CN105565327A - Silicon dioxide nano sol and preparation method thereof - Google Patents
Silicon dioxide nano sol and preparation method thereof Download PDFInfo
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- CN105565327A CN105565327A CN201510945192.8A CN201510945192A CN105565327A CN 105565327 A CN105565327 A CN 105565327A CN 201510945192 A CN201510945192 A CN 201510945192A CN 105565327 A CN105565327 A CN 105565327A
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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
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/145—Preparation of hydroorganosols, organosols or dispersions in an organic medium
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Abstract
The invention provides a silicon dioxide nano sol and a preparation method thereof. The silicon dioxide nano sol is generated by the steps of dissolving tetraethyl orthosilicate in ethanol, then adding ammonia water as a catalyst, stirring, then adding a fluorocarbon surfactant and a compounded surfactant, and further stirring. The silicon dioxide nano sol provided by the invention can realize surface coating permeability improvement of a hydrophobic and lipophobic inert fluorinated polymer, and the light transmittance of a polymer film after permeability improvement can meet requirements of laser target shooting. By adjusting a formula and a process of the silicon dioxide nano sol, the aim of carrying out permeability improvement on laser light of any wavelength can be achieved.
Description
Technical field
The invention belongs to the manufacture of special copolymer optical thin film and Application Areas, be specifically related to a kind of silica nanosol and preparation method thereof.
Background technology
In target practice process, sputter thing because pulse laser and target interaction can produce the very strong target of surging force, these targets sputtering thing is likely punched in diagnositc system light path, reduces cell transmittance, cause element surface to damage, bring target practice cost unprecedented soaring.U.S. Sandia laboratory adopts special polymeric film directly to keep off before optical element in Z-pinch experiment, absorbing target steam and fragment, protective effect (Proc.ofSPIE.2007,6720:67200Q-1-67200Q-10) is all had to nearly all target sputtering thing.But Sandia researchist is only studied for the laser of more than 400nm wavelength, in visible region, high saturating polymkeric substance all has at ultraviolet region and absorbs more by force the nitrocotton that they choose, polyester, polyimide these three kinds, cannot meet the service requirements of shorter wavelength laser target shooting protection from splash film.And this respect, domestic more without matured product and associated materials application.
The author finds that in early-stage Study fluoropolymer has the laser damage threshold higher than melting quartz glass, match in excellence or beauty uv transmittance (the 355nm place transmitance 93% of melting quartz glass, visible region more than 95%), there is great application potential (light laser and ionic fluid in target practice protection from splash, 2014,3:032010-1 ~ 032010-4).But this kind of film really will be applied to laser field as optical element, matter of utmost importance improves the light transmission rate of laser work wavelength, although the transmitance at 355nm place 93% has belonged to rare in the polymeric material, applied in the laser and still need to improve.
Fluorinated polymer is due to high unreactiveness and water and oil repellence characteristic, make in its plated surface anti-reflection film difficulty very large, feasible method is limited, and existing report mostly is and changes its hydrophobe or biocompatibility etc., and there is not been reported in the work carrying out anti-reflection to it.Consider sol-gel technique have simple to operate, can the multiple advantage (CeramicsInternational such as big area film, the laser damage threshold that also can improve base material, 2011,37:615-619), the invention provides and a kind ofly can be used for silica nanosol of fluorinated polymer surface coating and preparation method thereof, utilize this silica nanosol at inertia fluorinated polymer surface coating, anti-reflection object can be reached.
Summary of the invention
The technical problem that the present invention will solve is to provide a kind of silica nanosol, and another technical problem that the present invention will solve is to provide a kind of silica nanosol preparation method.
Silica nanosol of the present invention, is characterized in, described silica nanosol is composed of the following components by weight percentage:
Ammoniacal liquor 1.5% ~ 3%;
Tetraethoxy 10% ~ 19%;
Fluorocarbon surfactant 0.02% ~ 0.2%;
Compound surfactant 0 ~ 0.08%;
Ethanol 78% ~ 88%;
Above component concentration sum meets 100%.
