CN104560030A - Method for environment-friendly preparation of fluorescent silicon nanoparticles - Google Patents
Method for environment-friendly preparation of fluorescent silicon nanoparticles Download PDFInfo
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- CN104560030A CN104560030A CN201510032900.9A CN201510032900A CN104560030A CN 104560030 A CN104560030 A CN 104560030A CN 201510032900 A CN201510032900 A CN 201510032900A CN 104560030 A CN104560030 A CN 104560030A
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Abstract
The invention discloses a method for environment-friendly preparation of fluorescent silicon nanoparticles. The method comprises the following steps: cutting a plant with high silicon content into pieces, cleaning with deionized water, adding into acid liquor, and heating in a water bath; washing a sample subjected to acid treatment to be neutral by using deionized water, putting the sample into a crucible, and heating until the sample becomes white powder; and adding the white powder into an alkali solution, and performing microwave radiation heating to obtain the fluorescent silicon nanoparticles. The method for environment-friendly preparation of the fluorescent silicon nanoparticles is completely implemented in a water phase, is cheap in raw material, is environmentally friendly, is safe in operation, is quick, simple and convenient, and is small in toxicity, and the obtained fluorescent silicon nanoparticles have very good monodispersity and fluorescent property, are high in quantum yield, good in storage stability and good in water solubility, and can be widely applied to various optical correlation fields as a fluorescent marker.
Description
Technical field
The invention belongs to silicon nano material technical field, relate to a kind of preparation method of fluorescence silicon nano particles, the plant high by silicon content being specifically related to a kind of green prepares the method for fluorescence silicon nano particles.
Background technology
The silicon nano material of functionalization has good optical/electrical/mechanical properties, surface modificability and good unique character such as compatible, and thus the silicon nano material of people to functionalization has extremely strong interest (see 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 nano materials, because it has good biocompatibility and a hypotoxicity and is expected at biology and is medically applied (see 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.).Up to now, the preparation method of fluorescence silicon nano particles needs expensive or poisonous silicon precursor solution, such as silicon nanowires, bulk silicon, organosilicon small molecules, also needs to add organic reagent, such as alkene, alkane, alcohol compound in the process of synthesis.The step of synthesis is usually more, and environmental pollution also to be caused (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.).
As everyone knows, element silicon is contained in the middle of plant.And the silicone content of some plant is relatively high, the silicone content in Equisetum and grass can account for 50% ~ 70% of plant ass.But the method up to now, utilizing the natural materials of this cheap environmental protection to prepare fluorescence silicon nano particles there is no report.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of environmental protection, operational safety, the fast and convenient method preparing fluorescence silicon nano particles.
Concrete, the invention provides following technical scheme:
The method of Green synthesis fluorescence silicon nano particles of the present invention, comprises the steps:
(1), by the plant of silicon content 10wt% ~ 35wt% subtract broken rear deionized water to clean, add the acid solution of 38wt% ~ 5wt%, under the water-bath of temperature 50 C ~ 100 DEG C, heat 1h ~ 10h;
Preferably, the plant of described silicon content 10wt% ~ 35wt% is grass, bryophyte, Lycophytina class plant, pteridophyte, Ping Cao section class plant, sedge, composite family artemisia, Violaceae plant, Equisetaceae plant or madder wort.
Preferably, described acid solution is hydrochloric acid, phosphoric acid, nitric acid or sulfuric acid.
(2), by the acid-treated sample deionized water of step (1) be washed till neutrality, put into crucible, be heated to sample and become white powder;
(3), get the white powder of step (2) gained, add the alkaline solution of 0.1mol/L ~ 10mol/L, at power 15W ~ 1000W, carry out microwave radiation heating 30min ~ 20h at temperature 100 DEG C ~ 160 DEG C, obtains fluorescence silicon nano particles.
Preferably, described alkaline solution is sodium hydroxide solution or potassium hydroxide solution.
The method of Green synthesis fluorescence silicon nano particles of the present invention, carry out in aqueous phase completely, raw material is cheap, environmental protection, operational safety, fast and convenient, toxicity is little, the fluorescence silicon nano particles of gained have good monodispersity and photoluminescent property, quantum yield is high, stability in storage is good, has good water-soluble, can be widely used in various optical correlation field as fluorescent marker.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme in the embodiment of the present invention, below the accompanying drawing used required in describing embodiment is briefly described, apparently, accompanying drawing for the present invention in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the fluorescence spectrum figure of the fluorescence silicon nano particles that preferred embodiment 6 prepares, and excitation wavelength is 300nm ~ 500nm;
Fig. 2 is transmission electron microscope (TEM) figure and high resolution TEM (HRTEM) figure of the fluorescence silicon nano particles that preferred embodiment 6 prepares, wherein a) be TEM figure, b) be HRTEM figure.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is described in detail.
