CN105858667A - Preparation method for morphology-controllable SiO2 nanometer fibers or particles - Google Patents
Preparation method for morphology-controllable SiO2 nanometer fibers or particles Download PDFInfo
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- CN105858667A CN105858667A CN201610189459.XA CN201610189459A CN105858667A CN 105858667 A CN105858667 A CN 105858667A CN 201610189459 A CN201610189459 A CN 201610189459A CN 105858667 A CN105858667 A CN 105858667A
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- sio
- nanofiber
- morphology
- preparation
- granule
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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
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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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- 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
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX 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
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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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 invention provides a preparation method for morphology-controllable SiO2 nanometer fibers or particles. The method comprises the following steps: (1) adding a proper amount of a binder solution into SiC powder with an average particle size of 1 [mu]m, carrying out mixing under stirring, and carrying out granulating; (2) placing the SiC powder mixed with the binder solution into a tablet press, carrying out axial compression under a pressure of 10 to 20 MPa for 1 to 3 min, and carrying out demolding so as to obtain a SiC green body; and (3) subjecting the SiC green body to direct laser sintering under the conditions of 0.5 to 6 kW of a laser sintering power, 120 to 600 mm/min of a scanning speed and 1 to 5 mm of a light spot diameter so as to prepare the morphology-controllable SiO2 nanometer fibers or particles. The invention has the following advantages: the prepared nanometer SiO2 has controllable morphology; process parameters of laser sintering can be adjusted according to design needs; the SiO2 nanometer fibers or particles with a specific morphology is obtained; and the adopted preparation method for the nanometer SiO2 has simple and convenient process and low cost.
Description
Technical field
The present invention relates to a kind of SiO2Nanofiber or the preparation method of granule, particularly to the SiO of a kind of morphology controllable2Nanofiber or preparation method of granules.
Background technology
Nano-meter SiO_22And SiO2Based composites is widely used in catalyst, electronic equipment, photoelectron and magnetic material.Due to nanometer size effect, Nano-meter SiO_22Micron SiO relatively2There is physically better, chemical and mechanical performance.
At present, Nano-meter SiO_22Preparation mainly use sol-gel process (Masashi F, Ayae S, Atsushi S, et al. One-dimensional
assembly of silica nanospheres mediated by block copolymer in liquid phase.
Journal of the American Chemical Society, 2009,131:16344-16345), template (Deng Wei, Chen Guo, Jia Liankun, etc. template is prepared SiO by preparation method2The impact of hollow microsphere pattern. chemistry journal, 2010,68 (19): 2000-2006), the sedimentation method (Han Jingxiang, She Lijuan, Zhai Lixin, etc. chemical precipitation method prepares nano silicon. and silicate is circulated a notice of, and 2010,29 (3): 681-685), microemulsion method (Arriagada F J, Osseo A K.Controlled hydrolysis of
tetraethoxysilane in a anon ionic water-in-oil micro-emulsion: A statistical
Model of silica nucleation.
Colloids and Surfaces, 1999,154 (3): 311-326), flame hydrolysis (Lazaro A. Nano-silica
production at low temperatures from the dissolution of olivine: synthesis,
tailoring and modeling. (PhD thesis) Eindhoven University of Technology, the
Netherlands, 2014:20-32) etc..Can be seen that, these methods belong to liquid-phase synthesis process mostly, and process is loaded down with trivial details, and the later stage processes complexity, and the Morphological control of product is relatively difficult.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, it is provided that the fiber of a kind of morphology controllable or graininess Nano-meter SiO_22Preparation method.
A kind of SiO of morphology controllable2Nanofiber or granule, it is characterised in that described SiO2Nanofiber diameter 20 ~ 50 nm, Fiber Aspect Ratio is more than 20:1, SiO2Particle diameter 50 ~ 100 nm of nano-particle.
SiO of the present invention2Nanofiber is rope form, SiO2Nano-particle is spherical.
A kind of SiO of morphology controllable2Nanofiber or the preparation method of granule, comprise the following steps:
(1) by the SiC powder of mean diameter 1 μm through being pressed into block base substrate after binding agent mixing granulation；
(2) the SiC block that step (1) obtains is carried out Direct Laser sintering, use different laser sintering process to obtain the SiO of morphology controllable2Nanofiber or granule.
In step of the present invention (2), the power of Direct Laser sintering is 0.5 ~ 6 kW, and scanning speed is 120 ~ 600 mm/min, and spot diameter is 1 ~ 5 mm.
In step of the present invention (1), described binding agent is the one in polyvinyl alcohol, polyvinyl butyral resin or Polyethylene Glycol.The mass concentration of binder solution is 5 ~ 15%, and binding agent is 1 ~ 10% with the mass ratio of SiC powder.
In step of the present invention (1), the thickness of described briquetting base substrate is 2 ~ 5 mm.