The weight percent of described fluorocarbon surfactant is preferably 0.01% ~ 0.1%.
The weight percent of described compound surfactant is preferably 0 ~ 0.05%.
Described fluorocarbon surfactant is the one in FS-10, FS-3100, FSN or FSO-100.
Described compound surfactant is the one in sodium lauryl sulphate, polysorbate60 or tween 70.
Silica nanosol preparation method of the present invention, comprises the following steps:
A. tetraethoxy is dissolved in ethanol, in cooling bath, stirs 10min, obtain solution A;
B. ammonia solvent is stirred 10min in ethanol, obtain solution B;
C. solution B is added drop-wise in solution A, obtains solution C;
D. solution C is warming up to 60 gradually
oc, do not stop in heat-processed to stir, the time is 6h, obtains solution D;
E. by adding fluorocarbon surfactant and compound surfactant in solution D, stir, needed for obtaining.
Utilize silica nanosol of the present invention can realize the inertia fluorinated polymer surface coating of water and oil repellence anti-reflection.The concrete steps that inertia fluorinated polymer surface coating is anti-reflection are, first, optical maser wavelength as required, in conjunction with the specific refractory power of fluorinated polymer film and silicon-dioxide block materials, drawn the processing parameters such as the thickness of the silica dioxide gel layer that will obtain required for target transmitance, specific refractory power, porosity, the particle number of plies by Theoretical Calculation; Then according to the calculated results, silica nanosol is prepared according to silica nanosol preparation method of the present invention; Using plasma processing mode modification inertia fluorinated polymer surface afterwards, Cement Composite Treated by Plasma mode adopts water plasmas, and the treatment time is 30min, and temperature is normal temperature; Finally adopt lift plated film mode by silica nanosol uniform loading to the inertia fluorinated polymer surface through water plasmas process, pull rate is 100mm/min, whole process is carried out in the drying cupboard closed, after solvent nature volatile dry, obtain the fluorinated polymer film that silica dioxide gel is anti-reflection.
Silica nanosol preparation method of the present invention is simple, and production cost is low, and can realize the inertia fluorinated polymer surface coating of water and oil repellence anti-reflection, the polymeric film light transmission rate after anti-reflection can meet the requirement of laser target shooting.By regulating the composition and engineering of silica nanosol, can reach and anti-reflection object is implemented to the laser of arbitrary wavelength.The fluorinated polymer film crossed by silica nanosol Film Coating Antireflection is used as laser target shooting protection from splash film, has saved target practice cost.
Embodiment
Embodiment 1
Silica nanosol is prepared by the component concentration in table 1, concrete steps are: ethanol is divided uniformly two parts, mix with tetraethoxy and ammoniacal liquor respectively, after magnetic agitation 10min, the alcoholic solution of ammoniacal liquor is added dropwise in the alcoholic solution of tetraethoxy gradually, drips while stir (5min).Be warming up to 60 DEG C, stir 6h, stopped reaction, stand for standby use.In reaction system, add weight percent is the FS-10 fluorocarbon surfactant of 0.1% and the sodium lauryl sulphate of 0.02%, is fully uniformly mixed, obtains silica nanosol.Fluorinated polymer film is adopted water plasmas process 30min.Adopt lift plated film mode (pull rate is 100mm/min) to fluorinated polymer film surface coating with silica nanosol, coating process carries out in the drying cupboard of relative closure, film surface silicon dioxide gel layer only gravitate, ensure that silicon dioxide gel is in the load of fluorinated polymer surface uniform, namely solvent evaporates obtains silica dioxide gel antireflection layer after doing in its natural state as far as possible.After tested, the fluorinated polymer film light transmission rate that silica nanosol is anti-reflection significantly improves, and light transmission rate is increased to 94.02% by 92.98%.
