CN105969344A - Silicon quantum dot aqueous phase preparation method - Google Patents

Silicon quantum dot aqueous phase preparation method Download PDF

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CN105969344A
CN105969344A CN201610387705.2A CN201610387705A CN105969344A CN 105969344 A CN105969344 A CN 105969344A CN 201610387705 A CN201610387705 A CN 201610387705A CN 105969344 A CN105969344 A CN 105969344A
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quantum dot
silicon quantum
aqueous phase
phase preparation
silicon
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赵丹
马诗瑶
郝健
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South Central Minzu University
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South Central University for Nationalities
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    • C09K11/59—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing silicon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

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Abstract

The invention discloses a silicon quantum dot aqueous phase preparation method. The method includes the following steps that firstly, a reduction agent and a silane coupling agent are obtained and dissolved in water under inertia gas protection, wherein the molar ratio of the silane coupling agent to the reduction agent is 1:(0.2-10); secondly, the mixed solution obtained in the first step is conveyed into a high-pressure reaction kettle to be heated to 140-220 DEG C, and a silicon quantum dot solution can be obtained after reaction; or the mixed solution obtained in the first step is conveyed into a microwave reaction kettle to be heated to 140-220 DEG C, and a silicon quantum dot solution can be obtained after reaction; thirdly, the silicon quantum dot solution obtained in the second step is mixed with an organic solvent, centrifugation is conducted, supernate is removed, drying is conducted, and solid silicon quantum dots are obtained, wherein the reaction agent is a mixture composed of two or more of citric acid, sodium sulfite, sodium borohydride, sodium citrate, ascorbic acid, urea, thiourea, hydrazine hydrate, L-cysteine, bovine serum albumin or modified ovine serum albumin.

Description

A kind of aqueous phase preparation method of silicon quantum dot
Technical field
The invention belongs to the preparation method technical field of nano material, specifically disclose a kind of with silane coupler as silicon Source, utilizes the synergism of reducing agent, uses hydro-thermal method or the preparation side of microwave method synthesis in water water soluble fluorescence silicon quantum dot Method.
Background technology
Quantum dot, is a kind of, diameter elementary composition by II-VI group or iii-v quasi-zero-dimension nano at 1 ~ 10nm Material.Silicon is indirect band-gap semiconductor, and traditional silicon nano material luminescence is the most weak, is restricted in the application of device.So And, when its size constantly reduces, quantum size effect makes the fluorescence intensity of silicon quantum dot strengthen, and shows and direct band gap half The photophysical property that conductor is similar.Additionally, compared with traditional II-VI group or iii-v quantum dot, silicon quantum dot photochemistry property Of fine quality good, good biocompatibility, abundant raw material, can be with large-scale production.At present in optoelectronics, solar energy conversion, biological biography The aspect such as sensor, fluorescent probe has a wide range of applications.
Before this about in the report of the preparation of silicon quantum dot, the reducing agent mentioned is mainly sodium citrate, and its productivity is low, It is not suitable for factory to produce on a large scale yet.
Summary of the invention
The technical problem to be solved in the present invention is that existing method prepares silicon quantum dot, and quantum yield is low.
In order to solve above-mentioned technical problem, the present invention provides the preparation method of a kind of new silicon quantum dot: use silane even Connection agent, utilizes the synergism of two or more reducing agent, uses hydro-thermal method or microwave method aqueous phase to prepare the water solublity of high fluorescence Silicon quantum dot.This synthetic method is simple to operate, abundant raw material source, can be effectively improved the quantum yield of silicon quantum dot and steady Qualitative, beneficially structure of modification and large-scale production.
The aqueous phase preparation method of the silicon quantum dot that the present invention provides, comprises the steps:
(1) under inert gas shielding, take reducing agent and silane coupler be soluble in water, silane coupler and reducing agent mole Ratio is 1:0.2 ~ 10；
(2) mixed solution that step (1) obtains is proceeded to be heated in autoclave 140-220 DEG C, the most available after reaction Silicon quantum dot solution；Or the mixed solution that step (1) obtains is proceeded to be heated in microwave reaction kettle 140-220 DEG C, reaction After silicon quantum dot solution；
(3) the silicon quantum dot solution that step (2) obtains is mixed with organic solvent, centrifugal, remove supernatant, be dried, must consolidate Body silicon quantum dot；
Wherein said reducing agent is citric acid, sodium sulfite, sodium borohydride, sodium citrate, ascorbic acid, carbamide, thiourea, hydration Two or more mixture in hydrazine, Cys, bovine serum albumin or degeneration bovine serum albumin.
