CN102851022A - Preparation method of fluorescent silica nanoparticles - Google Patents
Preparation method of fluorescent silica nanoparticles Download PDFInfo
- Publication number
- CN102851022A CN102851022A CN2012103744654A CN201210374465A CN102851022A CN 102851022 A CN102851022 A CN 102851022A CN 2012103744654 A CN2012103744654 A CN 2012103744654A CN 201210374465 A CN201210374465 A CN 201210374465A CN 102851022 A CN102851022 A CN 102851022A
- Authority
- CN
- China
- Prior art keywords
- silicon
- preparation
- fluorescence
- silicon wafer
- nano particles
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Silicon Compounds (AREA)
Abstract
Disclosed is a preparation method of fluorescent silica nanoparticles. A two-step method is used. The preparation method includes firstly preparing silica nanowires through a hydrogen fluoride assisted etching method and then preparing water-soluble fluorescent silica nanoparticles through a microwave radiation method. Dibasic acid or an amino acid solution used in the microwave radiation method can perform hydrophilic modification on silica nanoparticles in itself, and the obtained nanoparticles are provided with good surface defects, therefore the fluorescent silica nanoparticles obtained through the preparation method are provided with good water dispersity, high in fluorescence quantum efficiency, good in stability and capable of being used for bioinstrumentation and analysis as fluorescence labels.
Description
Technical field
The present invention relates to field of nano material preparation, relate to particularly a kind of method that adopts microwave radiation to prepare fluorescence silicon nano particles.
Background technology
The function silicon nano material obtains scientist's extensive concern (Nature2000,408,440-444 day by day owing to its unique optical/electrical/mechanical properties, surface modificability and good biocompatibility; Science2002,296,1293-1297; Science2003,299,1874-1877; Science2006,313,1100-1104.).It is worth noting especially, as representative zero dimension silicon nano material---fluorescence silicon nano particles, because it has good biocompatibility and hypotoxicity, being expected to be used widely at biology and biomedicine, (Science 2005,307,538-544; Chem.Soc.Rev.2010,39,4234-4243; Nano Today2010,5,282-295.).Yet most fluorescence silicon nano particles surface is hydrophobic group, causes its water dispersible poor, can not satisfy the requirement of biologic applications.In the past few years, scientists has developed diverse ways, adopts hydrophilic radical (such as hydrophilic small molecules, polymkeric substance and microbeam) that hydrophobicity nano silicon particles surface is modified, thereby improves its water dispersible (Nano Lett.2004,4,1463-1467; Angew.Chem., Int.Ed.2005,44,4550-4554; ACS Nano2008,2,873-878; J.Am.Chem.Soc.2009,131,4434-4438; Angew.Chem.Int.Ed.2009,121,134-138).Yet, although these methods can strengthen the water dispersible of nano silicon particles to a great extent, (as: at first need to prepare hydrophobic nano silicon particles but process is comparatively complicated, and then with hydrophilic radical it is modified), and destroy easily the nano silicon particles surface in the modification, (the nano silicon particles pH stability of vinylformic acid/allylamine modification is bad to affect its physical/chemical; The nano silicon particles oversize (60-300nm) that polymkeric substance/microbeam is modified) (Angew.Chem.Int.Ed.2009,121,134-138; Nano Today2010,5,282-295; ACS Nano2011,5,413-423).This has limited the development based on the nano silicon particles biologic applications to a great extent.Therefore, how to adopt more easy method, need not extra finishing step, directly prepare the fluorescence silicon nano particles with superior water dispersibility, become a difficult problem that needs to be resolved hurrily.
Summary of the invention
The object of the invention is to for problem recited above, provide a kind of operational safety, fast and convenient microwave radiation to prepare the method for fluorescence silicon quantum dot, directly prepare the fluorescence silicon nano particles with good photoluminescent property, superior water dispersibility and excellent light/chemical stability at aqueous phase first.
