CN107311179A - A kind of quick method and silicon nano for preparing silicon nano - Google Patents
A kind of quick method and silicon nano for preparing silicon nano Download PDFInfo
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- CN107311179A CN107311179A CN201710448091.9A CN201710448091A CN107311179A CN 107311179 A CN107311179 A CN 107311179A CN 201710448091 A CN201710448091 A CN 201710448091A CN 107311179 A CN107311179 A CN 107311179A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The present invention discloses a kind of quick method and silicon nano for preparing silicon nano, wherein, the quick method for preparing silicon nano includes step：A, add alkali compounds into pre-configured organic alcoholic solution, generate mixed liquor；B, add silester into the mixed liquor, after 1 120min of stirring, liquid after being reacted；C, separation of solid and liquid is carried out to liquid after the reaction, the solid after separation is washed, drying process, that is, obtain silicon nano.Solve in the prior art can not Fast back-projection algorithm uniform particle diameter silicon nano the problem of.
Description
Technical field
The present invention relates to silicon nano field, more particularly to a kind of quick method for preparing silicon nano and silicon nanometer
Particle.
Background technology
Silicon nano（SiNPs）It is widely used to the neck such as electronics, photonic propulsion, biology sensor and drug discovery
Domain.Field generally requires different physicochemical properties when SiNPs is applied to different, such as different particle diameters, surface charge, colloid point
Property and surface roughness etc. are dissipated, and these properties depend on SiNPs size and form.Obtained using traditional sol-gel process
The SiNPs arrived has wider Size Distribution, and SiNPs size and form can be controlled by adjusting response parameter, separately
Outer this method is also very simple, is the prefered method for synthesizing SiNPs.But traditional sol-gel process synthesis SiNPs is to exist
Some limitations：1st, this method needs longer time（It is generally necessary to about 20 hours）；2nd, this method uses ammoniacal liquor as catalyst
It is, it is often unstable in nucleation due to volatility, so as to cause the SiNPs of synthesis less uniform；3rd, in building-up process
The ammonia that middle ammoniacal liquor decomposes release may also be adsorbed to SiNPs surfaces, so as to disturb the processing of next step.4th, SiNPs granularity
Homogeneity may be influenceed by other many factors, so the problem of Control granularity size is still one extremely complex.
Therefore, prior art has yet to be improved and developed.
The content of the invention
In view of above-mentioned the deficiencies in the prior art, it is an object of the invention to provide a kind of quick side for preparing silicon nano
Method and silicon nano, it is intended to solve in the prior art can not Fast back-projection algorithm uniform particle diameter silicon nano the problem of.
Technical scheme is as follows：
A kind of quick method for preparing silicon nano, wherein, including step：
A, add alkali compounds into pre-configured organic alcoholic solution, generate mixed liquor；
B, add silester into the mixed liquor, after stirring 1-120min, liquid after being reacted；
C, separation of solid and liquid is carried out to liquid after the reaction, the solid after separation is washed, drying process, that is, obtain silicon nanometer
Particle.
A kind of quick method for preparing silicon nano, wherein, the Organic Alcohol is ethanol or isopropanol.
A kind of quick method for preparing silicon nano, wherein, in the aqueous solution of the Organic Alcohol, the concentration of Organic Alcohol is
50%-100%。
A kind of quick method for preparing silicon nano, wherein, the alkali compounds is solid base or aqueous slkali.
A kind of quick method for preparing silicon nano, wherein, the alkali compounds is potassium hydroxide or sodium hydroxide.
A kind of quick method for preparing silicon nano, wherein, the mixed liquor neutral and alkali compound concentration is 5-
200mmol/L。
A kind of quick method for preparing silicon nano, wherein, the concentration of the silester is 5-300 mmol/L.
A kind of quick method for preparing silicon nano, wherein, in the step C, the centrifugation rate of separation of solid and liquid is
6000-8000 rmp/min, centrifugation time is 10-15min.
A kind of quick method for preparing silicon nano, wherein, step is also included after the step B：
The deionized water that liquid is accumulated after 10-15 times of addition is reacted in liquid after to reaction.
A kind of silicon nano, wherein, it is prepared from using the above method.
Beneficial effect：The present invention is pre-configured with organic alcoholic solution by the present invention, then to the aqueous solution of the Organic Alcohol
The middle alkali added as catalyst, adds silester, separation of solid and liquid was to obtain surface light after 1 ~ 120 minute by stirring reaction
The silicon nano of sliding and uniform particle diameter, and by controlling the particle diameter of reaction time controllable prepared silicon nano big
It is small, solve in the prior art can not Fast back-projection algorithm uniform particle diameter silicon nano the problem of.
