CN104445203B - A kind of preparation method of silicon quantum dot - Google Patents
A kind of preparation method of silicon quantum dot Download PDFInfo
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- CN104445203B CN104445203B CN201410751335.7A CN201410751335A CN104445203B CN 104445203 B CN104445203 B CN 104445203B CN 201410751335 A CN201410751335 A CN 201410751335A CN 104445203 B CN104445203 B CN 104445203B
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Abstract
A kind of preparation method of silicon quantum dot, comprise the following steps: (1) gets silicon raw material, be placed in hydrothermal reaction kettle, react after adding distil water, described silicon raw material is monocrystalline silicon piece or monocrystalline silica flour, the mass ratio of described silicon raw material and distilled water is 1:200-1:20000, and temperature of reaction is 150-240 DEG C, and the reaction times is 4-24h.(2) reactant step (1) obtained filters, and obtains colourless, clear soln, is the aqueous solution of siliceous quantum dot.The present invention has green non-pollution, technique is simple, the advantage such as cost is low, easy control of reaction conditions, reaction times are short, prepared silicon quantum dot is under 240-460nm excitation, turn blue green fluorescence (410-550nm), available should in fields such as optics, catalysis, bio-medical, sensings.
Description
Technical field
The present invention relates to a kind of technique simple, easy control of reaction conditions, the reaction times, short available should in the preparation method of the silicon quantum dot in the fields such as optics, catalysis, bio-medical, sensing.
Technical background
Silicon quantum dot is a kind of fluorescence lifetime length, hypotoxicity, have the semiconductor nano material of good biocompatibility.Make it in laser apparatus, photodiode, bio-medical, catalysis, biosensor etc., have good using value, thus cause the extensive concern of people.At present, there is the method much preparing silicon quantum dot, such as, in glass and SiO2, prepare silicon quantum dot, by injecting high-energy silicon ion and 1100 DEG C of annealing, melt coated material by spark and laser ablation and produce independent silicon quantum dot in quartz.Or use silane or other silicon sources, by smoulder, thermolysis gas phase prepares the silicon quantum dot of separation.Silicon quantum dot is prepared exactly in addition by electrochemical etching silicon chip.Chinese patent disclosed " a kind of large scale production method of silicon quantum dot " (CN103754880A), comprising: preparation reaction precursor liquid, is mixed with mixed solvent by tensio-active agent and base solvent, raw silicon nano-powder dispersion in mixed solvent; Naturally leave standstill or low-speed centrifugal, isolate the silicon nano power colloid of good dispersity; Acid droplet is added silicon nano power colloid, to implement oxidation-corrosion reaction, produces the good silicon quantum dot of size evenness; Utilize ultraviolet band laser device and spectrograph, in real time the characteristics of luminescence of monitoring product, the luminous peak position realizing product controls; Quantum dot cleaning and filtration.The method has and can be mass-produced, productive rate and purity high, luminous peak position is adjustable, and working condition requires the advantages such as low.Generally speaking, although the preparation method of this existing silicon quantum dot can prepare silicon quantum dot, there is the defects such as productive rate is low, cost is high, the very difficult control of long reaction time, size of particles.
Summary of the invention
The present invention exists mainly for the method preparing silicon quantum dot at present that productive rate is low, cost is high, size of particles technical problem very rambunctious, provides that a kind of green non-pollution, technique are simple, the preparation method of silicon quantum dot that easy control of reaction conditions, reaction times are short.
For achieving the above object, embodiment of the present invention are: a kind of preparation method of silicon quantum dot, comprises the following steps:
(1) get silicon raw material, be placed in hydrothermal reaction kettle, react after adding distil water, described silicon raw material is monocrystalline silicon piece or monocrystalline silica flour, and the mass ratio of described silicon raw material and distilled water is 1:200-1:20000, and temperature of reaction is 150-240 DEG C, and the reaction times is 4-24h.
(2) reactant step (1) obtained filters, and obtains colourless, clear soln, is the aqueous solution of siliceous quantum dot.
As preferably, described silicon raw material is monocrystalline silica flour.
As preferably, the mass ratio of described silicon raw material and distilled water is 1:2000
As preferably, temperature of reaction is 220 DEG C.
As preferably, the reaction times is 8h.
The present invention prepares silicon quantum dot to be had and has following advantage: (1) green non-pollution; (2) technique is simple, and cost is low; (3) easy control of reaction conditions; (4) reaction times is short.Silicon quantum dot prepared by the present invention under 240-460nm excitation, the green fluorescence that turns blue (410-550nm), available should in fields such as optics, catalysis, bio-medical, sensings.
Accompanying drawing explanation
Fig. 1 is the fluorescent emission collection of illustrative plates under different excitation wavelength excites of silicon quantum dot prepared by embodiment 1.