Preferably, described reducing agent includes citric acid and sodium borohydride.
Preferably, described reducing agent also includes sodium sulfite.
Preferably, described reducing agent be the mol ratio of citric acid, sodium borohydride and sodium sulfite be 1:0.2-5:0.2-5's Mixture.
Preferably, described reducing agent is the mixture that mol ratio is 1:0.2-5 of citric acid and sodium borohydride.
Preferably, described silane coupler is 3-aminopropyl trimethoxysilane, 3-aminopropyl triethoxysilane, N-ammonia Ethyl-γ-aminopropyltrimethoxysilane, N-aminoethyl-gamma-aminopropyl-triethoxy-silane, N-normal-butyl-3-aminopropyl three Methoxy silane, N-normal-butyl-3-aminopropyl triethoxysilane, N-N-dimethyl-3-TSL 8330 or Diethylenetriamine base propyl trimethoxy silicane.
Preferably, described organic solvent be methanol, ethanol, acetonitrile, acetone, dimethyl sulfoxide, ethyl acetate, oxolane or Isopropanol.
Preferably, in step (3), the volume ratio of silicon quantum dot solution and organic solvent is 1:2-10.
Preferably, in step (2): the mixed solution that step (1) the obtains response time in autoclave is 1- 3.5h；The mixed solution that step (1) the obtains response time in microwave reaction kettle is 5-40min.
Preferably, described noble gas is nitrogen or argon.
Be dried method for for noble gas dry up, lyophilization, vacuum drying.
Compared with prior art, the advantage of the inventive method and having the beneficial effects that:
1. utilizing two or more reducing agent synergism can prepare high fluorescent water-soluble silicon quantum dot, the method is selectable The screening of reducing agent when reducing agent wide variety, beneficially laboratory and factory are prepared on a large scale.
2. the invention provides a kind of simple hydro-thermal method and method that microwave method aqueous phase prepares silicon quantum dot, the method is adopted Being silicon source with silane coupler, synthetic operation is simple, enormously simplify laboratory operating procedures, shortens the response time, and raw material is just Preferably and be easy to get.
3. the silicon quantum dot that the present invention prepares has pH stability, heat stability, salt-resistance and anti-metal ion interference.
4, cooperative effect is the rule that nature is widely present.During such as two or more drug combination, if their work It is consistent with direction, the effect strengthened each other can be reached.Soda acid synergism is also prevalent in the catalysis of enzyme and antibody During.Equally, during synergism also apply be applicable to the synthesis of quantum dot.The substance classes with reproducibility is enriched, its reduction All there is significant difference in ability, mechanism of action, response speed.When being used alone a kind of reducing agent (such as citric acid, sodium borohydride Deng) time, the quantum dot prepared, its quantum yield only has 5%-10%.The present invention utilizes the synergism of two kinds of reducing agents, by two Kind or two or more reducing agent are provided commonly for the preparation of quantum dot, can improve silicon quantum dot quantum yield to 60%-70%.
Accompanying drawing explanation
The fluorescence pattern of three kinds of silicon quantum dot solution in Fig. 1: embodiment 1.
The TEM figure of the silicon quantum dot of preparation in Fig. 2: embodiment 1.
Fig. 3: change in embodiment 1 impact on silicon quantum dot fluorescence intensity of two kinds of reducing agent mol ratios.
The pH response diagram of gained silicon quantum dot in Fig. 4: embodiment 1.
The silicon quantum dot solution obtained in Fig. 5: embodiment 1 fluorescence intensity figure at 30 DEG C-55 DEG C.
Fig. 6: add many kinds of metal ions in the silicon quantum dot obtained in embodiment 1, measure its fluorescence intensity.
Fig. 7: joined in variable concentrations sodium chloride solution by the silicon quantum dot obtained in embodiment 1, measures its fluorescence strong Degree.
Detailed description of the invention
The invention will be further described with specific embodiment below in conjunction with the accompanying drawings, so that those skilled in the art is permissible It is better understood from the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
Embodiment 1
The method being silicon source water heat transfer water-soluble silicon quantum dot with 3-aminopropyl trimethoxysilane, its concrete steps are such as Under:
(1) under the protection of nitrogen, citric acid and sodium borohydride are dissolved in deionized water, add 3-aminopropyl trimethoxy Base silane as silicon source, controls silicon source: citric acid: the mol ratio=1:0.2:0.2 of sodium borohydride, wherein, and 3-aminopropyl trimethoxy Base silane concentration in water is 44mmol/L, and citric acid concentration in water is 8.8mmol/L, dense in water of sodium borohydride Degree is 8.8mmol/L.