Brief description of the drawings
Fig. 1 is the flow chart of the quick method preferred embodiment for preparing silicon nano of the present invention.
Fig. 2 is the infrared spectrogram of the silicon nano prepared by the embodiment of the present invention 2.
Fig. 3 is the ESEM of silicon nano prepared when the stirring reaction time is 30min in the embodiment of the present invention 4
Figure.
Fig. 4 is the ESEM of silicon nano prepared when the stirring reaction time is 45min in the embodiment of the present invention 4
Figure.
Fig. 5 is the ESEM of silicon nano prepared when the stirring reaction time is 60min in the embodiment of the present invention 4
Figure.
Embodiment
The present invention provides a kind of quick method and silicon nano for preparing silicon nano, for make the purpose of the present invention,
Technical scheme and effect are clearer, clear and definite, and the present invention is described in more detail below.It should be appreciated that described herein
Specific embodiment only to explain the present invention, is not intended to limit the present invention.
A kind of quick method for preparing silicon nano, as shown in figure 1, including step：
S1, add alkali compounds into pre-configured organic alcoholic solution, generate mixed liquor；
S2, add silester into the mixed liquor, after stirring 1-120min, liquid after being reacted；
S3, separation of solid and liquid is carried out to liquid after the reaction, the solid after separation is washed, drying process, that is, obtain silicon and receive
Rice corpuscles.
Because alkali can be catalyzed the synthesis of silicon nano, and the synthesis precursor silester of silicon nano need to be dissolved in
In Organic Alcohol, thus the present invention first configures the aqueous solution of Organic Alcohol, and the alkali compounds as catalyst is then added thereto,
Formed silester can be dissolved and alkali soluble solution can be played to the mixed liquor of its catalytic action again.
In the present invention, alkali compounds is added before silester is added, beneficial to the monodispersed SiNPs's of synthesis；And
If first adding silester adds alkali compounds, the SiNPs of synthesis is polydispersity.
It is preferred that the volume-fraction concentration of organic alcoholic solution is 50%-100%, organic alcoholic solution of the present invention
Middle solvent is water.
Organic Alcohol can improve the solubility of silester, and significantly reduce the hyperhydrated potential of water, so as to more
Critical aggregation concentration is reached in the short time；And if organic alcohol content is too low, because of compatibility difference silester can be caused to exist
Emulsion is formed in water.It is preferred that the Organic Alcohol can be relatively inexpensive, be easy to get and environmentally friendly ethanol or isopropanol.
It is preferred that the alkali compounds is potassium hydroxide or sodium hydroxide.Under gentle alkalescence condition, with potassium ion
Or sodium ion is used as counter ion, silica precursor（Silester）Nucleation can be broken out, the condition be conducive to silester with
Hydrolysis formation three-dimensional cyclic polysilicic acid chain network, these three-dimensional networks reach meeting after supersaturation in ethanol-water media
Aggregation, so as to produce nano silicon particles.
It is preferred that the alkali compounds is added in the aqueous solution of Organic Alcohol as a solution（For example with 1mol/L
Form add collocation Organic Alcohol the aqueous solution in）So that can be uniformly and rapidly in Organic Alcohol as the alkali of catalyst
Mixed in the aqueous solution, to form the silicon nano of substantial amounts of monodispersity, and if being added in the form of powder or solid
The silicon nano of polydispersity can be formed.
It is preferred that the concentration of the mixed liquor neutral and alkali compound is 5-200mmol/L, the concentration of alkali compounds is too low
Catalytic effect is not good, and with the increasing of alkali concn, gelation speed is faster, and the silicon nano size of synthesis is also bigger,
But after the concentration of alkali compounds reaches 200mmol/L concentration, reaction speed is not further added by, therefore by mixed liquor
The concentration of alkali compounds is limited in 5-200mmol/L.
It is preferred that the concentration of the silester is 5-300 mmol/L.If silester concentration is higher by this scope,
Because silester is excessive, then remaining silester is all without nano SiO 2 particle is converted into reacting, not only anti-
It will be wasted at the end of answering, and excessive silester will cause the nano particle diameter of synthesis excessive.
In the step S2, reaction is stirred at room temperature 1 ~ 120 minute, in the present invention, size of the reaction time to SiNPs
Control is greatly enhanced, and there is correlation between reaction time and SiNPs sizes, and reaction forms diameter about 60nm's after 5-20 minutes
Small size SiNPs, as the reaction time increases, it is longer that the SiNPs particle diameters of synthesis will accordingly increase the reaction time, synthesis
SiNP is bigger；But, due to fast reaction kinetics, in 70min or so, silester will be depleted, therefore, if reaction
Last much longer, then the size of nano particle will not further increase, or due to being deposited on big in smaller particle
It may increase on grain, but can also cause polydispersity.It is thus preferable to, the stirring reaction is 5 ~ 70 minutes.
