910709960A CN 110484236 A CN110484236 A CN 110484236A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C09K11/74—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing arsenic, antimony or bismuth
Abstract
The invention discloses the preparation methods that bismuth quanta point material is grown in a kind of mesoporous silica nano-particle, belong to nano material preparation research field.This method prepares mesoporous silicon oxide using organic formwork, and grows bismuth quantum dot in in-situ reducing, so that the partial size that mesoporous silicon oxide is prepared is about 150nm, aperture is about 10nm, bismuth quantum point grain diameter about 1-2nm.Mesoporous silicon oxide using this method preparation has excellent absorption property, and has good protective effect to bismuth, improves the photothermal conversion efficiency of bismuth, has broad application prospects in fields such as electronic device, sensor, pharmaceutical carriers.Bismuth quantum dot (the Bi@SiO grown in mesoporous monox nanometer particle using this method preparation2), there is excellent photothermal conversion performance, have a high potential in tumor thermal therapy field.Preparation method equipment provided by the invention is simple, and has many advantages, such as easy control of process conditions, low in cost.
Description
Technical field
The invention belongs to inorganic nanoparticles field of material technology, and in particular to raw in a kind of mesoporous monox nanometer particle
Long bismuth quantum dot (Bi@SiO2) material preparation method.
Background technique
Porous material has many advantages, such as biggish specific surface area, biggish pore volume, lower density, is widely used in
The fields such as adsorbing separation, catalysis, electrochemistry, biological medicine, optics and electronic device.It is mesoporous compared with other porous materials
Silica has more excellent performance, such as has adjustable morphology and size size, cellular structure high-sequential, aperture is big
Small to be uniformly distributed, high porosity and big specific surface area, it is easy, nontoxic, stable, cheap etc. that surface is modified, so that mesoporous two
Silica has a good application prospect in catalysis, sensor, pharmaceutical carrier field.
When silica is as pharmaceutical carrier, drug load capability and its pattern have close contact with structure.
In various patterns, mesoporous nano SiO 2 particle material shows the distinguishing feature better than other patterns, such as: (1)
High specific surface area allows it to adsorb a large amount of chemical substance；(2) it is more to allow it to load for big cellular structure
Drug；(3) surface group rich is easy to be modified.
Organic formwork method is widely used in preparing mesopore silicon oxide, but it has several drawbacks in that: (1) preparation process is complicated
(2) nano particle (3) aperture that can not prepare the controlled dimensions less than 200nm is less than 5nm more.And the present invention uses a kind of acetic acid
Ethyl ester can synthesize the nano SiO 2 particle in controllable aperture and partial size as expanding agent.And equipment is simple, operation letter
It is single, it is low in cost, therefore, mesoporous silica nano-particle is used to prepare with good prospect.
Bismuth is a kind of " green " metal, is widely used in tumor thermal therapy field.Photo-thermal therapy is a kind of based on light
The therapeutic modality of thermit powder, under the excitation of suitable outfield light source, light thermit powder can locally generate higher temperature, and then realize tumour
The even necrosis of the apoptosis of cell.The selection principle of ideal light thermit powder is based on nontoxic, photothermal conversion efficiency height, low cost, system
The advantages that standby simple.And bismuth has very strong absorption near infrared light, so bismuth is a kind of good light thermit powder, and bismuth is due to original
Sub- ordinal number is higher, can serve as the contrast medium of CT imaging.But bismuth is oxidized easily, it can not be real using present preparation method
Now it is effectively protected.And the present invention can be good at protecting using the method preparation of the in-situ reducing in mesoporous silicon oxide duct
Protect bismuth quantum dot, the Bi@SiO of synthesis2With very high photothermal conversion efficiency, there is very big application in tumor thermal therapy field
Prospect.
Summary of the invention
The object of the present invention is to provide a kind of mesoporous silica nano-particles to grow bismuth quantum dot (Bi@SiO2) material
Preparation method successfully synthesizes the nanometer with controllable aperture (10nm) and partial size (150nm) using organic formwork method
Grain.Using local reduction way, the successful growth 1-2nm bismuth quantum dot in silica duct.
