CN104560030B - A kind of method that green prepares fluorescence silicon nano particles - Google Patents
A kind of method that green prepares fluorescence silicon nano particles Download PDFInfo
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- CN104560030B CN104560030B CN201510032900.9A CN201510032900A CN104560030B CN 104560030 B CN104560030 B CN 104560030B CN 201510032900 A CN201510032900 A CN 201510032900A CN 104560030 B CN104560030 B CN 104560030B
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Abstract
The invention discloses a kind of method that green prepares fluorescence silicon nano particles, and net, addition acid solution, heating water bath are washed with deionized water after the high plant of silicon content is shredded；It will be washed with deionized water with acid-treated sample to neutrality, be put into crucible, be heated to sample and become white powder；Extracting waste powder, aqueous slkali is added, microwave radiation heating, obtains fluorescence silicon nano particles.The method that the green of the present invention prepares fluorescence silicon nano particles, carried out completely in aqueous phase, raw material is cheap, green, safe operation, fast and convenient, small toxicity, the fluorescence silicon nano particles of gained have good monodispersity and photoluminescent property, quantum yield is high, storage stability is good, has good water solubility, can be widely used in various optical correlation fields as fluorescent marker.
Description
Technical field
The invention belongs to silicon nano material technical field, is related to a kind of preparation method of fluorescence silicon nano particles, specifically relates to
And a kind of method that green plant high by silicon content prepares fluorescence silicon nano particles.
Background technology
The silicon nano material of functionalization have good optical/electrical/engineering properties, surface modificability and well it is simultaneous
Unique property such as capacitive, thus people have to the silicon nano material of functionalization extremely strong interest (referring to：Pavesi,L.；
Negro,L.D.；Mazzoleni,C.；Franzo,G.；Priolo,F.Nature 2000,408,440-444.Ding,Z.F.；
Quinn,B.M.；Haram,S.K.；Pell,L.E.；Korgel,B.A.；Bard,A.J.Science 2002,296,1293-
1297.Ma,D.D.D.；Lee,C.S.；Au,F.C.K.；Tong,S.Y.；Lee,S.T.Science 2003,299,1874-
1877.Patolsky,F.；Timko,B.P.；Yu,G.H.；Fang,Y.；Greytak,A.B.；Zheng,G.F.；Lieber,
C.M.Science 2006,313,1100-1104.).Typical fluorescence silicon nano particles are very representational zero dimension silicon nanometers
Material, because it has good biocompatibility and hypotoxicity and be expected in biology and be medically applied (referring to：
Michalet,X.；Pinaud,F.F.；Bentolila,L.A.；Tsay,J.M.；Doose,S.；Li,J.J.；Sundaresan,
G.；Wu,A.M.；Gambhir,S.S.；Weiss,S.Science 2005,307,538-544.Song,S.P.；Qin,Y.；He,
Y.；Huang,Q.；Fan,C.H.；Chen,H.Y.Chem.Soc.Rev.2010,39,4234-4243.He,Y.；Fan,C.H.；
Lee,S.T.Nano Today 2010,5,282-295.).So far, the preparation method of fluorescence silicon nano particles needs costliness
Or poisonous silicon precursor solution, such as silicon nanowires, bulk silicon, organosilicon small molecule, also needed to during synthesis
Add organic reagent, such as alkene, alkane, alcohol compound.The step of synthesis, is generally more, can also cause environmental pollution (ginseng
See：Li,Z.F.；Ruckenstein,E.NanoLett.2004,4,1463-1467.Warner,J.H.；Hoshino,A.；
Yamamoto,K.；Tilley,R.D.Angew.Chem.,Int.Ed.2005,44,4550-4554.Erogbogbo,F.；
Yong,K.T.；Roy,I.；Xu,G.X.；Prasad,P.N.；Swihart,M.T.ACS Nano 2008,2,873-
878.14.He,Y.；Su,Y.Y.；Yang,X.B.；Kang,Z.H.；Xu,T.T.；Zhang,R.Q.；Fan,C.H.；Lee,
S.T.J.Am.Chem.Soc.2009,131,4434-4438.)。
It is well known that contain element silicon among plant.And the silicone content of some plants is of a relatively high, Equisetum and grass family
Silicone content in plant can account for the 50%~70% of plant ass.But up to now, utilize the natural material of this cheap environmental protection
The method for preparing fluorescence silicon nano particles there is no report.