After the time required to reaction, can by into liquid after reaction add 10-15 times of reaction solution volume deionized water
To stop reaction（Because silester dissolves in ethanol and water insoluble, adding substantial amounts of water makes silester formation emulsion,
From without participating in reaction）.It is of course also possible to solid-liquid separation step is directly entered, namely by centrifuging SiNP and abandoning reaction solution
To stop reaction.
It is preferred that in the step S3, separation of solid and liquid processing is carried out to liquid after reaction in eccentric fashion, separation of solid and liquid
Centrifugation rate is 6000-8000 rmp/min, and centrifugation time is 10-15min.Centrifugal rotational speed is too low, it is impossible to fully carry out solid-liquid
Separation, and it is not only tightened up to equipment requirement if centrifugal rotational speed is too big, and silicon nano can also be produced certain
Influence.
Based on the above method, present invention also offers a kind of silicon nano, it is prepared from using above-mentioned preparation method.
It is described further with reference to specific embodiment.
Embodiment 1
The aqueous isopropanol that volume fraction is 50% is configured, and adds 1mol/L sodium hydroxide thereto to concentration of potassium hydroxide
For 5mmmol/L, mixed liquor is generated；The concentration that silester to silester are added into the mixed liquor is 5mmol/L, then
Reaction 1 minute, liquid after must reacting is stirred at room temperature；Then centrifuged 10 minutes under 6000rmp/min speed, liquid after reaction is entered
The processing of row separation of solid and liquid, with the isolated solid of deionized water rinsing 3 times, finally dries, obtains silicon nano.
Embodiment 2
The ethanol solution that volume fraction is 50% is configured, and it is dense to potassium hydroxide to add 1mol/L potassium hydroxide solution thereto
Spend for 100mmmol/L, generation mixed liquor；The concentration that silester to silester are added into the mixed liquor is 5mmol/
L, then reaction 30min, liquid after must reacting is stirred at room temperature；Then 10min is centrifuged under 6000rmp/min speed, after reaction
Liquid carries out separation of solid and liquid processing, then with the isolated solid of deionized water rinsing 3 times, finally dries, obtains silicon nanoparticle
Son, the silicon nano surface of synthesis is smooth, uniform particle sizes；The silicon nano is subjected to examination of infrared spectrum, as a result such as
Shown in Fig. 2, the very strong peak value at 1088.26cm-1 is the characteristic peak that the asymmetric stretching vibrations of Si-O-Si are produced,
Further demonstrate the successful synthesis of silicon nano.
Embodiment 3
The ethanol solution that volume fraction is 50% is configured, and it is dense to potassium hydroxide to add 1mol/L potassium hydroxide solution thereto
Spend for 100mmmol/L, generation mixed liquor；Into the mixed liquor, the concentration of addition silester to silester is
100mmol/L, then reaction 45min, liquid after must reacting is stirred at room temperature；10min is centrifuged under 6000rmp/min speed, to anti-
Should after liquid carry out separation of solid and liquid processing, then with the isolated solid of deionized water rinsing 4 times, finally dry, obtain silicon and receive
Rice corpuscles, the silicon nano surface of synthesis is smooth, uniform particle sizes.
Embodiment 4
The ethanol solution that volume fraction is 75% is configured, and it is dense to potassium hydroxide to add 1mol/L potassium hydroxide solution thereto
Spend for 100mmmol/L, generation mixed liquor；Into the mixed liquor, the concentration of addition silester to silester is
300mmol/L, then reaction 60min, liquid after must reacting is stirred at room temperature；15min is centrifuged under 8000rmp/min speed, to anti-
Should after liquid carry out separation of solid and liquid processing, then with the isolated solid of deionized water rinsing 5 times, finally dry, obtain silicon and receive
Rice corpuscles, the silicon nano surface of synthesis is smooth, uniform particle sizes.
Embodiment 5
The ethanol solution that volume fraction is 50% is configured, 1mol/L sodium hydroxide is added into the ethanol solution to hydroxide
Potassium concn is 90mmmol/L, generates mixed liquor；Into the mixed liquor, the concentration of addition silester to silester is
90mmol/L, is stirred at room temperature reaction 30min, 45min and 60min respectively, obtains liquid after three kinds of reactions；Then exist respectively
10min is centrifuged under 6000rmp/min speed, separation of solid and liquid processing is carried out to liquid after reaction, then with deionized water rinsing point
3 times from obtained solid, finally dry, obtain three kinds of silicon nanos, to being obtained after described reaction 30min, 45min and 60min
To three kinds of silicon nanos carry out electron-microscope scanning experiment respectively, scanning result is as shown in Fig. 3 ~ 5, it can be seen that the silicon of synthesis
Nanoparticle surface is smooth, uniform particle sizes, and as the reaction time increases, the particle diameter of nano SiO 2 particle also constantly increases
Greatly.
