CN101695756B - A method for preparing gold-silver alloy nanoparticles in polyelectrolyte multilayer film - Google Patents
A method for preparing gold-silver alloy nanoparticles in polyelectrolyte multilayer film Download PDFInfo
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- CN101695756B CN101695756B CN2009102177931A CN200910217793A CN101695756B CN 101695756 B CN101695756 B CN 101695756B CN 2009102177931 A CN2009102177931 A CN 2009102177931A CN 200910217793 A CN200910217793 A CN 200910217793A CN 101695756 B CN101695756 B CN 101695756B
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Abstract
本发明涉及一种在聚电解质多层膜中制备金银合金纳米粒子的方法。首先通过层接层自组装得到含支化的聚乙烯亚胺或线性的聚乙烯亚胺，和聚丙烯酸或聚甲基丙烯酸的多层膜，依次浸泡在氯金酸和硝酸银的水溶液中，然后把吸附有金和银离子的多层膜置于烘箱中加热还原，即得到金银合金纳米粒子。该方法操作简便，可用于在多层膜中直接制备含不同金银比例的合金纳米粒子。所获得的合金纳米粒子具有特征的表面等离子体共振吸收信号，在催化、光学等领域具有极高的应用价值。The invention relates to a method for preparing gold-silver alloy nanoparticles in a polyelectrolyte multilayer film. First, a multilayer film containing branched polyethyleneimine or linear polyethyleneimine, and polyacrylic acid or polymethacrylic acid is obtained by layer-by-layer self-assembly. Then place the multi-layer film with the gold and silver ions adsorbed therein in an oven for heating and reduction to obtain gold-silver alloy nanoparticles. The method is easy to operate and can be used to directly prepare alloy nanoparticles containing different gold-silver ratios in multilayer films. The obtained alloy nanoparticles have characteristic surface plasmon resonance absorption signals, and have extremely high application value in the fields of catalysis and optics.
Description
Technical field
The present invention relates to a kind of method that in polyelectrolyte multilayer film, prepares gold-silver alloy nanoparticles.
Background technology
The bimetal nano material all has potential using value in a lot of fields because of physics, the chemical property that has two kinds of metal components simultaneously, such as catalysis, optical detection, immunoassay, information storage etc.The gold and silver nano particle is owing to optics, the electronics character of the uniqueness that it produced have important basic research and actual application value, for example can be as the base material of tunable surface enhanced Raman scattering effect, or as surface plasma resonance sensor etc.The Dor nano material comprises gold and silver nucleocapsid structure and electrum structure, and is wherein less relatively about the research of gold-silver alloy nanoparticles.At present, the synthetic of gold-silver alloy nanoparticles mainly concentrates on the various methods that prepare nano particle of development in the liquid phase, and these alloy nano particles all need to be fixed to (B.H.Ong in substrate or the film phase material in actual applications, et al, Fiber Integr.Opt.2007,26,229; X.Liu, et al, Chem.Mater.2009,21,410).Of the present invention in polyelectrolyte multilayer film the method for in situ preparation gold-silver alloy nanoparticles do not appear in the newspapers as yet.
Summary of the invention
The purpose of this invention is to provide a kind of method that in polyelectrolyte multilayer film, prepares gold-silver alloy nanoparticles.
Described preparation method may further comprise the steps:
1) be that 7: 3 mass percent is after 98% sulfuric acid and mass percent are to soak 30 fens kinds in the mixed solution of 30% hydrogen peroxide, with pure water this sheet glass to be rinsed well with sheet glass in volume ratio;
2) sheet glass that step 1) was handled is 5.0-9.0 at pH, and concentration is to soak 10 minutes in the aqueous solution of the polymine of branching of 5mg/ml or linear polymine, and is clean with pure water rinsing;
3) then, with step 2) to be soaked in pH be 3.0-7.0 for the sheet glass handled, and concentration is the polyacrylic acid of 5mg/ml or polymethyl acid solution 10 minutes, and water is rinsed well again;
4) repeating step 2) and step 3), polyelectrolyte multilayer film obtained;
5) polyelectrolyte multilayer film that step 4) is obtained is 2.0-3.0 at pH, and concentration is to soak 15 minutes in the aqueous solution of gold chloride of 5mM, and is clean with pure water rinsing; In the aqueous solution of 10mM silver nitrate, soaked 1-10 minute then, clean with pure water rinsing; This multilayer film that will obtain at last places baking oven, heats 1 hour down at 200 ℃, obtains gold-silver alloy nanoparticles.