The content of the invention
In view of this, it is an object of the invention to provide a kind of green, safe operation, fast and convenient prepare fluorescence
The method of nano silicon particles.
Specifically, the present invention provides following technical scheme：
The method that the green of the present invention prepares fluorescence silicon nano particles, comprises the steps：
(1) it is washed with deionized water after, silicon content 10wt%~35wt% plant is shredded only, addition 38wt%~
5wt% acid solution, 1h~10h is heated under the water-bath of temperature 50 C~100 DEG C；
Preferably, described silicon content 10wt%~35wt% plant is grass, bryophyte, fern plant
Thing, sedge, composite family sagebruss, Violaceae plant or madder wort.
Preferably, described acid solution is hydrochloric acid, phosphoric acid, nitric acid or sulfuric acid.
(2), step (1) is washed with deionized water to neutrality with acid-treated sample, is put into crucible, is heated to sample
Become white powder；
(3), take the white powder obtained by step (2), add 0.1mol/L~10mol/L aqueous slkali, power 15W~
1000W, microwave radiation heating 30min~20h, obtains fluorescence silicon nano particles at 100 DEG C~160 DEG C of temperature.
Preferably, described aqueous slkali is sodium hydroxide solution or potassium hydroxide solution.
The green method for preparing fluorescence silicon nano particles of the present invention, is carried out completely in aqueous phase, and raw material is cheap, green ring
Guarantor, safe operation, fast and convenient, small toxicity, the fluorescence silicon nano particles of gained have good monodispersity and photoluminescent property, amount
Sub- yield is high, and storage stability is good, has good water solubility, can be widely used in various optics phases as fluorescent marker
Pass field.
Brief description of the drawings
Technical scheme in order to illustrate the embodiments of the present invention more clearly, make required in being described below to embodiment
Accompanying drawing is briefly described, it should be apparent that, the accompanying drawing for the present invention in describing below is only the one of the present invention
A little embodiments, for those of ordinary skill in the art, on the premise of not paying creative work, can also be according to these
Accompanying drawing obtains other accompanying drawings.
Fig. 1 is the fluorescence spectra for the fluorescence silicon nano particles that preferred embodiment 6 is prepared, and excitation wavelength is
300nm~500nm；
Fig. 2 is transmission electron microscope (TEM) figure and high score for the fluorescence silicon nano particles that preferred embodiment 6 is prepared
Resolution transmission electron microscope (HRTEM) figure, wherein a) scheme for TEM, b) scheme for HRTEM.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, detailed retouch is carried out to the technical scheme in the embodiment of the present invention
State.
Raw material used in the present invention can freely be bought by market, and chemical agent is that analysis is pure；Received for preparing fluorescence silicon
The microwave reactor model of rice grain：NOVA SII, it is purchased from the Preekem companies in Shanghai.
Embodiment 1
(1) pre-treatment is carried out with acid
Net rice husk will be washed with deionized water and be heated at reflux 3h with 10wt% hydrochloric acid water-bath.
(2) silica sample is prepared
The rice husk handled well is placed in porcelain crucible, it is in canescence to be heated to alcolhol burner.
(3) microwave radiation prepares fluorescence silicon nano particles
0.04g silica samples are taken, add 0.5mol/L NaOH solution 10mL, are placed in the special glass of microwave radiation
Microwave radiation is carried out in pipe, can obtain fluorescence silicon nano particles.
Microwave radiation condition is：Microwave power 600W；Temperature：100℃；Time：2h.
Embodiment 2
(1) pre-treatment is carried out with acid
Net wheat-straw will be washed with deionized water and be heated at reflux 3h with 10wt% hydrochloric acid water-bath.
(2) silica sample is prepared
The wheat-straw handled well is placed in porcelain crucible, it is in canescence to be heated to alcolhol burner.
(3) microwave radiation prepares fluorescence silicon nano particles
0.05g silica samples are taken, add 0.5mol/L KOH solution 10mL, are placed in the special glass of microwave radiation
Microwave radiation is carried out in pipe, can obtain fluorescence silicon nano particles.
Microwave radiation condition is：Microwave power 600W；Temperature：110℃；Time：2.5h.
Embodiment 3
(1) pre-treatment is carried out with acid
Net bagasse will be washed with deionized water and be heated at reflux 2h with 20wt% hydrochloric acid water-bath.