The purpose of the present invention is what is be achieved through the following technical solutions: a kind of mesoporous silica nano-particle growth bismuth amount
Sub- point (Bi@SiO2) material preparation method, comprising the following steps:
(1) 200mg cetyl trimethylammonium bromide is weighed to be dissolved in 10ml deionized water, magnetic agitation until dissolution,
Obtain the first solution.
(2) 20ml ethyl acetate, 5ml methanol and 3ml ammonium hydroxide are sequentially added into 95ml deionized water, and it is molten to obtain second
Liquid.
(3) under stirring, the first solution is added dropwise into the second solution, obtains third solution.
(4) under stirring, 0.5ml tetraethyl orthosilicate is added dropwise into third solution, is then stirred at room temperature 12 hours,
Obtain mesoporous silicon oxide solution.
(5) the mesoporous silicon oxide solution that step (4) obtains is mixed with the ethyl alcohol of 100ml or more, is centrifuged, the speed of centrifugation
Rate 10000rpm, the time 6 minutes, then mesoporous silica particles are dispersed in water again, obtain mesoporous silicon oxide solution.
(6) the mesoporous silicon oxide solution for obtaining step (5) is placed in 550 DEG C of air and anneals 3 hours, obtains mesoporous
Nano SiO 2 particle.
(7) it takes 30mg mesoporous silica particles to be dissolved in 15ml deionized water, obtains mesoporous silicon oxide solution, for use.
(8) 300mg polyvinylpyrrolidone (PVP) and 100mg bismuth nitrate (Bi (NO are weighed3)3·5H2O) it is dissolved in 10ml second
Alcohol, stirring and dissolving under the conditions of 55 DEG C, obtains the 4th solution.
(9) solution 4 is added in the resulting mesoporous silicon oxide solution of step (7), ultrasound makes the 4th solution enter Jie
In the duct of hole silica, 10mM NaBH is added410ml stirs 1min, obtains Bi@SiO2Solution.
(10) the Bi@SiO for obtaining step (9)2Solution centrifugation, centrifugation rate 10000rpm, the time 3 minutes, washing obtained
To Bi@SiO2。
Further, the Bi@SiO2Middle silica is meso-hole structure, wraps up bismuth quantum dot, the meso-porous titanium dioxide
The partial size of silicon is 150nm, aperture 10nm, bismuth quantum dot 1-2nm.
Compared with prior art, the invention has the advantages that: the present invention is prepared for having using organic formwork method
The mesoporous silica nano-particle in controllable aperture (10nm) and partial size (150nm).Using local reduction way, in silica
Successful growth 1-2nm bismuth quantum dot in duct.The hydrolytic condensation that the method is related to tetraethyl orthosilicate forms silica.System
Standby process has used ethyl acetate as expanding agent and cetyl trimethylammonium bromide as surfactant.Silicon positive first
Sour tetra-ethyl ester is hydrolyzed into silicate, then between silicate electronegative in the system and cationic surface active agent CTAB
It is self-assembled into silicate micella by electrostatic interaction, mesoporous silica nanospheres can be obtained in the environment of ammonium hydroxide.And add
Add ethyl acetate, the aperture of silica can be expanded.Present invention employs simple organic formwork method, it is prepared for uniformly,
The mesoporous silica nano-particle of stable structure.The mesoporous silica nano-particle has excellent absorption property, in electricity
Sub- device, sensor, the fields such as pharmaceutical carrier have broad application prospects.The mesoporous monox nanometer prepared using this method
Bismuth quantum dot (Bi@SiO is grown in particle2), there is excellent photothermal conversion performance, have in tumor thermal therapy field very big
Application prospect, and silica has good protective effect to bismuth, improves the photothermal conversion efficiency of bismuth.Method of the invention
Equipment is simple, easy to operate, easily controllable, low in cost.