(2) mixed solution proceeds to be heated in autoclave 140 DEG C, react 3.5h, obtain silicon quantum dot solution.
(3) the silicon quantum dot solution of preparation is mixed homogeneously by the volume ratio of 1:3 with methanol, be centrifuged by 8000r/min 10min, removes supernatant, and by lyophilization, gained precipitation is obtained solid silicon quantum dot.
To be dissolved in 0.1 mol/L H2SO4Quinoline sulfate in solution (refraction coefficient (η) is 1.33) is object of reference (amount Sub-productivity=54%).By comparing fluorescence area (Ex=320 nm) produce with the quantum of the ratio calculation silicon quantum dot of absorbance Rate.All of sample (η=1.33) soluble in water, and control its absorbance under 320 nm less than 0.1, relative quantum is produced The computing formula of rate is as follows:
ΦX = ΦST (GradX/ GradST) (ηX 2/ ηST 2)
Φ be quantum yield, Grad be the ratio of fluorescence area and absorbance, η is the refraction coefficient of solvent, and ST represents reference material Matter, X representative sample.
Calculating after testing, the silicon quantum dot of the present embodiment, quantum yield is up to 67%, illustrates that the synergism of reducing agent is Highly significant.
The fluorescence pattern of the silicon quantum dot solution that the embodiment of the present invention 1 prepares is shown in Fig. 1.
The solid silicon quantum dot obtained in above-mentioned experiment is dissolved in the water, Purification by filtration, measure its particle diameter by TEM big Little, as in figure 2 it is shown, the silicon quantum dot that the present embodiment prepares, particle diameter is at about 31nm.
The study on the stability of silicon quantum dot:
By soluble in water for the solid silicon quantum dot obtained by the present embodiment, obtain quantum dot solution, and to it in different environments Stability investigate:
In the Tris-HCL solution of 900 μ LpH=4-12, add the silicon quantum dot solution of 100 μ L, survey its fluorescence intensity, the amount of obtaining The pH response diagram of son point, result is shown in such as Fig. 4.Silicon quantum dot is respectively provided with strong fluorescence under different pH value as can be seen from Figure 4, Illustrate that the silicon quantum dot that the present embodiment prepares has pH stability.
Being placed in by quantum dot solution in 30 DEG C of-55 DEG C of environment, measure its fluorescence intensity, result is shown in Fig. 5.Can from Fig. 5 Going out in certain scope, the silicon quantum dot that the present embodiment prepares has good heat stability.
Adding concentration in quantum dot solution is the metal ion of 100mmol/L, measures its fluorescence intensity, and result is shown in Fig. 6.From Fig. 6 can be seen that the silicon quantum dot that the present embodiment prepares has good anti-metal ion interference ability.
Adding the sodium chloride of variable concentrations in quantum dot solution, measure its fluorescence intensity, result is shown in Fig. 7, permissible from Fig. 7 Find out that the silicon quantum dot that the present embodiment prepares has preferable salt-resistance.
Embodiment 2
The method being silicon source water heat transfer water-soluble silicon quantum dot with 3-aminopropyl trimethoxysilane, its preparation method is same Embodiment 1,3-aminopropyl trimethoxysilane concentration in water is 44mmol/L, and difference is reducing agent citric acid and boron hydrogen The concentration changing sodium is different.3-aminopropyl trimethoxysilane: citric acid: the mol ratio of sodium borohydride is 1:0.2:0.2 ~ 1.Through surveying Fixed, the fluorescence intensity of the silicon quantum dot prepared under different proportion is shown in Fig. 3.
Under each proportioning, quantum yield see table:
3-aminopropyl trimethoxysilane: citric acid: the mol ratio of sodium borohydride 1:0.2:0.2 1:0.2:0.4 1:0.2:0.6 1:0.2:0.8 1:0.2:1
Quantum yield 32% 57% 67% 49% 45%
After measured, the quantum dot that the present embodiment prepares has good pH stability, heat stability, salt-resistance and anti-metal ion Interference.
Can be seen that from upper table, when 3-aminopropyl trimethoxysilane: citric acid: the mol ratio=1:0.2 of sodium borohydride: 0.6, temperature is 140 DEG C, and the response time is 3.5h, for preferred version.