The preparation method of a kind of fluorescence silicon nano particles that propose according to purpose of the present invention comprises step:
1) hydrogen fluoride auxiliary etch method prepares silicon nanowires: at first clean silicon wafer and obtain clean silicon wafer; The silicon wafer that cleans up inserted carry out silicon-hydrogenation in the hydrogen fluoride solution, obtain the silicon wafer of surface coverage silicon-hydrogen bond; Then will put into Silver Nitrate and hydrofluoric mixing solutions through resulting silicon wafer after the above-mentioned processing, the certain hour that slowly vibrates, the mixed solution of putting into hydrogen fluoride and hydrogen peroxide after the taking-up reacts, and obtains silicon nanowire array; Utilize ultrasonic silicon nanowires to be come off from silicon chip, and then by sedimentator silicon nanowires is collected and to be scattered in the aqueous solution;
2) microwave radiation means prepares the water soluble fluorescence nano silicon particles: at first with silicon nanowires and diprotic acid or the abundant stirring and evenly mixing of amino acid solution, under the environment of Microwave Field Heating, silicon nanowires fragments into nano silicon particles, obtains diprotic acid or fluorescigenic water-soluble silicon nano particle amino acid modified and that have fine surface imperfection.
Preferably, the step of cleaning silicon wafer described in the step 1) comprises and at first silicon wafer is placed the acetone soln ultrasonic cleaning, then put into again the vitriol oil after cleaning with ultrapure water and hydrogen peroxide mixed solution is removed the pollution impurity on surface, clean with ultrapure water more at last, obtain clean silicon wafer.
Preferably, the concentration of described hydrogen peroxide is 5% to 30%, the described vitriol oil and hydrogen peroxide volume ratio=1:(0.1 to 0.8).
Preferably, described silicon wafer is p-type or the N-shaped silicon wafer of 0.01 Ω * cm to 20 Ω * cm.
Preferably, the concentration of the hydrogen fluoride solution in the described step 1) is 3% to 40%.
Preferably, in the step 1), the concentration of described Silver Nitrate is mass percent 0.85%-17.0%, this Silver Nitrate and hydrogen fluoride volume ratio=1:(0.01 to 0.5).
Preferably, in the step 1), the reaction times of described silicon-hydrogenation is 2 minutes to 1 hour.
Preferably, in the step 1), described hydrogen fluoride and hydrogen peroxide mixed solution adopt 10% hydrogen fluoride and 1% hydrogen peroxide, making take volume ratio as 1:1 to 1:1.5.
Preferably, step 2) in, diprotic acid or amino acid and silicon nanowires are to be in mass ratio diprotic acid or amino acid: silicon nanowires=1:1 to 10:1.
Preferably, step 2) diprotic acid or the amino acid described in comprises: one or more mixing in pentanedioic acid, Succinic Acid, amino capric acid or the glycine.
Preferably, the temperature of Microwave Field Heating is described step 2): 100 ℃ to 200 ° C.
There is good water dispersible in the fluorescence silicon nano particles residence for preparing by method of the present invention, and fluorescence quantum efficiency is high, and good stability can be used as fluorescent marker and is used for biological detection and analysis.
Embodiment
Just as described in the background art, in order to obtain having the fluorescence silicon nano particles of superior water dispersibility.The finishing that often needs in the prior art to increase hydrophilic radical is processed, yet this processing is not only so that the increase of complex process degree, in the process of processing, change easily the chemical physical property of nano silicon particles, so that the applicability of nano silicon particles weakens simultaneously.
Therefore the present invention proposes a kind of preparation method of fluorescence silicon nano particles, the method adopts two step method, at first make silicon nanowires, and then utilize diprotic acid or amino acid solution that silicon nanowires is made into nano silicon particles, because diprotic acid or amino acid solution itself just can be done hydrophilic modification to nano silicon particles, and the nano particle that obtains has good surface imperfection.Therefore not only technique is simple for preparation method of the present invention, and the nano silicon particles that makes is had good technology stability, can overcome problems of the prior art.
