CN102432187A - Method for preparing metal nano-particle thin films in various shapes on conductive glass - Google Patents
Method for preparing metal nano-particle thin films in various shapes on conductive glass Download PDFInfo
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- CN102432187A CN102432187A CN2011102293906A CN201110229390A CN102432187A CN 102432187 A CN102432187 A CN 102432187A CN 2011102293906 A CN2011102293906 A CN 2011102293906A CN 201110229390 A CN201110229390 A CN 201110229390A CN 102432187 A CN102432187 A CN 102432187A
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Abstract
The invention discloses a method for preparing metal nano-particle thin films in various shapes on conductive glass, which comprises the steps of: adding gold and silver nano-particles in different shapes, further coating the nano-particles in different shapes on ITO conductive glass, treating the surface of the ITO conductive glass and changing the electrifying characteristics on the surface of the ITO conductive glass in the process of coating the surface of Indium-Tin Oxide-ITO conductive glass. When different charges are electrified on the surface of the ITO conductive glass, the nano-particles in different shapes will be absorbed on the surface of treated ITO conductive glass so as to change the optical properties of the ITO conductive glass so that the ITO conductive glass is featured by optical properties of nano-particles in different shapes at the same time. The method provided by the invention controls the thickness of the nano-particle thin film by increasing the number of times of treatment.
Description
Technical field
The present invention relates to the preparation method of nanometer particle film.
Background technology
The nano-noble metal particle is because its special optical characteristics; Be surface plasma body resonant vibration (Surface Plasmon Resonance; SPR), and excellent biological compatibility, demonstrate the huge applications prospect in fields such as Photobiology sensing, medical diagnosis, clinical treatments.The ball shaped nano gold grain has a SPR absorption peak, is positioned at about 520nm, and the rod-like nano gold grain has major axis and two geometric parameters of short-axis direction, and its absorption spectrum has two SPR absorption peaks, and wherein the major axis peak is with when the environment variations in refractive index is very responsive in length and breadth.The trilateral nano-Ag particles has three SPR absorption peaks, and wherein when the environment variations in refractive index is very responsive with length of side thickness at face interior dipole resonance peak.Resonance photoabsorption and electric field enhanced characteristic that these local dielectric environments rely on make the nano-noble metal particle of different-shape at bio-sensing and area of medical diagnostics very big development prospect arranged.
In recent years; The size of electronics and biochip is more and more littler; And detection sensitivity is increasingly high, and the nano particle of colloidal state is owing to be difficult to device, and can't satisfy the needs that carry out bio-sensing and medical diagnosis easily and efficiently; So study the nano-grain array of solid film state, become the inexorable trend in bio-sensing field.
At present, the method for preparing nanometer particle film is many, all is based on plane and spatial and piles up the wood block type assembling; Approach mainly is to electroplate methods such as chemistry; The substrate that uses is also inequality, and metal, glass, plastics etc. are arranged.
By contrast, use transparent glass substrate, utilize chemical process to carry out electric charge absorption, successively assemble, have that the preparation process is simple, processing ease, easy to use, optical characteristics keep good characteristics.This method is through glass substrate being handled, changed the charged characteristic of glass substrate, make that the charged characteristic of this glass substrate and nano particle are opposite, then metal nanoparticle being fixed on the glass substrate through the mode that electric charge attracts mutually.The glass substrate that often uses at present mainly contains golden film glass and tin indium oxide film glass (ITO).
Because the charged characteristic and the optical characteristics of different nano particles are inequality, so become nano thin-film to have great importance different-shape, different types of preparation of nanoparticles.And present existent method just prepares the spherical nanometer gold or the rod-like nano gold grain of single shape usually.The present invention is using transparent glass substrate; Utilize chemical process to carry out electric charge absorption; On the basis of successively assembling, through changing assembling material and chemical process, successful is assembled on the same substrate with the rod-like nano gold grain spherical; Be prepared into mixed film, also can be used for the preparation of Yin Nami triangle particle film.
Summary of the invention
The object of the present invention is to provide a kind of on the ITO conductive glass method of the multiple pattern noble metal nano particles film of preparation, through changing ITO conductive glass surface charged characteristic, the gold and silver preparation of nanoparticles of different-shape is become nanometer particle film; The nanometer particle film that makes has kept the optical property of good nano particle.
