CN102633304A - Bismuth sulfide nanorod with CT (computed tomography) angiography function, nano-composite material and preparation thereof - Google Patents
Bismuth sulfide nanorod with CT (computed tomography) angiography function, nano-composite material and preparation thereof Download PDFInfo
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Abstract
The invention discloses a bismuth sulfide nanorod with a CT (computed tomography) angiography function, a nano-composite material and preparation thereof. The preparation method of the bismuth sulfide nanorod comprises the following steps of: (1) dissolving bismuth chloride in a solvent in an ultrasonic manner to get a solution A; (2) dissolving sulfur powder or thiacetamide in the solvent in the ultrasonic manner to get a solution B; and (3) increasing the temperature of the solvent to 80-180 DEG C under the protection of argon, sequentially adding the solution A and the solution B, stirring to realize complete reaction, cooling, and then adding ethanol for centrifugation so as to get the bismuth sulfide nanorod, wherein the solvent is selected from oleyl amine, ethylene glycol and glycerin. The oleyl amine and a metal salt type compound are added into a toluene solution of the bismuth sulfide nanorod, stirring is performed at room temperature, and the ethanol is added for centrifugation so as to get the nano-composite material. The method disclosed by the invention is fast, simple and convenient, and the prepared bismuth sulfide nanorod and the nano-composite material thereof have the advantages of controllable appearance, uniform size and low cost and have excellent CT signals.
Description
Technical field
The present invention relates to the synthetic and application on the CT radiography of a kind of nano material, be specifically related to a kind of bismuth sulfide nano-rod, nano composite material and preparation method thereof.
Background technology
Bismuth sulfide (Bi
2S
3) as A
2 VB
3 VI(A=Sb, Bi, As; B=S; Se; Te) a kind of important semiconductor material in; On thermoelectric, electronics and opto-electronic device and electrochemical hydrogen storage, hydrogen sensor, have the potential using value, also have a wide range of applications simultaneously at aspects such as photochromics, nonlinear optical material, photocatalyst material, biological radiography material, coating materials.In recent years, Bi
2S
3The research of nano material mainly concentrates on the nanostructure that obtains different-shape and size; Comprise: nano wire, nanotube, nanometer rod, nanofiber, nanometer sheet, nanometer ball, nanometer flower and quantum dot etc.; These novel nanostructures often have particular performances separately, thereby are applied in fields such as photoelectricity, thermoelectricity, transmitter, biomolecule detection and biomedicine.The method of at present synthetic bismuth sulfide nano material has hydro-thermal (solvent thermal) method, electrochemical process, ultrasonic method, microwave method, solid phase method, co-precipitation etc.But from the preparation process, reaction conditions is relatively harsher, the reaction times is long; From the preparation effect, all there are some defectives in form, monodispersity.Like Weissleder; (the Nat.Mater.2006 of R seminar; 5,118 – 122) research shows that bismuth sulfide has excellent performance on the CT contrast medium, but because synthetic bismuth sulfide nano particle morphology is uncontrollable; The size heterogeneity, largely limit bismuth sulfide as the application of contrast medium on CT.Therefore, how to realize Bi
2S
3Fast and convenient, the pattern controlledly synthesis of nano material have become one of the focus in current nano materials research field.
Summary of the invention
Goal of the invention of the present invention provides a kind ofly has that excellent CT radiography function, pattern are controlled, the bismuth sulfide nano-rod and the nano composite material thereof of size homogeneous, and another goal of the invention of the present invention provides the fast and convenient preparation method of above-mentioned bismuth sulfide nano-rod and nano composite material thereof.
For reaching the foregoing invention purpose, the technical scheme that the present invention adopts is: a kind of preparation method of bismuth sulfide nano-rod of the CT of having radiography function, comprise the following steps: that (1) obtains solution A with the bismuth chloride ultrasonic dissolution in solvent, and concentration is 0.1～1M; (2) sulphur powder or thioacetamide ultrasonic dissolution are obtained solution B in solvent, concentration is 0.1～1M; (3) solvent is warming up to 80～180 ℃ under the protection of argon gas; Add solution A and solution B successively; Solvent and solution A, solution B volume ratio are 4: 1: 1, stir and make complete reaction, and it is centrifugal to add ethanol after the cooling; Obtain bismuth sulfide nano-rod, said solvent is selected from a kind of in oleyl amine, terepthaloyl moietie, the glycerine.
In the technique scheme, usually, when selecting oleyl amine as solvent for use, sulphur powder or thioacetamide can be selected in the sulphur source; And said solvent adds thioacetamide when being terepthaloyl moietie or glycerine in the step (2); In the step (3), before intensification, in solvent, add earlier Vinylpyrrolidone polymer.
Optimized technical scheme, churning time are 10 ~ 30 minutes.