Detailed description of the invention
Fig. 1 is the SEM figure of the mesoporous silica nano-particle of preparation；
Fig. 2 is the TEM figure of the mesoporous silica nano-particle of preparation；
Fig. 3 is that bismuth quantum dot (Bi@SiO is grown in the mesoporous silica nano-particle of preparation2) SEM figure；
Fig. 4 is that bismuth quantum dot (Bi@SiO is grown in the mesoporous silica nano-particle of preparation2) TEM figure；
Fig. 5 is the mesoporous silica nano-particle that example 1 obtains and the mesoporous silica nano-particle that example 2 obtains
Middle growth bismuth quantum dot (Bi@SiO2) BET analyze result；
Bismuth quantum dot (Bi@SiO is grown in the mesoporous silica nano-particle that Fig. 6 obtains for example 22) and PVP-Bi amount
Son point places 0 day and 4 days in water XRD diagram；
Fig. 7 is the situation of change for recording temperature under different irradiation times with thermal infrared imager: (a) being the Bi@of various concentration
SiO2Nano particle is in 808nm laser (1W/cm2) curve that changes over time of temperature under irradiation；It (b) is the Bi@of various concentration
SiO2Nano particle is in 808nm laser (1W/cm2) irradiation under thermal imaging photo；(c) the Bi@SiO for being 400 μ g/ml2Nanometer
Grain is in 808nm laser (1W/cm2) under irradiate 900s heating curve and natural cooling temperature lowering curve；It (d) is time and-ln θ
Linear fit relationship.
Specific embodiment
Below in conjunction with drawings and examples, invention is further explained.
A kind of mesoporous silica nano-particle provided by the present invention grows bismuth quantum dot (Bi@SiO2) material preparation
Method is specifically included using the mesoporous silica nano-particle in aperture and partial size that organic formwork method is prepared for having controllable
Following steps:
(1) 200mg cetyl trimethylammonium bromide is weighed to be dissolved in 10ml deionized water, magnetic agitation until dissolution,
Obtain the first solution.
(2) 20ml ethyl acetate, 5ml methanol and 3ml ammonium hydroxide are sequentially added into 95ml deionized water, and it is molten to obtain second
Liquid.
(3) under stirring, the first solution is added dropwise into the second solution, obtains third solution.
(4) under stirring, 0.5ml tetraethyl orthosilicate is added dropwise into third solution, is then stirred at room temperature 12 hours,
Obtain mesoporous silicon oxide solution.
(5) the above ethyl alcohol centrifugation of the mesoporous silicon oxide solution 11ml obtained step (4), the rate of centrifugation
10000rpm, the time 6 minutes, then mesoporous silica particles are dispersed in water again, obtain mesoporous silicon oxide solution.
(6) the mesoporous silicon oxide solution for obtaining step (5) is placed in 550 DEG C of air and anneals 3 hours, obtains mesoporous
Nano SiO 2 particle.
The mesoporous silica nano-particle that the above method is prepared is as shown in Figure 1.As can be seen from Figure, mesoporous two
The partial size of silica nano particle is about 150nm, and aperture is about 10nm, uniform particle sizes, as shown in figures 1 and 2.
Fig. 3,4 grow bismuth quantum dot for preparation method provided by the present invention mesoporous silica nano-particle obtained.
Its preparation process specifically includes:
(7) it takes 30mg mesoporous silica particles to be dissolved in 15ml deionized water, obtains mesoporous silicon oxide solution, for use.
(8) 300mg polyvinylpyrrolidone (PVP) and 100mg bismuth nitrate (Bi (NO are weighed3)3·5H2O) it is dissolved in 10ml second
Alcohol, stirring and dissolving under the conditions of 55 DEG C, obtains the 4th solution.
(9) the 4th solution is added in the resulting mesoporous silicon oxide solution of step (7), ultrasound enters the 4th solution
In the duct of mesoporous silicon oxide, 10mM NaBH is added410ml is vigorously stirred 1min, obtains Bi@SiO2Solution.
(10) the Bi@SiO for obtaining step (9)2Solution centrifugation, centrifugation rate 10000rpm, the time 3 minutes, washing obtained
To Bi@SiO2。
The silica dioxide granule size that grown bismuth quantum dot it can be seen from Fig. 3,4 is almost unchanged, but surface becomes
Coarse, aperture becomes larger, it may be possible to since bismuth quantum dot is grown in the duct of silica, so the duct to silica has
Certain destruction；It is also possible that because sodium borohydride aqueous solution be it is alkaline, have certain corrosiveness for silica.