The present invention's raw material used freely can be buied by market, and chemical agent is analytical pure; Microwave reactor model for the preparation of fluorescence silicon nano particles: NOVASII, is purchased from the Preekem company in Shanghai.
Embodiment 1
(1) pre-treatment is carried out with acid
By the hydrochloric acid water-bath reflux 3h of rice husk 10wt% cleaned with deionized water.
(2) silica sample is prepared
The rice husk handled well is placed in porcelain crucible, is heated in canescence with spirit lamp.
(3) microwave radiation prepares fluorescence silicon nano particles
Get 0.04g silica sample, add the NaOH solution 10mL of 0.5mol/L, be placed in the special Glass tubing of microwave radiation and carry out microwave radiation, can fluorescence silicon nano particles be obtained.
Microwave radiation condition is: microwave power 600W; Temperature: 100 DEG C; Time: 2h.
Embodiment 2
(1) pre-treatment is carried out with acid
By the hydrochloric acid water-bath reflux 3h of wheat-straw 10wt% cleaned with deionized water.
(2) silica sample is prepared
The wheat-straw handled well is placed in porcelain crucible, is heated in canescence with spirit lamp.
(3) microwave radiation prepares fluorescence silicon nano particles
Get 0.05g silica sample, add the KOH solution 10mL of 0.5mol/L, be placed in the special Glass tubing of microwave radiation and carry out microwave radiation, can fluorescence silicon nano particles be obtained.
Microwave radiation condition is: microwave power 600W; Temperature: 110 DEG C; Time: 2.5h.
Embodiment 3
(1) pre-treatment is carried out with acid
By the hydrochloric acid water-bath reflux 2h of bagasse 20wt% cleaned with deionized water.
(2) silica sample is prepared
The bagasse handled well is placed in porcelain crucible, is heated in canescence with spirit lamp.
(3) microwave radiation prepares fluorescence silicon nano particles
Get 0.03g silica sample, add the NaOH solution 10mL of 0.6mol/L, be placed in the special Glass tubing of microwave radiation and carry out microwave radiation, can fluorescence silicon nano particles be obtained.
Microwave radiation condition is: microwave power 600W; Temperature: 130 DEG C; Time: 3h.
Embodiment 4
(1) pre-treatment is carried out with acid
By the hydrochloric acid water-bath reflux 3h of rice husk 15wt% cleaned with deionized water.
(2) silica sample is prepared
The rice husk handled well is placed in porcelain crucible, is heated in canescence with spirit lamp.
(3) microwave radiation prepares fluorescence silicon nano particles
Get 0.07g silica sample, add the KOH solution 10mL of 0.5mol/L, be placed in the special Glass tubing of microwave radiation and carry out microwave radiation, can fluorescence silicon nano particles be obtained.
Microwave radiation condition is: microwave power 600W; Temperature: 140 DEG C; Time: 4h.
Embodiment 5
(1) pre-treatment is carried out with acid
By the hydrochloric acid water-bath reflux 3h of bagasse 10wt% cleaned with deionized water.
(2) silica sample is prepared
The rice husk handled well is placed in porcelain crucible, is heated in canescence with spirit lamp.
(3) microwave radiation prepares fluorescence silicon nano particles
Get 0.04g silica sample, add the KOH solution 10mL of 0.8mol/L, be placed in the special Glass tubing of microwave radiation and carry out microwave radiation, can fluorescence silicon nano particles be obtained.
Microwave radiation condition is: microwave power 600W; Temperature: 150 DEG C; Time: 3h.
Embodiment 6
(1) pre-treatment is carried out with acid
By the hydrochloric acid water-bath reflux 3h of rice husk 15wt% cleaned with deionized water.
(2) silica sample is prepared
The rice husk handled well is placed in porcelain crucible, is heated in canescence with spirit lamp.
(3) microwave radiation prepares fluorescence silicon nano particles
Get 0.04g silica sample, add the NaOH solution 10mL of 0.5mol/L, be placed in the special Glass tubing of microwave radiation and carry out microwave radiation, can fluorescence silicon nano particles be obtained.
Microwave radiation condition is: microwave power 600W; Temperature: 160 DEG C; Time: 2h.