Embodiment 3
The method being silicon source water heat transfer water-soluble silicon quantum dot with 3-aminopropyl triethoxysilane, its concrete steps are such as Under:
(1) under the protection of argon, 3-aminopropyl triethoxysilane is dissolved in deionized water, 3-aminopropyl trimethoxy Silane concentration in water is 44mmol/L, adds sodium borohydride and sodium sulfite, control silicon source: sodium borohydride: sulfurous acid Mol ratio=the 1:1:0.5 of sodium.
(2) solution of stirring and evenly mixing is proceeded to be heated in autoclave 170 DEG C, react 2h, obtain silicon quantum dot molten Liquid.
(3) by gained silicon quantum dot solution in quantum dot: the ratio of ethanol=1:2 is mixed homogeneously with ethanol.By 8000r/ Min is centrifuged 15min, removes supernatant, and by vacuum drying, gained precipitation is obtained solid silicon quantum dot.
The quantum yield of the present embodiment is 50%.
After measured, the quantum dot that the present embodiment prepares has good pH stability, heat stability, salt-resistance and anti-metal Ion interference.
Embodiment 4
The method being silicon source microwave method synthesizing water-solubility silicon quantum dot with N-aminoethyl-gamma-aminopropyl-triethoxy-silane, its Specifically comprise the following steps that
(1) under argon shield, citric acid and sodium sulfite and sodium borohydride are dissolved in deionized water, add N-aminoethyl- Gamma-aminopropyl-triethoxy-silane, N-aminoethyl-gamma-aminopropyl-triethoxy-silane concentration in water is 44mmol/L, makes Silicon source: citric acid: sodium sulfite: the mol ratio of sodium borohydride is 1:1:0.2 ~ 5:0.2 ~ 5,
(2) solution of mix homogeneously is proceeded to be heated in autoclave 220 DEG C, react 15min, obtain quantum dot.
(3) obtained silicon quantum dot solution is pressed quantum dot: isopropanol=1:10 mixes with isopropanol.By 8000r/ Min is centrifuged 10min, removes supernatant, and by lyophilization, gained precipitation is obtained solid silicon quantum dot.
Under each proportioning, quantum yield see table:
N-aminoethyl-gamma-aminopropyl-triethoxy-silane: citric acid: sodium sulfite: the mol ratio of sodium borohydride 1:1:0.2:1 1:1:0.5:1.2 1:1:2:5 1:1:5:0.5 1:1:3:0.2
Quantum yield 35% 63% 57% 42% 30%
After measured, the quantum dot that the present embodiment prepares has good pH stability, heat stability, salt-resistance and anti-metal ion Interference.
Embodiment 5
N-aminoethyl-γ-aminopropyltrimethoxysilane is the method for silicon source microwave method synthesizing water-solubility silicon quantum dot, its tool Body step is as follows:
(1) under the protection of argon, sodium sulfite and hydrazine hydrate are dissolved in deionized water, add N-aminoethyl-γ-ammonia third Base trimethoxy silane, N-aminoethyl-γ-aminopropyltrimethoxysilane concentration in water is 44mmol/L, controls silicon source : sodium sulfite: hydrazine hydrate mol ratio is 1:0.8:1.2,
(2) solution after stirring and evenly mixing is proceeded to be heated in microwave reaction kettle 180 DEG C, react 40min, obtain silicon quantum dot.
(3) by prepared silicon quantum dot solution in quantum dot: the ratio of acetonitrile=1:4 mixes with acetonitrile.By 8000r/min Centrifugal 10min, removes supernatant, and gained precipitation is obtained by the way of drying up with nitrogen solid silicon quantum dot.
The quantum yield of the present embodiment is 25%.
After measured, the quantum dot that the present embodiment prepares has good pH stability, heat stability, salt-resistance and anti-metal Ion interference.
Embodiment 6
The method being silicon source water heat transfer water-soluble silicon quantum dot with 3-aminopropyl trimethoxysilane, its concrete steps are such as Under:
(1) under the protection of nitrogen, 3-aminopropyl trimethoxysilane, bovine serum albumin and carbamide are dissolved in deionization simultaneously In water, 3-aminopropyl trimethoxysilane concentration in water is 44mmol/L, control silicon source: bovine serum albumin: carbamide Mol ratio is 1:0.4:2.5,
(2) solution of mix homogeneously is proceeded to be heated in autoclave 200 DEG C, react 3h, obtain the silicon quantum of functionalization Point.