Particularly, preparation method of the present invention comprises following two large steps:
S1: hydrogen fluoride auxiliary etch method prepares silicon nanowires: at first silicon wafer is at first placed the acetone soln ultrasonic cleaning, then (concentration: 5%-30%) mixing solutions is removed the pollution impurity on surface to put into the vitriol oil and hydrogen peroxide after utilizing ultrapure water to clean again, the vitriol oil and hydrogen peroxide volume ratio=1:(0.1～0.8), and then with the ultrapure water cleaning, obtain clean silicon wafer.The silicon wafer that cleans up is inserted hydrogen fluoride solution (concentration: carry out silicon-hydrogenation 3%-40%), obtain the silicon wafer of a large amount of silicon-hydrogen bonds of surface coverage (Si-H).Then will put into Silver Nitrate (mass percent 0.85%-17.0%) and hydrofluoric mixing solutions, the certain hour that slowly vibrates, Silver Nitrate and hydrogen fluoride volume ratio=1:(0.01～0.5 through resulting silicon wafer after the above-mentioned processing).The mixed solution of putting into hydrogen fluoride and hydrogen peroxide after the taking-up reacts, and according to principle of electrochemical reaction (that is: silver ions at first is reduced to silver nano-grain by the Si-H key, further is fluorinated the hydrogen etching, forms silicon nanowires), can obtain silicon nanowire array.Utilize ultrasonic concussion silicon nanowires can be split away off from silicon chip, and then by sedimentator silicon nanowires is collected in the aqueous solution that is scattered in 0.5ml-5ml.
S2: microwave radiation means prepares the water soluble fluorescence nano silicon particles: at first with silicon nanowires and diprotic acid or the abundant stirring and evenly mixing of amino acid solution, here diprotic acid or amino acid and silicon nanowires are to be in mass ratio diprotic acid or amino-acid compound: silicon nanowires=1:1～10:1, diprotic acid or amino acid comprise: pentanedioic acid, Succinic Acid, amino capric acid or glycine.Under the environment of Microwave Field Heating (100 ℃-200 ℃), silicon nanowires fragments into nano silicon particles, diprotic acid or amino acid also can react with the Si-H key of surface of silicon nanowires as the C=O key of its carboxyl functional group of part, obtain diprotic acid or amino acid modified water-soluble silicon nano particle, meanwhile diprotic acid or amino acid carry out the fluorescigenic nano silicon particles that slowly etching formation has fine surface imperfection to the silicon line.According to quantum size effect, by the proper extension reaction times, can reduce quantum dot size, can obtain the water-soluble silicon nano particle of different glow colors.
The below will be clearly and completely described technical scheme of the present invention by embodiment.Obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills belong to the scope of protection of the invention not making the every other embodiment that obtains under the creative work prerequisite.
Embodiment 1
(1) preparation silicon nanowires:
Be 2cm with reaction area
2, specific conductivity is that the p-type silicon wafer of 5 Ω adds an amount of acetone, be lower ultrasonic cleaning 10 minutes at 40Hz power, with ultrapure water flushing 3 times, again silicon wafer is put into 98% vitriol oil and 30% hydrogen peroxide mixed solution that the 20ml volume ratio is 3:1, soaked 2 minutes to 1 hour, and be preferably 30 minutes, then take out silicon wafer, and have ultrapure water to wash again 3 times, obtain clean silicon wafer.Again clean silicon wafer is put into 5% hydrogen fluoride solution and soaked 20 minutes, can obtain the clean silicon wafer of surface coverage Si-H key.Resulting silicon wafer was put into 0.85% Silver Nitrate that the 20ml volume ratio is 1:1 and 10% hydrogen fluoride mixing solutions 3 minutes, put into again volume ratio after the taking-up and be 10% hydrogen fluoride of 1:1 and the reaction of 1% hydrogen peroxide mixed solution 10 minutes, can obtain silicon nanowire array.Be lower ultrasonic 30 minutes with it at 60Hz power, centrifugal 15 minutes collecting precipitations under the 6000rpm/min condition, it is scattered in the 0.5ml ultrapure water again, can obtain the silicon nanowires precursor solution,