The present invention asks for protection the bismuth sulfide nano-rod that adopts method for preparing to obtain simultaneously.
The application of above-mentioned bismuth sulfide nano-rod in the CT radiography adopts polyoxyethylene glycol that bismuth sulfide nano-rod is modified into the hydrophilic nano material, and as the CT contrast medium, the molecular weight of said polyoxyethylene glycol is 2000～10000.
A kind of preparation method with nano composite material of CT radiography function adopts above-mentioned bismuth sulfide nano-rod, is prepared into toluene dispersive solution; Concentration is 0.02～0.1M; Add oleyl amine and metal salt compound, the volume ratio of oleyl amine and toluene is 1: 1～1: 20, and the mass ratio of metal salt compound and bismuth sulfide nano-rod is 1: 2～1: 4; At room temperature stirred 1～12 hour; It is centrifugal to add ethanol, obtains said nano composite material, and said metal salt compound is selected from a kind of in hydrochloro-auric acid, Platinic chloride, silver acetate or the venus crystals.
The present invention asks for protection the nano composite material that adopts method for preparing to obtain simultaneously.
The application of above-mentioned nano composite material in the CT radiography adopts polyoxyethylene glycol that nano composite material is modified into the hydrophilic nano material, and as the CT contrast medium, the molecular weight of said polyoxyethylene glycol is 2000～10000.
Because the technique scheme utilization, the present invention compared with prior art has advantage:
1, the present invention adopts hot injection, is the bismuth source with the bismuth chloride, and sulphur powder or thioacetamide are the sulphur source,, has synthesized that pattern is controlled under certain condition, size homogeneous, bismuth sulfide nano-rod with low cost; Bismuth sulfide nano-rod and nano composite material nanoparticle shape thereof, the uppity present situation of size have been changed.
2, reaction conditions of the present invention is gentle, and the reaction times is short, and bismuth sulfide nano-rod just can generate in half a hour fully.
3, the bismuth sulfide nano rod composite material at room temperature promptly can generate, and wherein metal nanoparticle is uniformly dispersed.
4, bismuth sulfide nano-rod and nano composite material CT signal thereof are higher than the medical iodine reagent strength of signal of respective concentration, applicable to the CT contrast medium.This material has the potential using value on thermoelectric, electronics and opto-electronic device and electrochemical hydrogen storage, hydrogen sensor, also have a wide range of applications at aspects such as photochromics, nonlinear optical material, photocatalyst material, biological radiography materials simultaneously.
3, technical scheme of the present invention is applied widely, and preparing method's productive rate is high, and technology is simple, easy handling, and cost is lower, is suitable for applying.
Description of drawings
Fig. 1 is the TEM figure of the bismuth sulfide nano-rod that obtains of embodiment 1.
Fig. 2 is the XRD figure of the bismuth sulfide nano-rod that obtains of embodiment 1.
Fig. 3 is bismuth sulfide nano-rod TEM figure (A) 10min that embodiment 1 obtained in the differential responses time, (B) 20min, (C) 30min.
Fig. 4 be embodiment 1 in differential responses temperature (A) room temperature, (B) 80 ℃, (C) 120 ℃ TEM figure and differential responses thing (D) embodiment 2, (E) embodiment 3, (F) TEM of embodiment 1 schemes.
Fig. 5 is the TEM figure of the bismuth sulfide nano rod composite material that obtains of embodiment 4.
Fig. 6 is the CT image of different concns bismuth.
Fig. 7 is the contrast of CT signal value of different concns bismuth and the corresponding concentration iodine of two kinds of materials.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is further described.
The 80mL oleyl amine joins in the reaction flask, under the protection of argon gas, is warmed up to 170 ℃, under this temperature, keeps 20min.1.26g BiCl
3The ultrasonic 20mL of the being dissolved in oleyl amine of the ultrasonic 20mL of being dissolved in oleyl amine and 0.5g sulphur powder or 1.5g thioacetamide also joins in the there-necked flask stirring reaction 30min successively.Remove heating unit, be cooled to room temperature, add the ethanol spinning, the gained deposition is washed drying at room temperature again three times.Fig. 1 is the TEM figure of resulting product, and Fig. 2 is an XRD figure, prove to have obtained bismuth sulfide nano-rod, and Bi and S mol ratio is 2: 3.
Fig. 3 is bismuth sulfide nano-rod TEM figure (A) 10min that embodiment 1 obtained in the differential responses time, (B) 20min, (C) 30min.As can be seen from the figure, oleyl amine mutually in the synthetic bismuth sulfide nano-rod with the reaction times increase (10min, 20min, 30min), length elongated (~ 70nm, ~ 80nm, ~ 100nm).
