CN109825280A - A kind of preparation method of Au@Si quantum dot - Google Patents
A kind of preparation method of Au@Si quantum dot Download PDFInfo
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- CN109825280A CN109825280A CN201910232821.0A CN201910232821A CN109825280A CN 109825280 A CN109825280 A CN 109825280A CN 201910232821 A CN201910232821 A CN 201910232821A CN 109825280 A CN109825280 A CN 109825280A
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Abstract
The invention discloses a kind of preparation methods of Au@Si quantum dot, the following steps are included: 1) prepare silicon quantum dot suspension using hydro-thermal method, 2) chlorauric acid solution is added dropwise in silicon quantum dot solution, it is stirred continuously, obtain the suspension of Au@Si quantum dot, 3) suspension of Au Si quantum dot is subjected to dialysis treatment, the Au Si quantum dot solution obtained after dialysis is put and is dried in a vacuum drying oven, solid Au Si quantum dot is obtained.Au@Si quantum dot prepared by the present invention has partial size small, is evenly distributed and the features such as biocompatibility, can be widely applied to the fields such as catalysis, analysis detection, cell imaging and biological medicine.
Description
Technical field
The invention belongs to a kind of preparation of nano material, in particular to a kind of preparation method of Au@Si quantum dot.
Background technique
Quantum dot is a kind of nano material being widely studied, and size is in 1-100nm.Silicon quantum dot and golden quantum dot are wide
General research and application have the characteristics that small toxicity, easily modification, fluorescence and biocompatibility.Two or more element shape
At core-shell structure quantum dot, the advantage that both can be had both has more performances, is also widely studied.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of preparation methods of Au@Si quantum dot.The quantum dot of preparation is molten
Liquid is convieniently synthesized, and fluorescence is good, has the features such as small toxicity, easily modification, good biocompatibility.
The preparation method of Au@Si quantum dot of the invention, includes the following steps:
(1) reducing agent is dissolved in deionized water and is made into reducing agent solution, be passed through nitrogen, remove the oxygen in solution；Then
Under nitrogen protection, silicon source compound is added into reducing agent solution, and continues stirring 5-15 minutes, obtains precursor solution；
Precursor solution is put into reaction kettle and carries out hydro-thermal reaction, is reacted 2-8 hours under 150-240 degrees Celsius, obtains silicon quantum
Point suspension；Silicon quantum dot suspension is centrifuged 5-30 minutes at 8000-10000 rpm, retains supernatant, obtains silicon quantum
Point solution；
(2) under logical condition of nitrogen gas, into the silicon quantum dot solution persistently stirred, be slowly added to chlorauric acid solution, then after
Under continuous stirring and logical condition of nitrogen gas, mixed solution is heated to 130 degrees Celsius of reactions 30-60 minutes, obtains Au@Si quantum dot
Suspension；Au@Si quantum dot suspension is centrifuged 5-30 minutes at 8000-10000 rpm, retains supernatant；
(3) supernatant that step (2) obtains is put into bag filter, carries out dialysis treatment, obtains Au@Si quantum dot solution,
Au Si quantum dot solution is put and is dried in a vacuum drying oven, solid Au Si quantum dot is obtained.
Further, the reducing agent in the step (1) is one or both of sodium citrate or sodium borohydride；It is described
The step of (1) in reducing agent solution concentration be 0.01-1.30 mol/L；Silicon source compound in the step (1) is
One or both of 3- aminopropyl trimethoxysilane or 3- aminopropyl triethoxysilane；Silicon in the step (1)
The molar ratio of source compound and reducing agent is 1:0.05-1:0.30.
Further, the mass ratio of the material of the gold chloride in the step (2) and silicon quantum dot is 0.2:1-1:1.
Further, the molecular cut off of the bag filter in the step (3) is 1000, saturating in the step (3)
Analysis processing is changed water 3-4 times altogether to change every 6-8 hours water 1 time.
The Au@Si quantum dot that the present invention obtains has partial size small, is evenly distributed and the features such as biocompatibility, can be extensive
Applied to fields such as catalysis, analysis detection, cell imaging and biological medicines.In addition the method used is easy, practical, operation
Simple process is suitble to the following large-scale production.
Detailed description of the invention
Fig. 1 is the TEM figure of Au@Si quantum dot obtained in embodiment 1.
Fig. 2 is the fluorogram of Au@Si quantum dot obtained in embodiment 1.
Specific embodiment
Specific example is chosen according to the technical scheme of the invention to be described as follows:
Embodiment 1
(1) 0.4g sodium citrate is dissolved in wiring solution-forming in the deionized water of 8mL, is passed through nitrogen, remove the oxygen in solution；
Then under nitrogen protection, 2mL 3- aminopropyl triethoxysilane is added, and continues stirring 15 minutes, it is molten to obtain presoma
Liquid；Precursor solution is put into reaction kettle and carries out hydro-thermal reaction, is reacted 4 hours at 200 degrees celsius, it is outstanding to obtain silicon quantum dot
Turbid；Silicon quantum dot suspension is centrifuged 20 minutes at 8000rpm, retains supernatant, obtains silicon quantum dot solution；Adjust silicon
The concentration of quantum dot solution；
(2) under logical condition of nitrogen gas, it is toward the volume persistently stirred in silicon quantum dot solution that 3mL concentration is 0.03mg/mL, it is slow
The slow chlorauric acid solution that 0.8 mg/mL is added, volume are that 150 μ L will be mixed molten then in the case where continuing stirring and logical condition of nitrogen gas
Liquid is heated to 130 degrees Celsius of reactions 30-60 minutes, obtains the suspension of Au@Si quantum dot；Au@Si quantum dot suspension is existed
It is centrifuged 5-30 minutes under 8000-10000 rpm, retains supernatant；
(3) supernatant that step (2) obtains is put into bag filter, molecular cut off 1000, carries out dialysis treatment, every
It changes within 6-8 hours water 1 time, changes altogether water 3-4 times, obtain Au@Si quantum dot solution, Au@Si quantum dot solution is placed on vacuum drying
It is dry in case, obtain solid Au@Si quantum dot.