(2) silica sample is prepared
The bagasse handled well is placed in porcelain crucible, it is in canescence to be heated to alcolhol burner.
(3) microwave radiation prepares fluorescence silicon nano particles
0.03g silica samples are taken, add 0.6mol/L NaOH solution 10mL, are placed in the special glass of microwave radiation
Microwave radiation is carried out in pipe, can obtain fluorescence silicon nano particles.
Microwave radiation condition is：Microwave power 600W；Temperature：130℃；Time：3h.
Embodiment 4
(1) pre-treatment is carried out with acid
Net rice husk will be washed with deionized water and be heated at reflux 3h with 15wt% hydrochloric acid water-bath.
(2) silica sample is prepared
The rice husk handled well is placed in porcelain crucible, it is in canescence to be heated to alcolhol burner.
(3) microwave radiation prepares fluorescence silicon nano particles
0.07g silica samples are taken, add 0.5mol/L KOH solution 10mL, are placed in the special glass of microwave radiation
Microwave radiation is carried out in pipe, can obtain fluorescence silicon nano particles.
Microwave radiation condition is：Microwave power 600W；Temperature：140℃；Time：4h.
Embodiment 5
(1) pre-treatment is carried out with acid
Net bagasse will be washed with deionized water and be heated at reflux 3h with 10wt% hydrochloric acid water-bath.
(2) silica sample is prepared
The rice husk handled well is placed in porcelain crucible, it is in canescence to be heated to alcolhol burner.
(3) microwave radiation prepares fluorescence silicon nano particles
0.04g silica samples are taken, add 0.8mol/L KOH solution 10mL, are placed in the special glass of microwave radiation
Microwave radiation is carried out in pipe, can obtain fluorescence silicon nano particles.
Microwave radiation condition is：Microwave power 600W；Temperature：150℃；Time：3h.
Embodiment 6
(1) pre-treatment is carried out with acid
Net rice husk will be washed with deionized water and be heated at reflux 3h with 15wt% hydrochloric acid water-bath.
(2) silica sample is prepared
The rice husk handled well is placed in porcelain crucible, it is in canescence to be heated to alcolhol burner.
(3) microwave radiation prepares fluorescence silicon nano particles
0.04g silica samples are taken, add 0.5mol/L NaOH solution 10mL, are placed in the special glass of microwave radiation
Microwave radiation is carried out in pipe, can obtain fluorescence silicon nano particles.
Microwave radiation condition is：Microwave power 600W；Temperature：160℃；Time：2h.
Embodiment 7
(1) pre-treatment is carried out with acid
Net rice husk will be washed with deionized water and be heated at reflux 3h with 15wt% hydrochloric acid water-bath.
(2) silica sample is prepared
The bagasse handled well is placed in porcelain crucible, it is in canescence to be heated to alcolhol burner.
(3) microwave radiation prepares fluorescence silicon nano particles
0.04g silica samples are taken, add 0.5mol/L NaOH solution 10mL, are placed in the special glass of microwave radiation
Microwave radiation is carried out in pipe, can obtain fluorescence silicon nano particles.
Microwave radiation condition is：Microwave power 600W；Temperature：160℃；Time：3h.
Embodiment 8
(1) pre-treatment is carried out with acid
Net rice husk will be washed with deionized water and be heated at reflux 3h with 15wt% hydrochloric acid water-bath.
(2) silica sample is prepared
The wheat-straw handled well is placed in porcelain crucible, it is in canescence to be heated to alcolhol burner.
(3) microwave radiation prepares fluorescence silicon nano particles
0.04g silica samples are taken, add 0.5mol/L NaOH solution 10mL, are placed in the special glass of microwave radiation
Microwave radiation is carried out in pipe, can obtain fluorescence silicon nano particles.
Microwave radiation condition is：Microwave power 600W；Temperature：160℃；Time：2.5h.
Embodiment 9
(1) pre-treatment is carried out with acid
Net rice husk will be washed with deionized water and be heated at reflux 3h with 15wt% hydrochloric acid water-bath.
(2) silica sample is prepared
The rice husk handled well is placed in porcelain crucible, it is in canescence to be heated to alcolhol burner.