Embodiment 7
(1) pre-treatment is carried out with acid
By the hydrochloric acid water-bath reflux 3h of rice husk 15wt% cleaned with deionized water.
(2) silica sample is prepared
The bagasse handled well is placed in porcelain crucible, is heated in canescence with spirit lamp.
(3) microwave radiation prepares fluorescence silicon nano particles
Get 0.04g silica sample, add the NaOH solution 10mL of 0.5mol/L, be placed in the special Glass tubing of microwave radiation and carry out microwave radiation, can fluorescence silicon nano particles be obtained.
Microwave radiation condition is: microwave power 600W; Temperature: 160 DEG C; Time: 3h.
Embodiment 8
(1) pre-treatment is carried out with acid
By the hydrochloric acid water-bath reflux 3h of rice husk 15wt% cleaned with deionized water.
(2) silica sample is prepared
The wheat-straw handled well is placed in porcelain crucible, is heated in canescence with spirit lamp.
(3) microwave radiation prepares fluorescence silicon nano particles
Get 0.04g silica sample, add the NaOH solution 10mL of 0.5mol/L, be placed in the special Glass tubing of microwave radiation and carry out microwave radiation, can fluorescence silicon nano particles be obtained.
Microwave radiation condition is: microwave power 600W; Temperature: 160 DEG C; Time: 2.5h.
Embodiment 9
(1) pre-treatment is carried out with acid
By the hydrochloric acid water-bath reflux 3h of rice husk 15wt% cleaned with deionized water.
(2) silica sample is prepared
The rice husk handled well is placed in porcelain crucible, is heated in canescence with spirit lamp.
(3) microwave radiation prepares fluorescence silicon nano particles
Get 0.04g silica sample, add the NaOH solution 10mL of 0.5mol/L, be placed in the special Glass tubing of microwave radiation and carry out microwave radiation, can fluorescence silicon nano particles be obtained.
Microwave radiation condition is: microwave power 600W; Temperature: 160 DEG C; Time: 6h.
Embodiment 6 is most preferred embodiment of the present invention, and the fluorescence spectrum figure of the fluorescence silicon nano particles prepared by the embodiment 6 of Fig. 1 can find out that the fluorescence silicon nano particles prepared have the dependent feature of excitation wavelength; The TEM figure of the fluorescence silicon nano particles prepared by the embodiment 6 of Fig. 2 learns that the water-soluble near infrared silicon quantum dot prepared is spherical and has the nano particle of good monodispersity, find out that fluorescence silicon nano particles have good lattice fringe from HRTEM figure, illustrate that the fluorescence silicon nano particles prepared have good crystallinity.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should by specification sheets integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (4)
1. a method for Green synthesis fluorescence silicon nano particles, comprises the steps:
(1), by the plant of silicon content 10wt% ~ 35wt% subtract broken rear deionized water to clean, add the acid solution of 38wt% ~ 5wt%, under the water-bath of temperature 50 C ~ 100 DEG C, heat 1h ~ 10h;
(2), by the acid-treated sample deionized water of step (1) be washed till neutrality, put into crucible, be heated to sample and become white powder;
(3), get the white powder of step (2) gained, add the alkaline solution of 0.1mol/L ~ 10mol/L, at power 15W ~ 1000W, carry out microwave radiation heating 30min ~ 20h at temperature 100 DEG C ~ 160 DEG C, obtains fluorescence silicon nano particles.
2. method according to claim 1, is characterized in that: the plant of described silicon content 10wt% ~ 35wt% is grass, bryophyte, Lycophytina class plant, pteridophyte, Ping Cao section class plant, sedge, composite family artemisia, Violaceae plant, Equisetaceae plant or madder wort.
3. method according to claim 1, is characterized in that: described acid solution is hydrochloric acid, phosphoric acid, nitric acid or sulfuric acid.
4. method according to claim 1, is characterized in that: described alkaline solution is sodium hydroxide solution or potassium hydroxide solution.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106479487A (en) * | 2016-09-27 | 2017-03-08 | 苏州大学 | A kind of preparation method of fluorescence silicon nano particles |
| 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 |
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| 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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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2004065296A1 (en) * | 2003-01-24 | 2004-08-05 | National Institute Of Advanced Industrial Science And Technology | Semiconductor ultrafine particles, fluorescent material, and light-emitting device |
| 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 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN106479487A (en) * | 2016-09-27 | 2017-03-08 | 苏州大学 | A kind of preparation method of fluorescence silicon nano particles |
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