Compared with prior art, it is an advantage of the current invention that:
1, Nano-meter SiO_2 prepared by the present invention2Morphology controllable, can require to adjust laser sintering process parameter according to design, it is thus achieved that the SiO of specific morphology2Nanofiber or granule.
2, the Nano-meter SiO_2 that the present invention uses2Preparation method simple process, with low cost.
3, the Nano-meter SiO_2 of preparation2Crystallite dimension is 20-100 nm, and chemical composition is homogeneous, and purity is high.
Accompanying drawing explanation
Fig. 1 is the microscopic appearance figure of SiC used in the embodiment of the present invention 1.
Fig. 2 is the SiO in the embodiment of the present invention 12The stereoscan photograph of nano-particle.
Fig. 3 is the SiO in the embodiment of the present invention 12The stereoscan photograph of nanofiber.
Fig. 4 is the Nano-meter SiO_2 in the embodiment of the present invention 12XPS collection of illustrative plates.
Detailed description of the invention
The present invention is achieved like this, and it is characterized in that process step is:
(1) one in polyvinyl alcohol, polyvinyl butyral resin or Polyethylene Glycol being dissolved in distilled water, carry out heated at constant temperature and be allowed to be formed binder solution at 60 ~ 130 DEG C, the mass concentration of solution is 5 ~ 15%；
(2) being added by binder solution in the SiC powder that mean diameter is 1 μm and carry out mix and blend, binding agent is 1 ~ 10% with the mass ratio of SiC powder；
(3) SiC powder being mixed with binder solution is put in tablet machine in 10-20
Axial compression 1-3 under the pressure of MPa
Min, obtaining thickness after depanning is 2 ~ 5
The SiC base substrate of mm；
(4) SiC base substrate employing Direct Laser sintering is prepared Nano-meter SiO_22, laser sintered power is 0.5 ~ 6 kW, and scanning speed is 120 ~ 600 mm/min, and spot diameter is 1 ~ 5 mm.
Nano-meter SiO_2 of the present invention2For nanometer ropy filament or spherical particle, raw material SiC is micron irregular particle.
Embodiment 1
(1) polyvinyl alcohol carrying out at 90 DEG C heated at constant temperature and be allowed to be formed binder solution, the mass concentration of solution is 10%；
(2) being added by binder solution and carry out mix and blend in the SiC powder of mean diameter 1 μm, binding agent is 5% with the mass ratio of SiC powder；
(3) SiC powder being mixed with binder solution is put in tablet machine axial compression 2 min under the pressure of 20 MPa, after depanning, obtains the SiC base substrate that thickness is 2 mm；
(4) SiC base substrate using Direct Laser sintering, laser sintered power is 0.5 ~ 2
KW, scanning speed is 360
Mm/min, spot diameter is 4 mm, obtains SiO2Nanofiber or granule.In the present embodiment, use the laser sintered power of 0.5 kW, obtain the SiO that particle diameter is about 90 nm2Nano-particle；Use the laser sintered power of 2 kW, obtain the SiO of a diameter of about 50 nm2Nanofiber.
The microscopic appearance of SiC raw material used by the present embodiment is as shown in Figure 1.
SiO prepared by the present embodiment2The microscopic appearance of nano-particle is as shown in Figure 2.
SiO prepared by the present embodiment2The microscopic appearance of nanofiber is as shown in Figure 3.
Fig. 4 is the Nano-meter SiO_2 prepared by the present embodiment2XPS collection of illustrative plates.
Embodiment 2
(1) Polyethylene Glycol carrying out at 60 DEG C heated at constant temperature and be allowed to be formed binder solution, the mass concentration of solution is 8%；
(2) being added by binder solution and carry out mix and blend in the SiC powder of mean diameter 1 μm, binding agent is 10% with the mass ratio of SiC powder；
(3) SiC powder being mixed with binder solution is put in tablet machine axial compression 2 min under the pressure of 15 MPa, after depanning, obtains the SiC base substrate that thickness is 3 mm；
(4) laser scanning speed is 240 mm/min, and spot diameter is 3 mm, uses the laser sintered power of 1 kW, obtains the SiO that particle diameter is about 60 nm2Nano-particle；Use the laser sintered power of 3 kW, obtain the SiO of a diameter of about 40 nm2Nanofiber.
Embodiment 3
(1) polyvinyl alcohol carrying out at 110 DEG C heated at constant temperature and be allowed to be formed binder solution, the mass concentration of solution is 15%；
(2) being added by binder solution and carry out mix and blend in the SiC powder of mean diameter 1 μm, binding agent is 3% with the mass ratio of SiC powder；
(3) SiC powder being mixed with binder solution is put in tablet machine axial compression 2 min under the pressure of 10 MPa, after depanning, obtains the SiC base substrate that thickness is 4 mm；
(4) laser scanning speed is 480 mm/min, and spot diameter is 4 mm, uses the laser sintered power of 0.8 kW, obtains the SiO that particle diameter is about 80 nm2Nano-particle；Use the laser sintered power of 6 kW, obtain the SiO that width is about 200 nm2Block is brilliant.