The TEM of embodiment 1 is as shown in Figure 1.It can be seen that obtained Au@Si quantum dot, has homogeneity.Its fluorogram is such as
Shown in Fig. 2, it can be seen that there is good fluorescence.
Finally, it is stated that preferred embodiment above is only used to illustrate the technical scheme of the present invention and not to limit it, although logical
It crosses above-mentioned preferred embodiments the present invention is described in detail, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (4)
1. a kind of preparation method of Au@Si quantum dot, which is characterized in that comprise the steps of:
(1) reducing agent is dissolved in deionized water and is made into reducing agent solution, be passed through nitrogen, remove the oxygen in solution；Then
Under nitrogen protection, silicon source compound is added into reducing agent solution, and continues stirring 5-15 minutes, obtains precursor solution；
Precursor solution is put into reaction kettle and carries out hydro-thermal reaction, is reacted 2-8 hours under 150-240 degrees Celsius, obtains silicon quantum
Point suspension；Silicon quantum dot suspension is centrifuged 5-30 minutes at 8000-10000 rpm, retains supernatant, obtains silicon quantum
Point solution；
(2) under logical condition of nitrogen gas, into the silicon quantum dot solution persistently stirred, it is slowly added to chlorauric acid solution, is then heated
To 130 degrees Celsius reaction 30-60 minutes, obtain the suspension of Au@Si quantum dot；By Au@Si quantum dot suspension in 8000-
It is centrifuged 5-30 minutes under 10000 rpm, retains supernatant；
(3) supernatant that step (2) obtains is put into bag filter, carries out dialysis treatment, obtains Au@Si quantum dot solution,
Au Si quantum dot solution is put and is dried in a vacuum drying oven, solid Au Si quantum dot is obtained.
2. a kind of preparation method of Au Si quantum dot according to claim 1, it is characterised in that: in the step (1)
Reducing agent be one or both of sodium citrate or sodium borohydride；The concentration of reducing agent solution in the step (1)
For 0.01-1.30 mol/L；Silicon source compound in the step (1) is 3- aminopropyl trimethoxysilane or 3- aminopropyl
One or both of triethoxysilane；The molar ratio of silicon source compound and reducing agent in the step (1) is 1:
0.05-1:0.30。
3. a kind of preparation method of Au Si quantum dot according to claim 1, it is characterised in that: in the step (2)
Gold chloride and silicon quantum dot the mass ratio of the material be 0.2:1-1:1.
4. a kind of preparation method of Au Si quantum dot according to claim 1, it is characterised in that: in the step (3)
The molecular cut off of bag filter be 1000, the dialysis treatment in the step (3) is to change every 6-8 hours water 1 time, is changed altogether
Water 3-4 times.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910232821.0A CN109825280A (en) | 2019-03-26 | 2019-03-26 | A kind of preparation method of Au@Si quantum dot |
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| CN201910232821.0A CN109825280A (en) | 2019-03-26 | 2019-03-26 | A kind of preparation method of Au@Si quantum dot |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101411879A (en) * | 2008-11-28 | 2009-04-22 | 暨南大学 | SiO2/Au nano material with nucleocapsid structure-biological protein medicament complex and preparation method thereof |
| CN106141200A (en) * | 2015-03-26 | 2016-11-23 | 上海交通大学 | A kind of Preparation method and use of carbon point/gold compound nano-particle |
| CN109266336A (en) * | 2018-09-26 | 2019-01-25 | 宝鸡文理学院 | A kind of preparation method of transient metal doped carbon fluorescence quantum |
-
2019
- 2019-03-26 CN CN201910232821.0A patent/CN109825280A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101411879A (en) * | 2008-11-28 | 2009-04-22 | 暨南大学 | SiO2/Au nano material with nucleocapsid structure-biological protein medicament complex and preparation method thereof |
| CN106141200A (en) * | 2015-03-26 | 2016-11-23 | 上海交通大学 | A kind of Preparation method and use of carbon point/gold compound nano-particle |
| CN109266336A (en) * | 2018-09-26 | 2019-01-25 | 宝鸡文理学院 | A kind of preparation method of transient metal doped carbon fluorescence quantum |
Non-Patent Citations (1)
| Title |
|---|
| BHAGWATI SHARMA等: "One Pot Green Synthesis of Si Quantum Dots and Catalytic Au Nanoparticle–Si Quantum Dot Nanocomposite", 《ACS SUSTAINABLE CHEM. ENG.》 * |
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