Fig. 4 be embodiment 1 in differential responses temperature (A) room temperature, (B) 80 ℃, (C) 120 ℃ TEM figure and differential responses thing (D) embodiment 2, (E) embodiment 3, (F) TEM of embodiment 1 schemes.
Embodiment 2
80mL terepthaloyl moietie, 8g PVP (15K) join in the reaction flask, under the protection of argon gas, are warmed up to 170 ℃, under this temperature, keep 20min.1.26g BiCl
3The ultrasonic 20mL of the being dissolved in terepthaloyl moietie of the ultrasonic 20mL of being dissolved in terepthaloyl moietie and 1.5g thioacetamide also joins in the there-necked flask stirring reaction 30min successively.Remove heating unit, be cooled to room temperature, add the ethanol spinning, the gained deposition is washed drying at room temperature again three times.
Embodiment 3
80mL glycerine, 8g PVP (15K) join in the reaction flask, under the protection of argon gas, are warmed up to 170 ℃, under this temperature, keep 20min.1.26g BiCl
3The ultrasonic 20mL of the being dissolved in glycerine of the ultrasonic 20mL of being dissolved in glycerine and 1.5g thioacetamide also joins in the there-necked flask stirring reaction 30min successively.Remove heating unit, be cooled to room temperature, add the ethanol spinning, the gained deposition is washed drying at room temperature again three times.
Embodiment 4
Get the toluene 80mL dispersive solution of half the above-mentioned case study on implementation 3 or 4 bismuth sulfide nano-rods; Add 0.4g hydrochloro-auric acid (being dissolved in 40mL toluene and 8mL oleyl amine), at room temperature stirred 1 hour, add the ethanol spinning; The gained deposition is washed three times again, obtains the bismuth sulfide nano matrix material.
Fig. 5 is the TEM figure of the bismuth sulfide nano matrix material that obtains of embodiment 4.
Fig. 6 is the CT image of different concns bismuth.
Fig. 7 is the CT signal value of different concns bismuth and corresponding concentration iodine.
Visible from embodiment 1 to embodiment 4, the bismuth sulfide nano material that aforesaid method obtains is a club shaped structure, and the system of preparation feedback is selected, and comprises that reaction times, temperature have considerable influence for control nanometer rod size and dimension.Oleyl amine mutually in the synthetic bismuth sulfide nano-rod with the reaction times increase (10min, 20min, 30min), length elongated (~ 70nm, ~ 80nm, ~ 100nm); With decrease of temperature, the regularity variation; At 170 ℃, under the 30min condition, nanometer rod length ~ 100nm, diameter ~ 8 nm; Terepthaloyl moietie mutually in about 200 nm
10 nm; Glycerine mutually in about 300 nm
10 nm.Metal nanoparticle on the bismuth sulfide nano rod composite material is evenly dispersed in the bismuth sulfide nano-rod surface, and diameter is between 1 ~ 2nm.Hydrophilic bismuth sulfide nano-rod and nano composite material CT signal thereof are higher than the medical iodine reagent strength of signal of respective concentration.
Claims (8)
1. the preparation method with bismuth sulfide nano-rod of CT radiography function is characterized in that, comprises the following steps: that (1) obtains solution A with the bismuth chloride ultrasonic dissolution in solvent, and concentration is 0.1～1M; (2) sulphur powder or thioacetamide ultrasonic dissolution are obtained solution B in solvent, concentration is 0.1～1M; (3) solvent is warming up to 80～180 ℃ under the protection of argon gas; Add solution A and solution B successively; Solvent and solution A, solution B volume ratio are 4: 1: 1, stir and make complete reaction, and it is centrifugal to add ethanol after the cooling; Obtain bismuth sulfide nano-rod, said solvent is selected from a kind of in oleyl amine, terepthaloyl moietie, the glycerine.
2. the preparation method with bismuth sulfide nano-rod of CT radiography function according to claim 1 is characterized in that: said solvent is terepthaloyl moietie or glycerine, adds thioacetamide in the step (2); In the step (3), before intensification, in solvent, add earlier Vinylpyrrolidone polymer.
3. the preparation method with bismuth sulfide nano-rod of CT radiography function according to claim 1 is characterized in that: churning time is 10～30 minutes.
4. adopt the bismuth sulfide nano-rod that arbitrary method prepares in the claim 1 to 3.
5. the application of the described bismuth sulfide nano-rod of claim 4 in the CT radiography is characterized in that: adopt polyoxyethylene glycol that bismuth sulfide nano-rod is modified into the hydrophilic nano material, as the CT contrast medium, the molecular weight of said polyoxyethylene glycol is 2000～10000.