(3) by obtained silicon quantum dot solution in quantum dot: the ratio of dimethyl sulfoxide=1:5 mixes with dimethyl sulfoxide.Press 8000r/min is centrifuged 10min, removes supernatant, and by lyophilization, gained precipitation is obtained solid silicon quantum dot.
The quantum yield of the present embodiment is 21%.
After measured, the quantum dot that the present embodiment prepares has good pH stability, heat stability, salt-resistance and anti-metal Ion interference.
Embodiment 7
N-aminoethyl-gamma-aminopropyl-triethoxy-silane is the method for silicon source microwave method synthesizing water-solubility silicon quantum dot, its tool Body step is as follows:
(1) under the protection of nitrogen, ascorbic acid and thiourea are dissolved in deionized water, add N-aminoethyl-γ-ammonia third Ethyl triethoxy silicane alkane, N-aminoethyl-gamma-aminopropyl-triethoxy-silane concentration in water is 44mmol/L, makes silicon source: anti- Bad hematic acid: the mol ratio of thiourea is 1:2.5:0.8, proceeds to be heated in autoclave 190 DEG C by the solution of mix homogeneously, instead Answer 5min, obtain quantum dot.
(2) by obtained silicon quantum dot solution in quantum dot: the ratio of ethyl acetate=1:6 mixes with ethyl acetate.Press 8000r/min is centrifuged 10min, removes supernatant, and gained precipitation is obtained by the way of drying up with argon solid silicon quantum dot.
The quantum yield of the present embodiment is 27%.
After measured, the quantum dot that the present embodiment prepares has good pH stability, heat stability, salt-resistance and anti-metal Ion interference.
Comparative example 1
The method being silicon source water heat transfer water-soluble silicon quantum dot with 3-aminopropyl trimethoxysilane, its concrete steps are such as Under:
(1) under the protection of nitrogen, citric acid is dissolved in deionized water, adds 3-aminopropyl trimethoxysilane conduct Silicon source, 3-aminopropyl trimethoxysilane concentration in water is 44mmol/L, control silicon source: mol ratio=1 of citric acid: 0.4,
(2) mixed solution proceeds to be heated in autoclave 140 DEG C, react 3.5h, obtain silicon quantum dot solution.
(3) the silicon quantum dot solution of preparation is mixed homogeneously by the volume ratio of 1:3 with methanol, be centrifuged by 8000r/min 10min, removes supernatant, and by lyophilization, gained precipitation is obtained solid silicon quantum dot.
After testing, the silicon quantum dot of this comparative example, quantum yield is 10%.
The fluorescence pattern of the silicon quantum dot solution that comparative example 1 prepares is shown in Fig. 1, and its fluorescence intensity is significantly lower than embodiment 1 Silicon quantum dot.
After measured, the quantum dot pH stability that this comparative example prepares, heat stability, salt-resistance and anti-metal ion interference Poor.
Comparative example 2
The method being silicon source water heat transfer water-soluble silicon quantum dot with 3-aminopropyl trimethoxysilane, its concrete steps are such as Under:
(1) under the protection of nitrogen, sodium borohydride is dissolved in deionized water, adds 3-aminopropyl trimethoxysilane and make For silicon source, 3-aminopropyl trimethoxysilane concentration in water is 44mmol/L, control silicon source: the mol ratio of sodium borohydride= 1:0.4,
(2) mixed solution proceeds to be heated in autoclave 140 DEG C, react 3.5h, obtain silicon quantum dot solution.
(3) the silicon quantum dot solution of preparation is mixed homogeneously by the volume ratio of 1:3 with methanol, be centrifuged by 8000r/min 10min, removes supernatant, and by lyophilization, gained precipitation is obtained solid silicon quantum dot.
After testing, the silicon quantum dot of this comparative example, quantum yield is 7%.
The fluorescence pattern of the silicon quantum dot solution that comparative example 2 prepares is shown in Fig. 1, and its fluorescence intensity is significantly lower than embodiment 1 Silicon quantum dot.
After measured, the quantum dot pH stability that this comparative example prepares, heat stability, salt-resistance and anti-metal ion interference Poor.
Embodiment described above is only the preferred embodiment lifted by absolutely proving the present invention, the protection model of the present invention Enclose and be not limited to this.The equivalent that those skilled in the art are made on the basis of the present invention substitutes or conversion, all in the present invention Protection domain within.Protection scope of the present invention is as the criterion with claims.