(2) preparation fluorescence silicon nano particle
The resulting silicon nanowires of preparation in (1) is added 20 milliliters be dissolved with in the 4 gram pentanedioic acid solution, stir, the mixing solutions that obtains is carried out carry out microwave radiation heating, can obtain fluorescence silicon nano particles.Control condition is as follows:
Microwave power: 150W; Temperature of reaction: 180 ℃; Reaction times: 15min;
Embodiment 2
(1) preparation silicon nanowires:
Be 3cm with reaction area
2, specific conductivity is that the p-type silicon wafer of 0.05 Ω adds an amount of acetone, it is lower ultrasonic 15 minutes at 60Hz power, with ultrapure water flushing 3 times, again silicon wafer is put into 98% vitriol oil and 30% hydrogen peroxide mixed solution that the 20ml volume ratio is 4:1, soak and take out silicon wafer after 30 minutes, and have ultrapure water to wash again 3 times, and put it into again in 5% hydrogen fluoride solution and soaked 20 minutes, can obtain the clean silicon wafer of surface coverage Si-H key.Resulting silicon wafer was put into 0.005M Silver Nitrate that the 20ml volume ratio is 1:0.8 and 10% hydrogen fluoride mixing solutions 3 minutes, put into again volume ratio after the taking-up and be 10% hydrogen fluoride of 1:1 and the reaction of 1% hydrogen peroxide mixed solution 8 minutes, can obtain silicon nanowire array.Be lower ultrasonic 30 minutes with it at 60Hz power, centrifugal 15 minutes collecting precipitations under the 8000rpm/min condition, it is scattered in the 0.5ml ultrapure water again, can obtain the silicon nanowires precursor solution,
(2) preparation fluorescence silicon nano particles
The resulting silicon nanowires of preparation in (1) is added 20 milliliters be dissolved with in the 3 gram pentanedioic acid solution, stir, the mixing solutions that obtains is carried out carry out microwave radiation heating, can obtain fluorescence silicon nano particles.Control condition is as follows:
Microwave power: 160W; Temperature of reaction: 185 ℃; Reaction times: 10min;
Embodiment 3
(1) preparation silicon nanowires:
Be 3.5cm with reaction area
2, specific conductivity is that the N-shaped silicon wafer of 5 Ω adds an amount of acetone, it is lower ultrasonic 12 minutes at 100Hz power, with ultrapure water flushing 3 times, again silicon wafer is put into 98% vitriol oil and 30% hydrogen peroxide mixed solution that the 15ml volume ratio is 3.5:1, soak and take out silicon wafer after 35 minutes, and have ultrapure water to wash again 3 times, and put it into again in 5% hydrogen fluoride solution and soaked 20 minutes, can obtain the clean silicon wafer of surface coverage Si-H key.Resulting silicon wafer was put into 0.85% Silver Nitrate that the 20ml volume ratio is 1:1.2 and 10% hydrogen fluoride mixing solutions 5 minutes, put into again volume ratio after the taking-up and be 10% hydrogen fluoride of 1:1.3 and the reaction of 1% hydrogen peroxide mixed solution 6 minutes, can obtain silicon nanowire array.Be lower ultrasonic 20 minutes with it at 100Hz power, centrifugal 20 minutes collecting precipitations under the 7000rpm/min condition, it is scattered in the 1ml ultrapure water again, can obtain the silicon nanowires precursor solution,
(2) preparation fluorescence silicon nano particles
The resulting silicon nanowires of preparation in (1) is added 20 milliliters be dissolved with in the 1.6 gram glycine solutions, stir, the mixing solutions that obtains is carried out carry out microwave radiation heating, can obtain fluorescence silicon nano particles.Control condition is as follows:
Microwave power: 130W; Temperature of reaction: 170 ℃; Reaction times: 15min;
Embodiment 4
(1) preparation silicon nanowires:
Be 2.5cm with reaction area
