CN101792268A - Method for preparing metal/SiO2 composite granular film by oil-water interface self assembly method - Google Patents
Method for preparing metal/SiO2 composite granular film by oil-water interface self assembly method Download PDFInfo
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- CN101792268A CN101792268A CN200910157003A CN200910157003A CN101792268A CN 101792268 A CN101792268 A CN 101792268A CN 200910157003 A CN200910157003 A CN 200910157003A CN 200910157003 A CN200910157003 A CN 200910157003A CN 101792268 A CN101792268 A CN 101792268A
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- 238000000034 method Methods 0.000 title claims abstract description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 239000002184 metal Substances 0.000 title claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000002131 composite material Substances 0.000 title claims abstract description 8
- 238000001338 self-assembly Methods 0.000 title claims abstract description 5
- 235000012239 silicon dioxide Nutrition 0.000 title abstract description 16
- 239000000377 silicon dioxide Substances 0.000 title abstract description 6
- 229910052681 coesite Inorganic materials 0.000 title abstract 4
- 229910052906 cristobalite Inorganic materials 0.000 title abstract 4
- 229910052682 stishovite Inorganic materials 0.000 title abstract 4
- 229910052905 tridymite Inorganic materials 0.000 title abstract 4
- 239000000758 substrate Substances 0.000 claims abstract description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000084 colloidal system Substances 0.000 claims abstract description 19
- JYVHOGDBFNJNMR-UHFFFAOYSA-N hexane;hydrate Chemical compound O.CCCCCC JYVHOGDBFNJNMR-UHFFFAOYSA-N 0.000 claims abstract description 15
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 17
- 239000007864 aqueous solution Substances 0.000 claims description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 14
- 229910052710 silicon Inorganic materials 0.000 claims description 14
- 239000010703 silicon Substances 0.000 claims description 14
- 239000010453 quartz Substances 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 3
- 230000001476 alcoholic effect Effects 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 239000002105 nanoparticle Substances 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 12
- 230000003287 optical effect Effects 0.000 abstract description 6
- 238000001514 detection method Methods 0.000 abstract description 4
- 239000003814 drug Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 abstract description 2
- 239000008187 granular material Substances 0.000 abstract 1
- 238000005286 illumination Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 26
- 239000010931 gold Substances 0.000 description 23
- 239000013528 metallic particle Substances 0.000 description 10
- 238000000862 absorption spectrum Methods 0.000 description 6
- 239000011246 composite particle Substances 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Substances OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 244000197975 Solidago virgaurea Species 0.000 description 1
- 235000000914 Solidago virgaurea Nutrition 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910021505 gold(III) hydroxide Inorganic materials 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
- 229940038773 trisodium citrate Drugs 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
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Abstract
The invention discloses a method for preparing a metal/SiO2 composite granular film by an oil-water interface self assembly method, which comprises the following steps: 1) preparing metal/SiO2 colloid, and carrying out centrifugal separation on the metal/SiO2 colloid until a colloid water solution is obtained in deionized water; 2) adding n-hexane in the colloid water solution for forming an n-hexane-water two-phase mixing solution, slowing dripping ethanol into the n-hexane-water two-phase mixing solution, enriching composite granules at an n-hexane-water interface for forming a film, and still standing obtained material until the n-hexane is completely volatilized after the dripping completion; and 3) transferring the formed film on a substrate. The medicine used by the method of the invention has low price and can be obtained easily, the process is simple and controllable, and the prepared film has the similar characteristic of optical absorption characteristic to that of the monodisperse metal granular solution, and can be used in various fields such as biological detection, surface-enhanced Raman scattering, surface plasma enhanced illumination and the like.
Description
Technical field
The present invention relates to prepare metal/SiO
2The method of composite granular film belongs to the photonic material field.
Background technology
The film that metal nanoparticle and metallic particles are formed is owing to have surface plasma resonance character, and in biological detection, strengthening luminous aspect has important application.Liquid phase method can be prepared the metallic particles of different shape, size, as gold grain, golden rod, golden nucleocapsid and silver-colored square etc.Utilize that metallic particles enhanced film or dyestuff are luminous, Raman strengthens or when surveying, usually need metallic particles is deposited on the substrate.At present, there has been report the particle that liquid phase method prepares to be self-assembled into film with method such as adsorbing after the substrate surface modification.But in absorption, particle is reunited easily, causes intergranular coupling, makes to compare the bigger variation of generation in film absorption peak and the solution, absorbs peak position and is difficult for regulating.And when film was used as aspects such as strengthening luminous and detection, the absorption peak position of specific particle film was important.