Embodiment 2
Complete embodiment 2 by the operation steps in the component concentration in table 1 and embodiment 1, wherein fluorocarbon surfactant is FS-3100, and compound surfactant is sodium lauryl sulphate, and test result is in table 1.
Embodiment 3
Complete embodiment 3 by the operation steps in the component concentration in table 1 and embodiment 1, wherein fluorocarbon surfactant is FS-10, and compound surfactant is sodium lauryl sulphate, and test result is in table 1.
Embodiment 4
Complete embodiment 4 by the operation steps in the component concentration in table 1 and embodiment 1, wherein fluorocarbon surfactant is FSO-100, and compound surfactant is sodium lauryl sulphate, and test result is in table 1.
Embodiment 5
Complete embodiment 5 by the operation steps in the component concentration in table 1 and embodiment 1, wherein fluorocarbon surfactant is FS-3100, and compound surfactant is polysorbate60, and test result is in table 1.
Embodiment 6
Complete embodiment 6 by the operation steps in the component concentration in table 1 and embodiment 1, wherein fluorocarbon surfactant is FS-3100, and compound surfactant is tween 70, and test result is in table 1.
Embodiment 7
Complete embodiment 7 by the operation steps in the component concentration in table 1 and embodiment 1, wherein fluorocarbon surfactant is FS-3100, and without compound surfactant, test result is in table 1.
Comparative example 1
Complete comparative example 1 by the operation steps in the component concentration in table 1 and embodiment 1, but without fluorocarbon surfactant and compound surfactant, test result is in table 1.
Comparative example 2
Only fluorinated polymer film is adopted water plasmas process 30min, applying silicon oxide Nano sol anti-reflection film, does not directly survey transmitance, and test result is in table 1.
Each embodiment in table 1 and the transmission measurement data declaration of comparative example, significantly improve by the fluorinated polymer film transmitance of silica nanosol plated film of the present invention, wherein embodiment 1 best results.
Table 1
Claims (6)
1. a silica nanosol, is characterized in that, described silica nanosol is composed of the following components by weight percentage:
Ammoniacal liquor 1.5% ~ 3%;
Tetraethoxy 10% ~ 19%;
Fluorocarbon surfactant 0.02% ~ 0.2%;
Compound surfactant 0 ~ 0.08%;
Ethanol 78% ~ 88%;
Above component concentration sum meets 100%.
2. silica nanosol according to claim 1, is characterized in that, the weight percent of described fluorocarbon surfactant is 0.01% ~ 0.1%.
3. silica nanosol according to claim 1, is characterized in that, the weight percent of described compound surfactant is 0 ~ 0.05%.
4. silica nanosol according to claim 1, is characterized in that, described fluorocarbon surfactant is the one in FS-10, FS-3100, FSN or FSO-100.
5. silica nanosol according to claim 1, is characterized in that, described compound surfactant is the one in sodium lauryl sulphate, polysorbate60 or tween 70.
6. a silica nanosol preparation method, is characterized in that, comprises the following steps:
A. tetraethoxy is dissolved in ethanol, in cooling bath, stirs 10min, obtain solution A;
B. ammonia solvent is stirred 10min in ethanol, obtain solution B;
C. solution B is added drop-wise in solution A, obtains solution C;
D. solution C is warming up to 60 gradually
oc, do not stop in heat-processed to stir, the time is 6h, obtains solution D;