2, specific conductivity is that the N-shaped silicon wafer of 0.02 Ω adds an amount of acetone, it is lower ultrasonic 18 minutes at 80Hz power, with ultrapure water flushing 3 times, again silicon wafer is put into 98% vitriol oil and 30% hydrogen peroxide mixed solution that the 20ml volume ratio is 2.5:1, soak and take out silicon wafer after 30 minutes, and have ultrapure water to wash again 3 times, and put it into again in 5% hydrogen fluoride solution and soaked 20 minutes, can obtain the clean silicon wafer of surface coverage Si-H key.Resulting silicon wafer was put into 0.85% Silver Nitrate that the 20ml volume ratio is 1:1 and 10% hydrogen fluoride mixing solutions 5 minutes, put into again volume ratio after the taking-up and be 10% hydrogen fluoride of 1:1.5 and the reaction of 1% hydrogen peroxide mixed solution 10 minutes, can obtain silicon nanowire array.Be lower ultrasonic 30 minutes with it at 100Hz power, centrifugal 30 minutes collecting precipitations under the 9000rpm/min condition, it is scattered in the 0.6ml ultrapure water again, can obtain the silicon nanowires precursor solution,
(2) preparation fluorescence silicon nano particles
The resulting silicon nanowires of preparation in (1) is added 20 milliliters be dissolved with in the 2 gram Succinic Acid solution, stir, the mixing solutions that obtains is carried out carry out microwave radiation heating, can obtain fluorescence silicon nano particles.Control condition is as follows:
Microwave power: 160W; Temperature of reaction: 175 ℃; Reaction times: 25min;
Embodiment 5
(1) preparation silicon nanowires:
Be 1cm with reaction area
2, specific conductivity is that the p-type silicon wafer of 10 Ω adds an amount of acetone, it is lower ultrasonic 15 minutes at 80Hz power, with ultrapure water flushing 3 times, again silicon wafer is put into 98% vitriol oil and 30% hydrogen peroxide mixed solution that the 20ml volume ratio is 3:1, soak and take out silicon wafer after 30 minutes, and have ultrapure water to wash again 3 times, and put it into again in 5% hydrogen fluoride solution and soaked 20 minutes, can obtain the clean silicon wafer of surface coverage Si-H key.Resulting silicon wafer was put into 0.85% Silver Nitrate that the 20ml volume ratio is 1:1.3 and 10% hydrogen fluoride mixing solutions 3 minutes, put into again volume ratio after the taking-up and be 10% hydrogen fluoride of 1:1.1 and the reaction of 1% hydrogen peroxide mixed solution 10 minutes, can obtain silicon nanowire array.Be lower ultrasonic 20 minutes with it at 90Hz power, centrifugal 15 minutes collecting precipitations under the 6000rpm/min condition, it is scattered in the 0.3ml ultrapure water again, can obtain the silicon nanowires precursor solution,
2) preparation fluorescence silicon nano particles
The resulting silicon nanowires of preparation in (1) is added 20 milliliters be dissolved with in the amino capric acid solution of 3.6 grams, stir, the mixing solutions that obtains is carried out carry out microwave radiation heating, can obtain fluorescence silicon nano particles.Control condition is as follows:
Microwave power: 150W; Temperature of reaction: 180 ℃; Reaction times: 20min;
Embodiment 6
(1) preparation silicon nanowires:
Be that 2.5cm2, specific conductivity are that the N-shaped silicon wafer of 5 Ω adds an amount of acetone with reaction area, it is lower ultrasonic 15 minutes at 80Hz power, with ultrapure water flushing 3 times, again silicon wafer is put into 98% vitriol oil and 30% hydrogen peroxide mixed solution that the 25ml volume ratio is 3.6:1, soak and take out silicon wafer after 30 minutes, and have ultrapure water to wash again 3 times, and put it into again in 5% hydrogen fluoride solution and soaked 20 minutes, can obtain the clean silicon wafer of surface coverage Si-H key.Resulting silicon wafer was put into 0.85% Silver Nitrate that the 20ml volume ratio is 1:1 and 10% hydrogen fluoride mixing solutions 3 minutes, put into again volume ratio after the taking-up and be 10% hydrogen fluoride of 1:1 and the reaction of 1% hydrogen peroxide mixed solution 25 minutes, can obtain silicon nanowire array.Be lower ultrasonic 30 minutes with it at 100Hz power, centrifugal 25 minutes collecting precipitations under the 8000rpm/min condition, it is scattered in the 1ml ultrapure water again, can obtain the silicon nanowires precursor solution,
(2) preparation fluorescence silicon nano particle