6. the preparation method with nano composite material of CT radiography function is characterized in that: adopt the described bismuth sulfide nano-rod of claim 4, be prepared into toluene dispersive solution; Concentration is 0.02～0.1M; Add oleyl amine and metal salt compound, the volume ratio of oleyl amine and toluene is 1: 1～1: 20, and the mass ratio of metal salt compound and bismuth sulfide nano-rod is 1: 2～1: 4; At room temperature stirred 1～12 hour; It is centrifugal to add ethanol, obtains said nano composite material, and said metal salt compound is selected from a kind of in hydrochloro-auric acid, Platinic chloride, silver acetate or the venus crystals.
7. the nano composite material that adopts the method for claim 6 to prepare.
8. the application of the described nano composite material of claim 7 in the CT radiography is characterized in that: adopting molecular weight is that 2000～10000 polyoxyethylene glycol is modified into the hydrophilic nano material with nano composite material, as the CT contrast medium.
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Cited By (7)
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| CN104491888A (en) * | 2014-12-18 | 2015-04-08 | 中国科学院上海硅酸盐研究所 | Multifunctional diagnosis and treatment agent based on MoS2/Bi2S3-PEG nanosheet as well as preparation method and application of multifunctional diagnosis and treatment agent |
| CN107158411A (en) * | 2017-03-31 | 2017-09-15 | 北京化工大学 | It is a kind of to be imaged the lower photo-thermal of guidance and the multifunctional nanocomposites of drug synergism and preparation method thereof for CT |
| CN109395106A (en) * | 2018-12-12 | 2019-03-01 | 华中科技大学 | A kind of nanometer bismuth ball cluster of stable structure and the preparation method and application thereof |
| CN110465311A (en) * | 2019-08-22 | 2019-11-19 | 青岛大学 | A kind of bismuth sulfide-palladium composite nano materials, preparation method and application |
| CN112472827A (en) * | 2020-11-27 | 2021-03-12 | 中国科学院大学宁波华美医院 | Novel bimodal PET/CT imaging material and preparation method and application thereof |
| CN112608747A (en) * | 2020-12-23 | 2021-04-06 | 武汉工程大学 | Bismuth sulfide fluorescent quantum dot and preparation method and application thereof |
| CN113772725A (en) * | 2020-06-10 | 2021-12-10 | 中国科学院宁波工业技术研究院慈溪生物医学工程研究所 | Bismuth-based semiconductor nano composite material, preparation method and application |
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| CN104491888A (en) * | 2014-12-18 | 2015-04-08 | 中国科学院上海硅酸盐研究所 | Multifunctional diagnosis and treatment agent based on MoS2/Bi2S3-PEG nanosheet as well as preparation method and application of multifunctional diagnosis and treatment agent |
| CN104491888B (en) * | 2014-12-18 | 2017-03-15 | 中国科学院上海硅酸盐研究所 | It is based on MoS2/Bi2S3Multi-functional diagnosis and treatment agent of PEG nanometer sheet and its preparation method and application |
| CN107158411A (en) * | 2017-03-31 | 2017-09-15 | 北京化工大学 | It is a kind of to be imaged the lower photo-thermal of guidance and the multifunctional nanocomposites of drug synergism and preparation method thereof for CT |
| CN109395106A (en) * | 2018-12-12 | 2019-03-01 | 华中科技大学 | A kind of nanometer bismuth ball cluster of stable structure and the preparation method and application thereof |
| CN109395106B (en) * | 2018-12-12 | 2021-04-20 | 华中科技大学 | Stable-structure nano bismuth ball cluster and preparation method and application thereof |
| CN110465311A (en) * | 2019-08-22 | 2019-11-19 | 青岛大学 | A kind of bismuth sulfide-palladium composite nano materials, preparation method and application |
| CN110465311B (en) * | 2019-08-22 | 2022-03-18 | 青岛大学 | Bismuth sulfide-palladium composite nanomaterial, preparation method and application |
| CN113772725A (en) * | 2020-06-10 | 2021-12-10 | 中国科学院宁波工业技术研究院慈溪生物医学工程研究所 | Bismuth-based semiconductor nano composite material, preparation method and application |
| CN113772725B (en) * | 2020-06-10 | 2023-06-06 | 中国科学院宁波工业技术研究院慈溪生物医学工程研究所 | Bismuth semiconductor nanocomposite, preparation method and application |
| CN112472827A (en) * | 2020-11-27 | 2021-03-12 | 中国科学院大学宁波华美医院 | Novel bimodal PET/CT imaging material and preparation method and application thereof |
| CN112608747A (en) * | 2020-12-23 | 2021-04-06 | 武汉工程大学 | Bismuth sulfide fluorescent quantum dot and preparation method and application thereof |
| CN112608747B (en) * | 2020-12-23 | 2022-07-19 | 武汉工程大学 | Bismuth sulfide fluorescent quantum dot and preparation method and application thereof |
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