Technical scheme of the present invention is achieved in that
(1) step of preparation nanometer gold (spherical or bar-shaped) film
A) in the ultrasonic cleaning machine, use suds and ultrapure water to clean respectively 10-20 minute the ITO conductive glass.
B) ito glass was immersed in the mixed aqueous solution of 5-20mM linear polyethyleneimine (LPEI) and 0.1-0.5M NaCl 1-3 hour.
C) ito glass was immersed in the mixed aqueous solution of 5-20mM Poly sodium styrene sulfonate (PSS) and 0.1-0.5M NaCl 1-3 hour.
D) after the ito glass handled cleans through ultrapure water, immersed in nanometer gold (the spherical or bar-shaped) colloidal solution 10-15 hour.
E) ito glass that will go up in the step immersed PSS solution 10-30 minute, and then immersed nanometer gold (spherical/bar-shaped) colloidal solution 30-60 minute.
F) repeating step e), up to obtaining satisfied coating effect.
(2) preparation contains spherical and the step rod-like nano gold thin film simultaneously
A) in the ultrasonic cleaning machine, use suds and ultrapure water to clean respectively 10-20 minute the ITO conductive glass.
B) ito glass was immersed in the mixed aqueous solution of 5-20mM LPEI and 0.1-0.5M NaCl 1-3 hour.
C) ito glass was immersed in the mixed aqueous solution of 5-20mM PSS and 0.1-0.5M NaCl 1-3 hour.
D) after the ito glass handled cleaned through ultrapure water, an end immersed in the spherical nanometer gold colloidal solution 10-15 hour.
E) go up in the mixed aqueous solution that ito glass in the step immerses 5-20mM PSS and 0.1-0.5M NaCl once more 1-3 hour.
F) after the ito glass handled cleaned through ultrapure water, the other end immersed in the rod-like nano gold colloid solution 10-15 hour.
G) ito glass that will go up in the step immersed PSS solution 10-30 minute, and then bulbous end was immersed spherical nanometer gold colloidal solution 30-60 minute.
H) ito glass that will go up in the step immersed PSS solution 10-30 minute, and then bar-shaped end was immersed the rod-like nano gold colloid solution 30-60 minute.
I) repeating step g), h), up to obtaining satisfied coating effect.
(3) step of the silver-colored trilateral nanometer particle film of preparation
A) in the ultrasonic cleaning machine, use suds and ultrapure water to clean respectively 10-20 minute the ITO conductive glass.
B) ito glass was immersed in the mixed aqueous solution of 5-20mM LPEI and 0.1-0.5M NaCl 1-3 hour.
C) after the ito glass handled cleans through ultrapure water, immersed in the nanometer silver triangle pearl glue liquid solution 10-15 hour.
D) ito glass that will go up in the step immersed LPEI solution 10-30 minute, was immersing nanometer silver triangle pearl glue liquid solution 30-60 minute then.
E) repeating step d), up to obtaining satisfied coating effect.
The key problem in technology that the present invention solves is that the gold and silver noble metal nano particles with different-shape is prepared into single and mixes nanometer particle film, and has kept the optical characteristics of good nano particle.
Effect of the present invention is embodied in:
(1) the present invention proposes the method that on the ITO conductive glass, prepares multiple pattern noble metal nano particles film, the preparation process is simple, quick, and equipment requirements is low, is easy to scale operation.
(2) adopt the prepared multiple pattern noble metal nano particles film of the present invention's technology, good maintenance the optical property of nano particle.
(3) the prepared multiple pattern nanometer particle film of the present invention can directly be used for sensing chip preparation and spectral detection.