Fig. 5 is that bismuth quantum dot (Bi@is grown in mesoporous silica nano-particle and mesoporous silica nano-particle
SiO2) BET result.By the figure it will also be appreciated that the aperture of silica becomes larger after growth bismuth, specific surface area reduces.
Bismuth quantum dot (Bi@SiO is grown in mesoporous silica nano-particle2) and PVP-Bi quantum dot place in water 0
The XRD spectrum of it and 4 days is as shown in fig. 6, as can be seen from Figure, the bismuth quantum dot for having silica to protect is placed in water
It four days, is not also oxidized, and PVP-Bi quantum dot 4 days have been oxidized to Bi2O2CO3.Therefore, one provided by the invention
Kind mesoporous silica nano-particle grows bismuth quantum dot (Bi@SiO2) material property is more stable.
By Bi@SiO2The aqueous solution that nano particle is configured to various concentration is placed in 24 orifice plates, concentration gradient 25,50,
100,200,400 μ g/mL, deionized water is as control.With laser (the power density 1W/cm of 808nm2) irradiation it is not same
The aqueous solution of product, with the situation of change of thermal infrared imager record temperature under different irradiation times.Fig. 7 (a) is various concentration
Bi@SiO2Nano particle is in 808nm laser (1W/cm2) curve (b) that changes over time of the lower temperature of irradiation is various concentration
Bi@SiO2Nano particle is in 808nm laser (1W/cm2) irradiation under thermal imaging photo.With the laser (power density of 808nm
For 1W/cm2) irradiation 400 μ g/mL Bi@SiO2Aqueous solution 900s, then stop irradiation, natural cooling uses infrared thermal imaging
The variation of instrument record temperature.Fig. 7 (c) is the Bi@SiO of 400 μ g/ml2Nano particle is in 808nm laser (1W/cm2) under irradiate
The heating curve of 900s and the temperature lowering curve of natural cooling.
From Fig. 7 (a), it can be seen that, under 808nm laser 10min irradiation, the temperature of water increases only 1.3 DEG C, can ignore
Disregard, and the Bi@SiO of 400 μ g/mL2Nanoparticles solution can rise 31.5 DEG C respectively, show Bi@SiO2Nano particle is certain
With preferable photothermal conversion performance, stronger photothermy is shown.Bi@SiO can be calculated according to Fig. 7 (c)2Nano particle
Photothermal conversion efficiency.It can be obtained by photothermal conversion efficiency η further according to Fig. 7 (d).By calculating, Bi@SiO2Nano particle
Photothermal conversion efficiency is~43%.This is than the photothermal conversion efficiency (30%) of PVP-Bi quantum dot in document and many common
Optothermal material (such as gold nanorods (21%), gold nano grain (11%), MoS2Nano particle (27.6%) etc.) photothermal conversion
Efficiency wants high.Due to its outstanding light thermal property, so Bi@SiO2Nano particle has very big in terms of the photo-thermal therapy of tumour
Prospect.
Claims (2)
1. growing bismuth quantum dot (Bi@SiO in a kind of mesoporous silica nano-particle2) material preparation method, feature exists
In, specifically includes the following steps:
(1) it weighs 200mg cetyl trimethylammonium bromide to be dissolved in 10ml deionized water, magnetic agitation obtains until dissolution
First solution.
(2) 20ml ethyl acetate, 5ml methanol and 3ml ammonium hydroxide are sequentially added into 95ml deionized water, obtain the second solution.
(3) under stirring, the first solution is added dropwise into the second solution, obtains third solution.
(4) under stirring, 0.5ml tetraethyl orthosilicate is added dropwise into third solution, is then stirred at room temperature 12 hours, obtains
Mesoporous silicon oxide solution.
(5) the mesoporous silicon oxide solution that step (4) obtains is mixed with the ethyl alcohol of 100ml or more, is centrifuged, the rate of centrifugation
10000rpm, the time 6 minutes, then mesoporous silica particles are dispersed in water again, obtain mesoporous silicon oxide solution.