Claims (10)

1. the aqueous phase preparation method of a silicon quantum dot, it is characterised in that comprise the steps:
(1) under inert gas shielding, take reducing agent and silane coupler be soluble in water, silane coupler and reducing agent mole Ratio is 1:0.2 ~ 10；
(2) mixed solution that step (1) obtains is proceeded to be heated in autoclave 140-220 DEG C, the most available after reaction Silicon quantum dot solution；Or the mixed solution that step (1) obtains is proceeded to be heated in microwave reaction kettle 140-220 DEG C, reaction After silicon quantum dot solution；
(3) the silicon quantum dot solution that step (2) obtains is mixed with organic solvent, centrifugal, remove supernatant, be dried, must consolidate Body silicon quantum dot；
Wherein said reducing agent is citric acid, sodium sulfite, sodium borohydride, sodium citrate, ascorbic acid, carbamide, thiourea, hydration Two or more mixture in hydrazine, Cys, bovine serum albumin or degeneration bovine serum albumin.
The aqueous phase preparation method of silicon quantum dot the most according to claim 1, it is characterised in that described reducing agent includes Fructus Citri Limoniae Acid and sodium borohydride.
The aqueous phase preparation method of silicon quantum dot the most according to claim 2, it is characterised in that described reducing agent also includes Asia Sodium sulfate.
The aqueous phase preparation method of silicon quantum dot the most according to claim 3, it is characterised in that described reducing agent is Fructus Citri Limoniae Acid, sodium borohydride and the mixture that mol ratio is 1:0.2-5:0.2-5 of sodium sulfite.
The aqueous phase preparation method of silicon quantum dot the most according to claim 2, it is characterised in that described reducing agent is citric acid The mixture that mol ratio is 1:0.2-5 with sodium borohydride.
The aqueous phase preparation method of silicon quantum dot the most according to claim 1, it is characterised in that described silane coupler is 3- Aminopropyl trimethoxysilane, 3-aminopropyl triethoxysilane, N-aminoethyl-γ-aminopropyltrimethoxysilane, N-ammonia second Base-gamma-aminopropyl-triethoxy-silane, N-normal-butyl-3-aminopropyl trimethoxysilane, N-normal-butyl-3-aminopropyl three second TMOS, N-N-dimethyl-3-TSL 8330 or diethylenetriamine base propyl trimethoxy silicane.
The aqueous phase preparation method of silicon quantum dot the most according to claim 1, it is characterised in that described organic solvent is first Alcohol, ethanol, acetonitrile, acetone, dimethyl sulfoxide, ethyl acetate, oxolane or isopropanol.
The aqueous phase preparation method of silicon quantum dot the most according to claim 1, it is characterised in that silicon quantum dot in step (3) Solution is 1:2-10 with the volume ratio of organic solvent.
The aqueous phase preparation method of silicon quantum dot the most according to claim 1, it is characterised in that in step (2): step (1) The mixed solution the obtained response time in autoclave is 1-3.5h；The mixed solution that step (1) obtains is anti-at microwave Answering the response time in still is 5-40min.
The aqueous phase preparation method of silicon quantum dot the most according to claim 1, it is characterised in that described noble gas is nitrogen Gas or argon.
CN201610387705.2A 2016-06-06 2016-06-06 Silicon quantum dot aqueous phase preparation method Pending CN105969344A (en)

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CN106544012A (en) * 2016-11-04 2017-03-29 兰州大学 High selectivity determines the water soluble fluorescence nano silicon particles synthesis of trace TNP and applies
CN109777401A (en) * 2018-12-31 2019-05-21 华南农业大学 A kind of preparation method of water-soluble blue luminescence silicon quantum dot, its application
CN110735333A (en) * 2019-11-13 2020-01-31 常州大学 Novel dyeing-color fixing method of micromolecular natural dye
CN111100631A (en) * 2019-11-29 2020-05-05 华南农业大学 Multicolor luminous solid silicon dot powder and multifunctional application of preparation method thereof
CN112300795A (en) * 2020-09-30 2021-02-02 江苏大学 Preparation method and application of molecular imprinting fluorescent probe based on silicon quantum dots
CN113149015A (en) * 2021-04-07 2021-07-23 中国石油大学(华东) Carbon-silicon composite quantum dot solution and preparation method thereof, resistance-reducing injection-increasing agent and application
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CN109777401A (en) * 2018-12-31 2019-05-21 华南农业大学 A kind of preparation method of water-soluble blue luminescence silicon quantum dot, its application
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