Summary of the invention
The invention provides the method that a kind of preparation has the containing metal particle film of different absorption characteristics.
A kind of oil-water interface self-assembly method prepares metal/SiO
2The method of composite granular film may further comprise the steps:
1) preparation metal/SiO
2Colloid is with metal/SiO
2Centrifugal being dispersed to of colloid obtains colloid aqueous solution in the deionized water;
2) in colloid aqueous solution, add normal hexane, form normal hexane-water two-phase mixing solutions; Slowly drip ethanol in normal hexane-water two-phase mixing solutions, composite particles forms film in normal hexane-water termination enrichment; Leave standstill after dropwising to normal hexane and be evaporated completely;
3) with the film transfer that forms to substrate.
Described metal/SiO
2Metal in the colloid is the micro-nano particle with different shape of plasma resonance character, and as Au, Ag, Pt or Pd etc., the absorption spectrum of these metals is along with factors vary such as particle size, size, shapes.
Described metal/SiO
2Colloid can adopt the method preparation in having published thesis, as Au/SiO
2, Ag/SiO
2According to Langmuir 2003,19, method preparation in the 6693-6700 literary composition, Au nanometer rod/SiO
2According to Chem.Mater.2006,18, method preparation in the 2465-2467 literary composition.
The add-on of normal hexane requires the complete covering metal/SiO of normal hexane energy in described normal hexane-water two-phase mixing solutions
2The colloid aqueous solution surface.The alcoholic acid add-on is controlled film forming area size, when film covers on whole normal hexane-water termination fully, does not need to add ethanol again.
Described alcoholic acid rate of addition is per minute 0.5-2mL, and too fast rate of addition causes forming in the film more cluster of grains aggressiveness easily.
In the step 3) with substrate immersing in the solution with the angle of solution water plane 1-5 degree, after careful the lifting, the film of formation has just been transferred on the substrate.Substrate generally adopts quartz substrate or silicon substrate.
The inventive method can obtain the film of different optical absorption characteristic by regulating the kind of metallic particles.SiO
2Covering makes composite granular film keep the particulate monodispersity, has avoided the coupling between metallic particles, makes film have adjustable optical absorption character.While SiO
2Covering is convenient to carry out follow-up modification, modification etc., also plays the certain protection effect.
The film of method preparation of the present invention is by the metal/SiO of solid matter
2Composite particles constitutes, and its optical absorption characteristic changes with the metallic particles kind, and the absorption spectrum shape of film and monodispersed composite particles solution are consistent.The coated with silica layer has been avoided the optical coupled between metallic particles, and metallic particles is had provide protection.
The used medicine of the inventive method is cheap and easy to get, the process simple controllable, and the film that makes has the characteristic optical absorption characteristic similar to the single dispersion metal particle solution, can be used for biological detection, surface enhanced Raman scattering, surface plasma and strengthens aspects such as luminous.
Description of drawings
The Au/SiO that Fig. 1 (a) makes for embodiment 1
2Transmission electron microscope photo;
The Ag/SiO that Fig. 1 (b) makes for embodiment 2
2Transmission electron microscope photo;
Au nanometer rod/SiO that Fig. 1 (c) makes for embodiment 3
2Transmission electron microscope photo;
Au/SiO on the silicon substrate that Fig. 2 (a) makes for embodiment 1
2The field emission scanning electron microscope photo of particle film;
Ag/SiO on the silicon substrate that Fig. 2 (b) makes for embodiment 2
2The field emission scanning electron microscope photo of particle film;
Au nanometer rod/SiO on the silicon substrate that Fig. 2 (c) makes for embodiment 3
2The field emission scanning electron microscope photo of particle film;
Fig. 3 is embodiment 1,2,3 Au/SiO that make
2, Ag/SiO
2, Au nanometer rod/SiO
2Au/SiO on the particle aqueous solution and the quartz substrate
2, Ag/SiO
2, Au nanometer rod/SiO
2The uv-visible absorption spectra of three kinds of particle films.