(6) the mesoporous silicon oxide solution for obtaining step (5) is placed in 550 DEG C of air and anneals 3 hours, obtains mesoporous dioxy
SiClx nano particle.
(7) it takes 30mg mesoporous silica particles to be dissolved in 15ml deionized water, obtains mesoporous silicon oxide solution, for use.
(8) 300mg polyvinylpyrrolidone (PVP) and 100mg bismuth nitrate (Bi (NO are weighed3)3·5H2O it) is dissolved in 10ml ethyl alcohol,
Stirring and dissolving under the conditions of 55 DEG C, obtains the 4th solution.
(9) solution 4 is added in the resulting mesoporous silicon oxide solution of step (7), ultrasound makes the 4th solution enter mesoporous two
In the duct of silica, 10mM NaBH is added410ml stirs 1min, obtains Bi@SiO2Solution.
(10) the Bi@SiO for obtaining step (9)2Solution centrifugation, the rate 10000rpm of centrifugation, the time 3 minutes, washing obtained
Bi@SiO2。
2. preparation method according to claim 1, which is characterized in that the Bi@SiO2Middle silica is meso-hole structure, packet
Bismuth quantum dot is wrapped up in, the partial size of the mesoporous silicon oxide is 150nm, aperture 10nm, bismuth quantum dot 1-2nm.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110898234A (en) * | 2019-12-25 | 2020-03-24 | 河南大学 | Two-dimensional bismuth nano composite material and preparation method and application thereof |
| CN111317825A (en) * | 2020-03-06 | 2020-06-23 | 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 |
| CN112316140A (en) * | 2020-11-10 | 2021-02-05 | 哈尔滨工程大学 | Preparation method of Bi-DMSNs @ PCM multifunctional nano composite material |
| CN113768899A (en) * | 2021-09-29 | 2021-12-10 | 广东彼迪药业有限公司 | Colloidal bismuth pectin capsule and preparation method thereof |
| CN113955961A (en) * | 2021-10-18 | 2022-01-21 | 东南大学 | Preparation method of solid waste surface in-situ growth C-S-H gel |
| CN113998730A (en) * | 2021-11-01 | 2022-02-01 | 哈尔滨工程大学 | Preparation method of hollow mesoporous tin dioxide applied to oxygen vacancy in tumor diagnosis and treatment |
| CN115007207A (en) * | 2022-06-04 | 2022-09-06 | 哈尔滨理工大学 | Preparation of BiNPs/TpBpy composite material and photocatalytic carbon dioxide reduction |
| CN115532220A (en) * | 2021-06-29 | 2022-12-30 | 香港大学深圳研究院 | Mesoporous silica-based deoxidizer and preparation method and application thereof |
| CN116139284A (en) * | 2023-04-23 | 2023-05-23 | 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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| CN110898234A (en) * | 2019-12-25 | 2020-03-24 | 河南大学 | Two-dimensional bismuth nano composite material and preparation method and application thereof |
| CN111317825A (en) * | 2020-03-06 | 2020-06-23 | 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 |
| CN112316140A (en) * | 2020-11-10 | 2021-02-05 | 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 |
| CN115532220A (en) * | 2021-06-29 | 2022-12-30 | 香港大学深圳研究院 | Mesoporous silica-based deoxidizer and preparation method and application thereof |
| CN113768899A (en) * | 2021-09-29 | 2021-12-10 | 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 |
| CN113955961A (en) * | 2021-10-18 | 2022-01-21 | 东南大学 | Preparation method of solid waste surface in-situ growth C-S-H gel |
| CN113998730A (en) * | 2021-11-01 | 2022-02-01 | 哈尔滨工程大学 | Preparation method of hollow mesoporous tin dioxide applied to oxygen vacancy in tumor diagnosis and treatment |
| 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 |
| CN115007207A (en) * | 2022-06-04 | 2022-09-06 | 哈尔滨理工大学 | Preparation of BiNPs/TpBpy composite material and photocatalytic carbon dioxide reduction |
| 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 |
| CN116139284A (en) * | 2023-04-23 | 2023-05-23 | 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 |
| 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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