Embodiment
Embodiment one:
In the ultrasonic cleaning machine, use suds and ultrapure water to clean respectively 15 minutes the ITO conductive glass.Ito glass was immersed in the mixed aqueous solution of 10mM LPEI and 0.2M NaCl 2 hours.Ito glass was immersed in the mixed aqueous solution of 10mM PSS and 0.2M NaCl 2 hours.After the ito glass handled cleaned through ultrapure water, an end immersed in the spherical nanometer gold colloidal solution 12 hours.Ito glass in last step immersed in the mixed aqueous solution of 10mM PSS and 0.2M NaCl 2 hours once more.After the ito glass handled cleaned through ultrapure water, the other end immersed in the rod-like nano gold colloid solution 12 hours.Ito glass in the last step was immersed PSS solution 20 minutes, and then bulbous end was immersed spherical nanometer gold colloidal solution 40 minutes.Ito glass in the last step was immersed PSS solution 20 minutes, and then bar-shaped end was immersed the rod-like nano gold colloid solution 40 minutes.Repeat two steps in front, up to obtaining satisfied coating effect.The nano thin-film for preparing contains spherical and the rod-like nano gold grain simultaneously, and the absorption spectrum test result shows that nano thin-film has the optical characteristics of good spherical and rod-like nano gold grain simultaneously.
Embodiment two:
In the ultrasonic cleaning machine, use suds and ultrapure water to clean respectively 20 minutes the ITO conductive glass.Ito glass was immersed in the mixed aqueous solution of 10mM LPEI and 0.1M NaCl 3 hours.After the ito glass handled cleans through ultrapure water, immersed in the trilateral nano-class silver colloidal solution 15 hours.Ito glass in the last step is immersed LPEI solution 10 minutes, and then immersed the trilateral nano-class silver colloidal solution 40 minutes.Repeat a step, up to obtaining satisfied coating effect.The nano thin-film for preparing contains the trilateral nano-Ag particles, and the absorption spectrum test result shows that nano thin-film has the optical property of good trilateral nano-Ag particles.
Embodiment three:
In the ultrasonic cleaning machine, use suds and ultrapure water to clean respectively 15 minutes the ITO conductive glass.Ito glass was immersed in the mixed aqueous solution of 10mM LPEI and 0.1M NaCl 2 hours.Ito glass was immersed in the mixed aqueous solution of 10mM PSS and 0.1MNaCl 1.5 hours.After the ito glass of handling cleans through ultrapure water; Immersed the golden mixed colloidal solution of spherical nanometer gold and rod-like nano 12 hours; Ito glass in the top was immersed in the PSS solution 20 minutes, after ultrapure water cleans, immersed the golden mixed colloidal solution of spherical nanometer gold and rod-like nano again 40 minutes.Repeat a step, know to obtain satisfied coating effect.The nano thin-film for preparing contains simultaneously and has spherical nm gold particles and rod-like nano gold grain, and the absorption spectrum test result shows that nano thin-film has the optical property of good admixture ball shaped nano gold grain and rod-like nano gold grain.
Claims (1)
- One kind on conductive glass the preparation multiple pattern film of metal nano-particles method, it is characterized in that this method comprises following classification:(1) step of the spherical or bar-shaped film of preparation nanometer goldA) in the ultrasonic cleaning machine, use suds and ultrapure water to clean respectively 10-20 minute tin indium oxide Indium-Tin Oxide-ITO conductive glass;B) ito glass was immersed in the mixed aqueous solution of 5-20Mm polymine linear polyethyleneimine-LPEI and 0.1-0.5M NaCl 1-3 hour;C) ito glass was immersed in the mixed aqueous solution of 5-20mM SSS Poly sodium styrene sulfonate-PSS and 0.1-0.5M NaCl 1-3 hour;D) after the ito glass handled cleans through ultrapure water, immersed in the spherical or bar-shaped colloidal solution of nanometer gold 10-15 hour;E) ito glass that will go up in the step immersed PSS solution 10-30 minute, and then immerse nanometer gold spherical/bar-shaped colloidal solution 30-60 minute;F) repeating step e), up to obtaining to apply effect;(2) preparation contains spherical and the step rod-like nano gold thin film simultaneouslyA) in the