The resulting silicon nanowires of preparation in (1) is added 20 milliliters be dissolved with in the 5 gram pentanedioic acid solution, stir, the mixing solutions that obtains is carried out carry out microwave radiation heating, can obtain fluorescence silicon nano particles.Control condition is as follows:
Microwave power: 190W; Temperature of reaction: 180 ℃; Reaction times: 20min;
In sum, the present invention proposes a kind of preparation method of fluorescence silicon nano particles, utilize two step method, at first make silicon nanowires, and then utilize diprotic acid or amino acid solution that silicon nanowires is made into nano silicon particles, because diprotic acid or amino acid solution itself just can be done hydrophilic modification to nano silicon particles, and the nano particle that obtains has good surface imperfection.Therefore the fluorescence silicon nano particles that prepare by method of the present invention occupy good water dispersible, and fluorescence quantum efficiency is high, and good stability can be used as fluorescent marker and is used for biological detection and analysis.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be apparent concerning those skilled in the art, and General Principle as defined herein can in the situation that does not break away from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will can not be restricted to embodiment illustrated herein, but will meet the widest scope consistent with principle disclosed herein and features of novelty.To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be apparent concerning those skilled in the art, and General Principle as defined herein can in the situation that does not break away from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will can not be restricted to embodiment illustrated herein, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (11)
1. the preparation method of fluorescence silicon nano particles is characterized in that, comprises step:
1) hydrogen fluoride auxiliary etch method prepares silicon nanowires: at first clean silicon wafer and obtain clean silicon wafer; The silicon wafer that cleans up inserted carry out silicon-hydrogenation in the hydrogen fluoride solution, obtain the silicon wafer of surface coverage silicon-hydrogen bond; Then will put into Silver Nitrate and hydrofluoric mixing solutions through resulting silicon wafer after the above-mentioned processing, the certain hour that slowly vibrates, the mixed solution of putting into hydrogen fluoride and hydrogen peroxide after the taking-up reacts, and obtains silicon nanowire array; Utilize ultrasonic silicon nanowires to be come off from silicon chip, and then by sedimentator silicon nanowires is collected and to be scattered in the aqueous solution;
2) microwave radiation means prepares the water soluble fluorescence nano silicon particles: at first with silicon nanowires and diprotic acid or the abundant stirring and evenly mixing of amino acid solution, under the environment of Microwave Field Heating, silicon nanowires fragments into nano silicon particles, obtains diprotic acid or fluorescigenic water-soluble silicon nano particle amino acid modified and that have fine surface imperfection.
2. the preparation method of fluorescence silicon nano particles as claimed in claim 1, it is characterized in that: the step of cleaning silicon wafer described in the step 1) comprises and at first silicon wafer is placed the acetone soln ultrasonic cleaning, then put into again the vitriol oil after cleaning with ultrapure water and hydrogen peroxide mixed solution is removed the pollution impurity on surface, clean with ultrapure water more at last, obtain clean silicon wafer.
3. the preparation method of fluorescence silicon nano particles as claimed in claim 2, it is characterized in that: the concentration of described hydrogen peroxide is 5% to 30%, the described vitriol oil and hydrogen peroxide volume ratio=1:(0.1 to 0.8).
4. the preparation method of fluorescence silicon nano particles as claimed in claim 1, it is characterized in that: described silicon wafer is p-type or the N-shaped silicon wafer of 0.01 Ω * cm to 20 Ω * cm.