Embodiment
Embodiment 1:
1) the 180mL0.7mM aqueous solution of chloraurate is heated to 100 degree, adds 10mM Trisodium Citrate 30mL reaction 15 minutes.Above-mentioned 90ml solution adds 1.5g PVP and stirred 24 hours, and is centrifugal to 90ml ethanol, adds ammoniacal liquor 15ml, water 15ml, and TEOS (10%) 1200 microlitre stirred 4 hours, and is centrifugal to 20ml water, obtains Au/SiO
2The water-sol is shown in Fig. 1 (a).In the watch-glass of 6 centimetres of diameters, add Au/SiO
2Particle colloid aqueous solution 10mL adds about 5mL normal hexane then, and mixed solution is divided into normal hexane-water two-phase, forms interface clearly, and to wherein slowly dripping ethanol 1mL, composite particles forms film in normal hexane-water termination enrichment.Leave standstill and treat that normal hexane is evaporated completely.2 square centimeters of big or small quartz substrate and silicon substrate in ethanol ultrasonic 20 minutes again with behind the deionized water rinsing, immerse in the solution with less angle, and careful lifts, and the film of formation has just been transferred on quartz substrate and the silicon substrate.Film on the silicon substrate can characterize (as Fig. 2 (a)) with SEM, and as can be seen from the figure, film is by Au/SiO
2The particle solid matter constitutes, and film is more even.On the quartz substrate absorption spectrum of particle film as shown in Figure 3, Au/SiO as seen from the figure
2The absorption lineshape of particle film and the Au particle aqueous solution are consistent, and peak position has skew to be caused by the variation of particle dielectric environment slightly.
Embodiment 2:
4gPVP adds 30mL30mMAgNO
3Ethylene glycol solution stirs, and 120 degree reaction 1h are centrifugal to ethanol, add ammoniacal liquor 15mL, water 15mL, and the 10%TEOS900 microlitre, it is centrifugal to 20ml water to stir 4h, obtains Ag/SiO
2The water-sol is shown in Fig. 1 (b).In the watch-glass of 6 centimetres of diameters, add Ag/SiO
2Particle colloid aqueous solution 10mL adds about 5mL normal hexane then, and mixed solution is divided into normal hexane-water two-phase, forms interface clearly, and to wherein slowly dripping ethanol 1mL, composite particles forms film in normal hexane-water termination enrichment.Leave standstill and treat that normal hexane is evaporated completely.2 square centimeters of big or small quartz substrate and silicon substrate in ethanol ultrasonic 20 minutes again with behind the deionized water rinsing, immerse in the solution with less angle, and careful lifts, and the film of formation has just been transferred on quartz substrate and the silicon substrate.Film on the silicon substrate can characterize (as Fig. 2 (b)) with SEM, and as can be seen from the figure, film is by Ag/SiO
2The particle solid matter constitutes, and film is more even.On the quartz substrate absorption spectrum of particle film as shown in Figure 3, Ag/SiO as seen from the figure
2The absorption lineshape of particle film and the Ag particle aqueous solution are consistent, and peak position has skew to be caused by the variation of particle dielectric environment slightly.
Embodiment 3:
The mixed aqueous solution of 35mLCTAB and 5mM hydrochloro-auric acid adds 0.1MAgNO successively
3200 microlitres, 4mL10mM vitamins C, 20 μ L10mMNaBH
4, room temperature growth 3 hours obtains golden excellent solution.Au rod solution centrifugal cleaned mix stirring 3 hours in the aqueous solution that is dispersed in 150mL0.1%PSS (molecular weight 70000) and small amount of N aCl, stirred 3 hours in the centrifugal aqueous solution that is distributed to 150mL0.1%PAH (molecular weight 56000) and small amount of N aCl, stirred 12 hours in centrifugal PVP (molecular weight 10000) aqueous solution that is distributed to 150mL2%, centrifugally add the 45mL Virahol to 10mL water, 2.5mL ammoniacal liquor and 150 μ L TEOS stirred 2 hours, centrifugal being dispersed in the water obtains Au nanometer rod/SiO
2The water-sol.Au nanometer rod/the SiO that obtains
2Transmission electron microscope photo shown in Fig. 1 c.Can see among the figure that the metallic particles micron has coated the silicon dioxide layer of one deck tens nanometer thickness, particle does not have obvious reunion.2 square centimeters of big or small quartz substrate and silicon substrate in ethanol ultrasonic 20 minutes again with behind the deionized water rinsing, immerse in the solution with less angle, and careful lifts, and the film of formation has just been transferred on quartz substrate and the silicon substrate.Film on the silicon substrate can characterize (as Fig. 2 (c)) with SEM, and as can be seen from the figure, film is by Au nanometer rod/SiO
2The particle solid matter constitutes, and film is more even.On the quartz substrate absorption spectrum of particle film as shown in Figure 3, Au nanometer rod/SiO as seen from the figure
2The absorption lineshape of particle film and the Au nanometer rod aqueous solution are consistent, and peak position has skew to be caused by the variation of particle dielectric environment slightly.