In summary, the present invention is pre-configured with organic alcoholic solution, is then added into organic alcoholic solution as catalysis
The alkali of agent, adds silester, and separation of solid and liquid was to obtain that surface is smooth and uniform particle diameter after 1 ~ 120 minute by stirring reaction
Silicon nano, and by controlling the reaction time to can control the particle size of prepared silicon nano, solve existing
In technology can not Fast back-projection algorithm uniform particle diameter silicon nano the problem of.
It should be appreciated that the application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can
To be improved or converted according to the above description, all these modifications and variations should all belong to the guarantor of appended claims of the present invention
Protect scope.
Claims (10)
1. a kind of quick method for preparing silicon nano, it is characterised in that including step：
A, add alkali compounds into pre-configured organic alcoholic solution, generate mixed liquor；
B, add silester into the mixed liquor, after stirring 1-120min, liquid after being reacted；
C, separation of solid and liquid is carried out to liquid after the reaction, the solid after separation is washed, drying process, that is, obtain silicon nanometer
Particle.
2. the quick method for preparing silicon nano according to claim 1, it is characterised in that the Organic Alcohol is ethanol
Or isopropanol.
3. the quick method for preparing silicon nano according to claim 1, it is characterised in that organic alcoholic solution
Concentration is 50-100%.
4. the quick method for preparing silicon nano according to claim 1, it is characterised in that the alkali compounds is
Solid base or aqueous slkali.
5. the quick method for preparing silicon nano according to claim 1, it is characterised in that the alkali compounds is
Potassium hydroxide or sodium hydroxide.
6. the quick method for preparing silicon nano according to claim 1, it is characterised in that the mixed liquor neutral and alkali
The concentration of compound is 5-200mmol/L.
7. the quick method for preparing silicon nano according to claim 1, it is characterised in that the silester it is dense
Spend for 5-300mmol/L.
8. the quick method for preparing silicon nano according to claim 1, it is characterised in that in the step C, solid-liquid
The centrifugation rate of separation is 6000-8000 rmp/min, and centrifugation time is 10-15min.
9. the quick method for preparing silicon nano according to claim 1, it is characterised in that after the step B also
Including step：
The deionized water that liquid is accumulated after 10-15 times of addition is reacted in liquid after to reaction.
10. a kind of silicon nano, it is characterised in that be prepared from using claim 1 ~ 9 either method.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110150738A1 (en) * | 2011-02-24 | 2011-06-23 | Alireza Badiei | Formation of silica compositions using low surfactant concentrations |
| CN102602943A (en) * | 2012-03-22 | 2012-07-25 | 陕西盟创纳米新型材料股份有限公司 | Method for rapidly preparing high-performance nano silicon dioxide aerogel in one step |
| CN104003409A (en) * | 2014-06-11 | 2014-08-27 | 北京化工大学 | Method for preparing controllable monodisperse spherical large-particle-size nano-silicon dioxide |
| CN105118973A (en) * | 2015-07-20 | 2015-12-02 | 中南大学 | Preparation method of hollow nano-silicon spheres |
| CN105110343A (en) * | 2015-07-20 | 2015-12-02 | 清华大学 | Method for rapid preparation of monodisperse ordered mesoporous silicon oxide hollow sphere |
-
2017
- 2017-06-14 CN CN201710448091.9A patent/CN107311179A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110150738A1 (en) * | 2011-02-24 | 2011-06-23 | Alireza Badiei | Formation of silica compositions using low surfactant concentrations |
| CN102602943A (en) * | 2012-03-22 | 2012-07-25 | 陕西盟创纳米新型材料股份有限公司 | Method for rapidly preparing high-performance nano silicon dioxide aerogel in one step |
| CN104003409A (en) * | 2014-06-11 | 2014-08-27 | 北京化工大学 | Method for preparing controllable monodisperse spherical large-particle-size nano-silicon dioxide |
| CN105118973A (en) * | 2015-07-20 | 2015-12-02 | 中南大学 | Preparation method of hollow nano-silicon spheres |
| CN105110343A (en) * | 2015-07-20 | 2015-12-02 | 清华大学 | Method for rapid preparation of monodisperse ordered mesoporous silicon oxide hollow sphere |
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