5. the preparation method of fluorescence silicon nano particles as claimed in claim 1, it is characterized in that: the concentration of the hydrogen fluoride solution in the described step 1) is 3% to 40%.
6. the preparation method of fluorescence silicon nano particles as claimed in claim 1, it is characterized in that: in the step 1), the concentration of described Silver Nitrate is mass percent 0.85%-17.0%, this Silver Nitrate and hydrogen fluoride volume ratio=1:(0.01 to 0.5).
7. the preparation method of fluorescence silicon nano particles as claimed in claim 1, it is characterized in that: in the step 1), described hydrogen fluoride and hydrogen peroxide mixed solution adopt 10% hydrogen fluoride and 1% hydrogen peroxide, make take volume ratio as 1:1 to 1:1.5.
8. the preparation method of fluorescence silicon nano particles as claimed in claim 1, it is characterized in that: in the step 1), the reaction times of described silicon-hydrogenation is 2 minutes to 1 hour.
9. the preparation method of fluorescence silicon nano particles as claimed in claim 1 is characterized in that: step 2) in, diprotic acid or amino acid and silicon nanowires are to be in mass ratio diprotic acid or amino acid: silicon nanowires=1:1 to 10:1.
10. the preparation method of fluorescence silicon nano particles as claimed in claim 1 is characterized in that: step 2) described in diprotic acid or amino acid, comprising: one or more mixing in pentanedioic acid, Succinic Acid, amino capric acid or the glycine.
11. the preparation method of fluorescence silicon nano particles as claimed in claim 1 is characterized in that: the temperature of Microwave Field Heating is described step 2): 100 ° C to 200 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103744654A CN102851022A (en) | 2012-09-27 | 2012-09-27 | Preparation method of fluorescent silica nanoparticles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103744654A CN102851022A (en) | 2012-09-27 | 2012-09-27 | Preparation method of fluorescent silica nanoparticles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102851022A true CN102851022A (en) | 2013-01-02 |
Family
ID=47398008
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012103744654A Pending CN102851022A (en) | 2012-09-27 | 2012-09-27 | Preparation method of fluorescent silica nanoparticles |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102851022A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103755384A (en) * | 2014-01-20 | 2014-04-30 | 中国科学院理化技术研究所 | Method for modifying organic small molecules on surface of silicon nanowire array |
| CN104310407A (en) * | 2014-09-16 | 2015-01-28 | 苏州大学 | Method for biomimetic preparation of water-soluble fluorescent silicon nano-particles |
| CN106479487A (en) * | 2016-09-27 | 2017-03-08 | 苏州大学 | A kind of preparation method of fluorescence silicon nano particles |
| CN107099294A (en) * | 2017-04-11 | 2017-08-29 | 枣庄学院 | A kind of corrosive liquid and its application process for being used to prepare silicon nanowire structure |
| CN109908464A (en) * | 2019-04-16 | 2019-06-21 | 北京师范大学 | A kind of biodegradable silicon nanometer needle injection and its application |
| CN112067587A (en) * | 2020-08-06 | 2020-12-11 | 福建医科大学 | Preparation of sulfur quantum dots with high quantum yield and method for measuring ascorbic acid by using sulfur quantum dots |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101719543A (en) * | 2009-09-30 | 2010-06-02 | 清华大学 | Method for preparing silicon nanowire array membrane electrode |
-
2012
- 2012-09-27 CN CN2012103744654A patent/CN102851022A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101719543A (en) * | 2009-09-30 | 2010-06-02 | 清华大学 | Method for preparing silicon nanowire array membrane electrode |
Non-Patent Citations (1)
| Title |
|---|
| 钟旖菱: "荧光量子点和荧光硅纳米线的微博制备及其在生物影像中的应用研究", 《中国优秀硕士学位论文全文数据库》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103755384A (en) * | 2014-01-20 | 2014-04-30 | 中国科学院理化技术研究所 | Method for modifying organic small molecules on surface of silicon nanowire array |