Claims (5)
1. the oil-water interface self-assembly method prepares metal/SiO
2The method of composite granular film is characterized in that may further comprise the steps:
1) preparation metal/SiO
2Colloid is with metal/SiO
2Centrifugal being dispersed to of colloid obtains colloid aqueous solution in the deionized water;
2) in colloid aqueous solution, add normal hexane, form normal hexane-water two-phase mixing solutions; In normal hexane-water two-phase mixing solutions, slowly drip ethanol, form film in normal hexane-water termination enrichment; Leave standstill after dropwising to normal hexane and be evaporated completely;
3) with the film transfer that forms to substrate.
2. the method for claim 1 is characterized in that: described metal/SiO
2Metal in the colloid is the micro-nano particle with plasma resonance character.
3. method as claimed in claim 2 is characterized in that: described metal/SiO
2Metal in the colloid is Au, Ag, Pt or Pd.
4. the method for claim 1 is characterized in that: step 2) in the alcoholic acid rate of addition be per minute 0.5-2mL.
5. the method for claim 1, it is characterized in that: described substrate is silicon substrate or quartz substrate.
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| CN200910157003A CN101792268A (en) | 2009-12-31 | 2009-12-31 | Method for preparing metal/SiO2 composite granular film by oil-water interface self assembly method |
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| CN200910157003A CN101792268A (en) | 2009-12-31 | 2009-12-31 | Method for preparing metal/SiO2 composite granular film by oil-water interface self assembly method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102928909A (en) * | 2012-10-29 | 2013-02-13 | 浙江大学 | Surface plasmon-based phase retarder |
| CN103983632A (en) * | 2014-06-09 | 2014-08-13 | 哈尔滨工业大学 | Preparation method of liquid/liquid interface self-assembled silver nanoparticle surface enhanced raman spectroscopy filter paper base |
| CN111085693A (en) * | 2019-12-31 | 2020-05-01 | 云南大学 | Synthetic AgNPs and preparation method of transplantable self-assembled film thereof |
| CN111560123A (en) * | 2020-05-14 | 2020-08-21 | 南方科技大学 | Single-layer colloid sphere film and preparation method thereof |
| CN112897575A (en) * | 2019-12-03 | 2021-06-04 | 中国科学院深圳先进技术研究院 | Method and structure for forming two-dimensional cadmium sulfide on substrate in large area |
-
2009
- 2009-12-31 CN CN200910157003A patent/CN101792268A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102928909A (en) * | 2012-10-29 | 2013-02-13 | 浙江大学 | Surface plasmon-based phase retarder |
| CN102928909B (en) * | 2012-10-29 | 2015-10-21 | 浙江大学 | A kind of phase delay device based on surface phasmon |
| CN103983632A (en) * | 2014-06-09 | 2014-08-13 | 哈尔滨工业大学 | Preparation method of liquid/liquid interface self-assembled silver nanoparticle surface enhanced raman spectroscopy filter paper base |
| CN112897575A (en) * | 2019-12-03 | 2021-06-04 | 中国科学院深圳先进技术研究院 | Method and structure for forming two-dimensional cadmium sulfide on substrate in large area |
| CN111085693A (en) * | 2019-12-31 | 2020-05-01 | 云南大学 | Synthetic AgNPs and preparation method of transplantable self-assembled film thereof |
| CN111560123A (en) * | 2020-05-14 | 2020-08-21 | 南方科技大学 | Single-layer colloid sphere film and preparation method thereof |
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Application publication date: 20100804 |