(3) microwave radiation prepares fluorescence silicon nano particles
0.04g silica samples are taken, add 0.5mol/L NaOH solution 10mL, are placed in the special glass of microwave radiation
Microwave radiation is carried out in pipe, can obtain fluorescence silicon nano particles.
Microwave radiation condition is：Microwave power 600W；Temperature：160℃；Time：6h.
Embodiment 6 is highly preferred embodiment of the present invention, the fluorescence silicon nano particles being prepared by Fig. 1 embodiment 6
Fluorescence spectra can be seen that the fluorescence silicon nano particles being prepared have the feature of excitation wavelength dependence；By Fig. 2 reality
The TEM figures for applying the fluorescence silicon nano particles that example 6 is prepared learn that the water-soluble near-infrared silicon quantum dot being prepared is spherical
And with good monodispersity nano particle, find out that fluorescence silicon nano particles have good lattice bar from HRTEM figures
Line, the fluorescence silicon nano particles for illustrating to be prepared have good crystallinity.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It is appreciated that other embodiment.
Claims (3)
1. a kind of method that green prepares fluorescence silicon nano particles, comprises the steps：
(1) net, addition 38wt%~5wt% acid solution, temperature are washed with deionized water after, shredding rice husk, wheat-straw or bagasse
1h~10h is heated under the water-bath of 50 DEG C~100 DEG C of degree；
(2), step (1) is washed with deionized water to neutrality with acid-treated sample, is put into crucible, is heated to sample and becomes
White powder；
(3), take the white powder obtained by step (2), add 0.1mol/L~10mol/L aqueous slkali, power 15W~
1000W, microwave radiation heating 30min~20h, obtains fluorescence silicon nano particles at 100 DEG C~160 DEG C of temperature.
2. according to the method for claim 1, it is characterised in that：Described acid solution is hydrochloric acid, phosphoric acid, nitric acid or sulfuric acid.
3. according to the method for claim 1, it is characterised in that：Described aqueous slkali is sodium hydroxide solution or potassium hydroxide
Solution.
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| CN106927471A (en) * | 2015-12-31 | 2017-07-07 | 新材料与产业技术北京研究院 | A kind of preparation method of nanometer silica line |
| CN106479487B (en) * | 2016-09-27 | 2018-10-09 | 苏州大学 | A kind of preparation method of fluorescence silicon nano particles |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101920966A (en) * | 2010-07-21 | 2010-12-22 | 化工部长沙设计研究院 | Method for producing porous nano silica and active carbon by utilizing rice hull ash |
| CN103194221A (en) * | 2013-04-25 | 2013-07-10 | 苏州大学 | Method for preparing water-soluble fluorescent silicon nanoparticle by utilizing microwave radiation |
| CN103408009A (en) * | 2013-04-27 | 2013-11-27 | 吉林大学 | Preparation method for coproduction of high-specific-capacitance active carbon and nano silicon dioxide from rice hull |
| CN103710023A (en) * | 2013-12-04 | 2014-04-09 | 华南理工大学 | Method for preparing porous photoluminescence material by utilization of rice husks |
| CN103896265A (en) * | 2012-12-29 | 2014-07-02 | 苏州格瑞展泰再生能源有限公司 | Method for producing activated carbon and inorganic silicon compounds from rice hulls |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2005105244A (en) * | 2003-01-24 | 2005-04-21 | National Institute Of Advanced Industrial & Technology | Semiconductor ultrafine particle and fluorescent substance |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101920966A (en) * | 2010-07-21 | 2010-12-22 | 化工部长沙设计研究院 | Method for producing porous nano silica and active carbon by utilizing rice hull ash |
| CN103896265A (en) * | 2012-12-29 | 2014-07-02 | 苏州格瑞展泰再生能源有限公司 | Method for producing activated carbon and inorganic silicon compounds from rice hulls |
| CN103194221A (en) * | 2013-04-25 | 2013-07-10 | 苏州大学 | Method for preparing water-soluble fluorescent silicon nanoparticle by utilizing microwave radiation |
| CN103408009A (en) * | 2013-04-27 | 2013-11-27 | 吉林大学 | Preparation method for coproduction of high-specific-capacitance active carbon and nano silicon dioxide from rice hull |
| CN103710023A (en) * | 2013-12-04 | 2014-04-09 | 华南理工大学 | Method for preparing porous photoluminescence material by utilization of rice husks |
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