| CN103755384B (en) * | 2014-01-20 | 2015-08-26 | 中国科学院理化技术研究所 | A kind of method of silicon nanowire array finishing organic molecule |
| CN104310407A (en) * | 2014-09-16 | 2015-01-28 | 苏州大学 | Method for biomimetic preparation of water-soluble fluorescent silicon nano-particles |
| CN106479487A (en) * | 2016-09-27 | 2017-03-08 | 苏州大学 | A kind of preparation method of fluorescence silicon nano particles |
| CN107099294A (en) * | 2017-04-11 | 2017-08-29 | 枣庄学院 | A kind of corrosive liquid and its application process for being used to prepare silicon nanowire structure |
| CN109908464A (en) * | 2019-04-16 | 2019-06-21 | 北京师范大学 | A kind of biodegradable silicon nanometer needle injection and its application |
| CN112067587A (en) * | 2020-08-06 | 2020-12-11 | 福建医科大学 | Preparation of sulfur quantum dots with high quantum yield and method for measuring ascorbic acid by using sulfur quantum dots |
| CN112067587B (en) * | 2020-08-06 | 2024-03-22 | 福建医科大学 | Preparation of high quantum yield sulfur quantum dot and determination method for ascorbic acid by using same |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102851022A (en) | Preparation method of fluorescent silica nanoparticles | |
| Pender et al. | Peptide-mediated formation of single-wall carbon nanotube composites | |
| Sivakov et al. | Realization of vertical and zigzag single crystalline silicon nanowire architectures | |
| CN106082184B (en) | A kind of nitrogen sulphur codope graphene and preparation method and application | |
| CN105215352B (en) | With the preparation method of the cationic polymer modified gold nanoclusters of coated with silica | |
| CN103693633A (en) | Method for green synthesis of fluorescent chiral carbon dots | |
| CN101913600A (en) | Method for preparing graphene/semiconductor quantum dot composite material | |
| CN101693196B (en) | Preparation method of silver/titanium dioxide compound | |
| Zhao et al. | Monolayer rubrene functionalized graphene-based eletrochemiluminescence biosensor for serum cystatin C detection with immunorecognition-induced 3D DNA machine | |
| JP5451710B2 (en) | Microscale flaky silver particles and method for producing the same | |
| CN110530950A (en) | The building of paper base sensor based on exciton Plasma Interaction efficient detection PSA | |
| CN108033432A (en) | A kind of cage structure material g-C3N4Preparation method and applications | |
| CN103232845B (en) | Preparation and application for silicon quantum dots | |
| CN104370282A (en) | Method for simply preparing N-type graphene field-effect tube | |
| CN103523773A (en) | High-conductivity graphene and graphene conducting film, and preparation method thereof | |
| CN103194221B (en) | Method for preparing water-soluble fluorescent silicon nanoparticle by utilizing microwave radiation | |
| CN104076075A (en) | Gold nano particle-titanium dioxide nano wire array composite material as well as preparation method and application thereof | |
| CN102618260A (en) | Method for preparing carbon nano tube/silica network/ligand/rare-earth organic and inorganic composite luminescent material | |
| CN106750278A (en) | The preparation method of the graft-functionalized Graphene composite sulfur cadmium quantum dot of modified polyaniline | |
| CN105600780A (en) | Co-combustion preparation method of chlorine doped graphene quantum dots | |
| CN1915834A (en) | Method for preparing Nano thin film of medium pore of titania | |
| CN104076072A (en) | High-sensitivity photoelectrochemical sensor made from iridium oxide-ferriporphyrin-titanium oxide and preparation method for sensor | |
| CN104876266A (en) | Aqueous-phase preparation method of bismuth sulfide/protein composite nanospheres | |
| CN104241116B (en) | A kind of method of germanium material surface-stable passivation | |
| CN107302040A (en) | The preparation method of Ag nano wire light trapping structures is inlayed based on wet etching silicon face |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20130102 |