E. by adding fluorocarbon surfactant and compound surfactant in solution D, stir, needed for obtaining.
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| CN201510945192.8A CN105565327A (en) | 2015-12-17 | 2015-12-17 | Silicon dioxide nano sol and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107561605A (en) * | 2017-09-18 | 2018-01-09 | 中国工程物理研究院激光聚变研究中心 | The method and laser splash protection film of a kind of anti-reflection fluorinated polymer film |
| CN109401173A (en) * | 2018-11-05 | 2019-03-01 | 中国工程物理研究院激光聚变研究中心 | A kind of high-performance vacuum anti-reflection film and preparation method thereof |
| CN113714646A (en) * | 2021-08-31 | 2021-11-30 | 苏州金航纳米技术研究有限公司 | Method for constructing super-hydrophobic and super-oleophobic surface by laser |
| CN114214053A (en) * | 2021-11-24 | 2022-03-22 | 东南大学 | Rock core drag reducer and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1657571A (en) * | 2004-02-17 | 2005-08-24 | 吉林市吉清科技开发有限公司 | Preparation method of microspherical silica used as alkene polymerization catalyst carrier |
| US20080268362A1 (en) * | 2007-04-25 | 2008-10-30 | Shin-Etsu Chemical Co., Ltd. | Hydrophobic spherical silica microparticles having a high degree of flowability, method of producing same, electrostatic image developing toner external additive using same, and organic resin composition containing same |
| CN103204666A (en) * | 2013-04-22 | 2013-07-17 | 同济大学 | Method for preparing aerogel or aerogel-fiber composite material in aqueous condition with low cost |
| CN103435054A (en) * | 2013-06-26 | 2013-12-11 | 临安市绿源精细化学品有限公司 | Preparation method for obtaining super-hydrophilic silica sol through one-step method |
| CN103951279A (en) * | 2014-05-04 | 2014-07-30 | 江南大学 | Hydrophobic and oleophobic silica-based translucent coating film and preparation method thereof |
| CN103964448A (en) * | 2014-05-09 | 2014-08-06 | 奇瑞汽车股份有限公司 | Method for preparing monodisperse silicon dioxide nanoparticle sol for paint |
-
2015
- 2015-12-17 CN CN201510945192.8A patent/CN105565327A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1657571A (en) * | 2004-02-17 | 2005-08-24 | 吉林市吉清科技开发有限公司 | Preparation method of microspherical silica used as alkene polymerization catalyst carrier |
| US20080268362A1 (en) * | 2007-04-25 | 2008-10-30 | Shin-Etsu Chemical Co., Ltd. | Hydrophobic spherical silica microparticles having a high degree of flowability, method of producing same, electrostatic image developing toner external additive using same, and organic resin composition containing same |
| CN103204666A (en) * | 2013-04-22 | 2013-07-17 | 同济大学 | Method for preparing aerogel or aerogel-fiber composite material in aqueous condition with low cost |
| CN103435054A (en) * | 2013-06-26 | 2013-12-11 | 临安市绿源精细化学品有限公司 | Preparation method for obtaining super-hydrophilic silica sol through one-step method |
| CN103951279A (en) * | 2014-05-04 | 2014-07-30 | 江南大学 | Hydrophobic and oleophobic silica-based translucent coating film and preparation method thereof |
| CN103964448A (en) * | 2014-05-09 | 2014-08-06 | 奇瑞汽车股份有限公司 | Method for preparing monodisperse silicon dioxide nanoparticle sol for paint |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107561605A (en) * | 2017-09-18 | 2018-01-09 | 中国工程物理研究院激光聚变研究中心 | The method and laser splash protection film of a kind of anti-reflection fluorinated polymer film |
| CN109401173A (en) * | 2018-11-05 | 2019-03-01 | 中国工程物理研究院激光聚变研究中心 | A kind of high-performance vacuum anti-reflection film and preparation method thereof |
| CN113714646A (en) * | 2021-08-31 | 2021-11-30 | 苏州金航纳米技术研究有限公司 | Method for constructing super-hydrophobic and super-oleophobic surface by laser |
| CN113714646B (en) * | 2021-08-31 | 2023-03-21 | 苏州金航纳米技术研究有限公司 | Method for constructing super-hydrophobic and super-oleophobic surface by laser |
| CN114214053A (en) * | 2021-11-24 | 2022-03-22 | 东南大学 | Rock core drag reducer and preparation method thereof |
| CN114214053B (en) * | 2021-11-24 | 2023-02-28 | 东南大学 | Rock core drag reducer and preparation method thereof |
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