Fig. 2 is the fluorescent emission collection of illustrative plates under different excitation wavelength excites of silicon quantum dot prepared by embodiment 2.
Fig. 3 is the fluorescent emission collection of illustrative plates under different excitation wavelength excites of silicon quantum dot prepared by embodiment 3.
Fig. 4 is the fluorescent emission collection of illustrative plates under different excitation wavelength excites of silicon quantum dot prepared by embodiment 4.
Embodiment
Exemplarily the present invention is described in detail further below in conjunction with specific embodiment.
In embodiment, used monocrystalline silicon piece or monocrystalline silica flour are commercially available below, can be obtained by commercial sources.
Embodiment 1: take monocrystalline silicon piece 20mg, be placed in hydrothermal reaction kettle, adds 40g distilled water.16h is reacted at 160 DEG C.Afterwards, the reactant obtained is filtered, obtains colourless, clear soln, be the aqueous solution of siliceous quantum dot.
Embodiment 2: take monocrystalline silica flour 20mg, be placed in hydrothermal reaction kettle, add 40g distilled water.5h is reacted at 220 DEG C.Afterwards, the reactant obtained is filtered, obtains colourless, clear soln, be the aqueous solution of siliceous quantum dot.
Embodiment 3: take monocrystalline silica flour 40mg, be placed in hydrothermal reaction kettle, add 40g distilled water.24h is reacted at 180 DEG C.Afterwards, the reactant obtained is filtered, obtains colourless, clear soln, be the aqueous solution of siliceous quantum dot.
Embodiment 4: take monocrystalline silica flour: 20mg, be placed in hydrothermal reaction kettle, adds 40g distilled water, at 220 DEG C, react 8h.Afterwards, the reactant obtained is filtered, obtains colourless, clear soln, be the aqueous solution of siliceous quantum dot.
Embodiment 4 is preferred version.
Claims (4)
1. a preparation method for silicon quantum dot, is characterized in that, comprises the following steps:
(1) get silicon raw material, be placed in hydrothermal reaction kettle, react after adding distil water, described silicon raw material is monocrystalline silicon piece or monocrystalline silica flour, and the mass ratio of described silicon raw material and distilled water is 1:200-1:20000, and temperature of reaction is 150-240 DEG C, and the reaction times is 4-24h;
(2) reactant step (1) obtained filters, and obtains colourless, clear soln, is the aqueous solution of siliceous quantum dot.
2. the preparation method of silicon quantum dot according to claim 1, is characterized in that, the mass ratio of described silicon raw material and distilled water is 1:2000.
3. the preparation method of silicon quantum dot according to claim 1, is characterized in that, temperature of reaction is 220 DEG C.
4. the preparation method of silicon quantum dot according to claim 1, is characterized in that, the reaction times is 8h.
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| CN201410751335.7A CN104445203B (en) | 2014-12-10 | 2014-12-10 | A kind of preparation method of silicon quantum dot |
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| CN201410751335.7A CN104445203B (en) | 2014-12-10 | 2014-12-10 | A kind of preparation method of silicon quantum dot |
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| CN104445203A CN104445203A (en) | 2015-03-25 |
| CN104445203B true CN104445203B (en) | 2016-01-20 |
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| CN105542746B (en) * | 2015-12-18 | 2018-07-20 | 湖南科技大学 | A kind of fluorescence silicon quantum dot material of polyisopropyl acrylamide functionalization and preparation method thereof |
| CN108362670A (en) * | 2018-02-12 | 2018-08-03 | 长春工业大学 | A kind of preparation method and applications of automobile formaldehyde examination fluorescence nano sensor |
| CN108844937B (en) * | 2018-08-07 | 2020-09-08 | 福建中医药大学 | Water-soluble fluorescent silicon dot and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1569628A (en) * | 2004-05-11 | 2005-01-26 | 湖南大学 | Method for preparing self assembled growth silicon nano-tube and silicon nano-line by hydrothermal method |
| CN103754880A (en) * | 2014-01-20 | 2014-04-30 | 复旦大学 | Large-scale production method of silicon quantum dots |
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| JP2009096669A (en) * | 2007-10-17 | 2009-05-07 | Konica Minolta Medical & Graphic Inc | Silicon quantum dot and biomaterial labeling agent using the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1569628A (en) * | 2004-05-11 | 2005-01-26 | 湖南大学 | Method for preparing self assembled growth silicon nano-tube and silicon nano-line by hydrothermal method |
| CN103754880A (en) * | 2014-01-20 | 2014-04-30 | 复旦大学 | Large-scale production method of silicon quantum dots |
Non-Patent Citations (1)
| Title |
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| Silicon quantum dot superlattice and metallic conducting behaviour in porous silicon;Qianwang Chen et al.;《J. Phys.: Condens. Matter》;19971231;第569-572 * |
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