ultrasonic cleaning machine, use suds and ultrapure water to clean respectively 10-20 minute the ITO conductive glass;B) ito glass was immersed in the mixed aqueous solution of 5-20mM LPEI and 0.1-0.5M NaCl 1-3 hour;C) ito glass was immersed in the mixed aqueous solution of 5-20mM PSS and 0.1-0.5M NaCl 1-3 hour;D) after the ito glass handled cleaned through ultrapure water, an end immersed in the spherical nanometer gold colloidal solution 10-15 hour;E) go up in the mixed aqueous solution that ito glass in the step immerses 5-20mM PSS and 0.1-0.5M NaCl once more 1-3 hour;F) after the ito glass handled cleaned through ultrapure water, the other end immersed in the rod-like nano gold colloid solution 10-15 hour;G) ito glass that will go up in the step immersed PSS solution 10-30 minute, and then bulbous end was immersed spherical nanometer gold colloidal solution 30-60 minute;H) ito glass that will go up in the step immersed PSS solution 10-30 minute, and then bar-shaped end was immersed the rod-like nano gold colloid solution 30-60 minute;I) repeating step g), h), up to obtaining satisfied coating effect;(3) step of the silver-colored trilateral nanometer particle film of preparationA) in the ultrasonic cleaning machine, use suds and ultrapure water to clean respectively 10-20 minute the ITO conductive glass;B) ito glass was immersed in the mixed aqueous solution of 5-20mM LPEI and 0.1-0.5M NaCl 1-3 hour;C) after the ito glass handled cleans through ultrapure water, immersed in the nanometer silver triangle pearl glue liquid solution 10-15 hour;D) ito glass that will go up in the step immersed LPEI solution 10-30 minute, was immersing nanometer silver triangle pearl glue liquid solution 30-60 minute then;E) repeating step d), up to obtaining to apply effect.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105215364A (en) * | 2015-09-28 | 2016-01-06 | 东南大学 | Based on the micro-fluidic 3D SERS substrate fabrication method of silver nanoparticle star self assembly |
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| CN1356543A (en) * | 2001-12-10 | 2002-07-03 | 中国科学院长春应用化学研究所 | Process for preparing film electrode of gold-monocrystal nano island array |
| US6416818B1 (en) * | 1998-08-17 | 2002-07-09 | Nanophase Technologies Corporation | Compositions for forming transparent conductive nanoparticle coatings and process of preparation therefor |
| CN101817645A (en) * | 2010-03-12 | 2010-09-01 | 浙江大学 | Method for construction of physical patterns on polyelectrolyte multilayer film |
| CN102051680A (en) * | 2011-01-21 | 2011-05-11 | 西安交通大学 | Rapid preparation method of gold nano rod with small aspect ratio |
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2011
- 2011-08-11 CN CN2011102293906A patent/CN102432187A/en active Pending
Patent Citations (4)
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|---|---|---|---|---|
| US6416818B1 (en) * | 1998-08-17 | 2002-07-09 | Nanophase Technologies Corporation | Compositions for forming transparent conductive nanoparticle coatings and process of preparation therefor |
| CN1356543A (en) * | 2001-12-10 | 2002-07-03 | 中国科学院长春应用化学研究所 | Process for preparing film electrode of gold-monocrystal nano island array |
| CN101817645A (en) * | 2010-03-12 | 2010-09-01 | 浙江大学 | Method for construction of physical patterns on polyelectrolyte multilayer film |
| CN102051680A (en) * | 2011-01-21 | 2011-05-11 | 西安交通大学 | Rapid preparation method of gold nano rod with small aspect ratio |
Non-Patent Citations (2)
| Title |
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| 刘秀: "《ITO电极表面二维有序微米球腔阵列的构筑及其电化学研究》", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》, no. 1, 15 January 2011 (2011-01-15), pages 52 - 54 * |
| 周静: "《三角形纳米银颗粒的制备及其热稳定性的研究》", 《分子科学学报》, vol. 25, no. 6, 31 December 2009 (2009-12-31), pages 436 - 438 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105215364A (en) * | 2015-09-28 | 2016-01-06 | 东南大学 | Based on the micro-fluidic 3D SERS substrate fabrication method of silver nanoparticle star self assembly |
| CN105215364B (en) * | 2015-09-28 | 2018-11-06 | 东南大学 | Micro-fluidic 3D SERS substrate fabrication methods based on silver nanoparticle star self assembly |
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Application publication date: 20120502 |