Claims (6)
1. the SiO of a morphology controllable2Nanofiber or granule, it is characterised in that described SiO2Nanofiber diameter 20 ~ 50 nm, Fiber Aspect Ratio is more than 20:1, SiO2Particle diameter 50 ~ 100 nm of nano-particle.
SiO the most according to claim 12Nanofiber or granule, it is characterised in that described SiO2Nanofiber is rope form, SiO2Nano-particle is spherical.
3. the SiO of a morphology controllable as claimed in claim 1 or 22Nanofiber or the preparation method of granule, comprise the following steps:
(1) by the SiC powder of mean diameter 1 μm through being pressed into block base substrate after binding agent mixing granulation；
(2) the SiC block that step (1) obtains is carried out Direct Laser sintering, use different laser sintering process to obtain the SiO of morphology controllable2Nanofiber or granule.
The SiO of a kind of morphology controllable the most according to claim 32Nanofiber or the preparation method of granule, it is characterised in that in described step (2), the power of Direct Laser sintering is 0.5 ~ 6 kW, and scanning speed is 120 ~ 600 mm/min, and spot diameter is 1 ~ 5 mm.
5. according to the SiO of morphology controllable a kind of described in claim 32Nanofiber or the preparation method of granule, it is characterised in that in described step (1), described binding agent is the one in polyvinyl alcohol, polyvinyl butyral resin or Polyethylene Glycol；The mass concentration of binder solution is 5 ~ 15%, and binding agent is 1 ~ 10% with the mass ratio of SiC powder.
6. according to the SiO of morphology controllable a kind of described in claim 32Nanofiber or the preparation method of granule, it is characterised in that in described step (1), the thickness of described briquetting base substrate is 2 ~ 5 mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610189459.XA CN105858667A (en) | 2016-03-30 | 2016-03-30 | Preparation method for morphology-controllable SiO2 nanometer fibers or particles |
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| CN201610189459.XA CN105858667A (en) | 2016-03-30 | 2016-03-30 | Preparation method for morphology-controllable SiO2 nanometer fibers or particles |
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| CN201610189459.XA Pending CN105858667A (en) | 2016-03-30 | 2016-03-30 | Preparation method for morphology-controllable SiO2 nanometer fibers or particles |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109437912A (en) * | 2018-12-05 | 2019-03-08 | 南昌航空大学 | A kind of preparation method of the silica in situ cladding silicon carbide nuclear-shell structured nano-composite material of morphology controllable |
Citations (6)
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|---|---|---|---|---|
| CN1861522A (en) * | 2005-05-13 | 2006-11-15 | 中国科学院合肥物质科学研究院 | Silicon oxide nano rope with reversible luminous feature and preparation process thereof |
| CN101279736A (en) * | 2007-04-04 | 2008-10-08 | 同济大学 | Preparation and application of silica white nano-wire |
| CN101798089A (en) * | 2010-01-21 | 2010-08-11 | 复旦大学 | Silicon oxide nanowire growing by catalysis of germanium and preparation method thereof |
| CN102099292A (en) * | 2008-08-22 | 2011-06-15 | 国立大学法人东京大学 | Silica nanoparticle structure and process for production of same |
| CN103896282A (en) * | 2012-12-25 | 2014-07-02 | 北京有色金属研究总院 | Method used for preparing silicon oxide nanowires via green compact of silicon carbide powder |
| CN104773737A (en) * | 2015-03-20 | 2015-07-15 | 天水佳吉化工有限公司 | Production method for fine spherical silicon powder |
-
2016
- 2016-03-30 CN CN201610189459.XA patent/CN105858667A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1861522A (en) * | 2005-05-13 | 2006-11-15 | 中国科学院合肥物质科学研究院 | Silicon oxide nano rope with reversible luminous feature and preparation process thereof |
| CN101279736A (en) * | 2007-04-04 | 2008-10-08 | 同济大学 | Preparation and application of silica white nano-wire |
| CN102099292A (en) * | 2008-08-22 | 2011-06-15 | 国立大学法人东京大学 | Silica nanoparticle structure and process for production of same |
| CN101798089A (en) * | 2010-01-21 | 2010-08-11 | 复旦大学 | Silicon oxide nanowire growing by catalysis of germanium and preparation method thereof |
| CN103896282A (en) * | 2012-12-25 | 2014-07-02 | 北京有色金属研究总院 | Method used for preparing silicon oxide nanowires via green compact of silicon carbide powder |
| CN104773737A (en) * | 2015-03-20 | 2015-07-15 | 天水佳吉化工有限公司 | Production method for fine spherical silicon powder |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109437912A (en) * | 2018-12-05 | 2019-03-08 | 南昌航空大学 | A kind of preparation method of the silica in situ cladding silicon carbide nuclear-shell structured nano-composite material of morphology controllable |
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