Beneficial effect: characteristics of the present invention are directly to connect a layer self assembly polyelectrolyte multilayer film by the electrostatic interaction layer on base material, adsorb gold chloride anion and silver ion successively after, prepare gold-silver alloy nanoparticles by adding thermal reduction.Whole process of preparation is easy and simple to handle, directly obtains nano particle in multilayer film, and particle diameter is 3.8 ± 0.8nm.This method can be used for preparing the preparation of the alloy that contains different gold and silver ratios.The gold-silver alloy nanoparticles that is obtained has the surface plasma body resonant vibration absorption signal of feature, has high using value in fields such as catalysis, optics.
Description of drawings
Fig. 1 is that particle diameter is that 3.8 ± 0.8nm, gold and silver atomic molar ratio are the transmission electron microscope picture of 2: 3 gold-silver alloy nanoparticles.
Fig. 2 is the ultraviolet-visible absorption spectroscopy figure of gold-silver alloy nanoparticles, and the gold, silver atomic molar ratio of absorption curve 1 to 3 expression gold-silver alloy nanoparticles wherein was followed successively by 17: 3,11: 9,2: 3.
The specific embodiment
Embodiment 1:
1) be that 7: 3 mass percent is after 98% sulfuric acid and mass percent are to soak 30 fens kinds in the mixed solution of 30% hydrogen peroxide, with pure water this sheet glass to be rinsed well with sheet glass in volume ratio;
2) sheet glass that step 1) was handled is 7.0 at pH, and concentration is to soak 10 minutes in the aqueous solution of polymine of branching of 5mg/ml, and is clean with pure water rinsing;
3) then, with step 2) to be soaked in pH be 3.5 to sheet glass, concentration is the polyacrylic acid solution 10 minutes of 5mg/ml, and is clean with pure water rinsing again;
4) repeating step 2) and step 3) be 7 polyelectrolyte multilayer film to the double-deck number that obtains polyelectrolyte;
5) the double-deck number that step 4) is obtained is that 7 polyelectrolyte multilayer film is 2.0 at pH, and concentration is to soak 15 minutes in the aqueous solution of gold chloride of 5mM, and is clean with pure water rinsing; Be to soak 10 minutes in the aqueous solution of 10mM silver nitrate in concentration then, clean with pure water rinsing; At last, this multilayer film that obtains is placed baking oven, heated 1 hour down, promptly obtain gold-silver alloy nanoparticles at 200 ℃.Can clearly see the existence of product nano particle from Fig. 1.
Embodiment 2:
1) be that 7: 3 mass percent is after 98% sulfuric acid and mass percent are to soak 30 fens kinds in the mixed solution of 30% hydrogen peroxide, with pure water this sheet glass to be rinsed well with sheet glass in volume ratio;
2) sheet glass that step 1) was handled is 9.0 at pH, and concentration is to soak 10 minutes in the aqueous solution of polymine of branching of 5mg/ml, and is clean with pure water rinsing;
3) then sheet glass being soaked in pH is 3.0, and concentration is the polyacrylic acid solution 10 minutes of 5mg/ml, and is clean with pure water rinsing again;
4) repeating step 2) and step 3) be 7 polyelectrolyte multilayer film to the double-deck number that obtains polyelectrolyte;
5) the double-deck number that step 4) is obtained is that 7 polyelectrolyte multilayer film is 2.5 at pH, and concentration is to soak 15 minutes in the aqueous solution of gold chloride of 5mM, and is clean with pure water rinsing; Be to soak 10 minutes in the aqueous solution of 10mM silver nitrate in concentration then, clean with pure water rinsing; This multilayer film that will obtain at last places baking oven, heats 1 hour down at 200 ℃, promptly obtains gold-silver alloy nanoparticles.
Embodiment 3:
1) be that 7: 3 mass percent is after 98% sulfuric acid and mass percent are to soak 30 fens kinds in the mixed solution of 30% hydrogen peroxide, with pure water this sheet glass to be rinsed well with sheet glass in volume ratio;
2) sheet glass that step 1) was handled is 5.0 at pH, and concentration is to soak 10 minutes in the aqueous solution of polymine of branching of 5mg/ml, and is clean with pure water rinsing;
3) then sheet glass being soaked in pH is 7.0, and concentration is the polyacrylic acid solution 10 minutes of 5mg/ml, and is clean with pure water rinsing again;
4) repeating step 2) and step 3) be 5 polyelectrolyte multilayer film to the double-deck number that obtains polyelectrolyte;
5) the double-deck number that step 4) is obtained is that 5 polyelectrolyte multilayer film is 3.0 at pH, and concentration is to soak 15 minutes in the aqueous solution of gold chloride of 5mM, and is clean with pure water rinsing; Be to soak 10 minutes in the aqueous solution of 10mM silver nitrate in concentration then, clean with pure water rinsing; This multilayer film that will obtain at last places baking oven, heats 1 hour down at 200 ℃, promptly obtains gold-silver alloy nanoparticles.
Embodiment 4:
1) be that 7: 3 mass percent is after 98% sulfuric acid and mass percent are to soak 30 fens kinds in the mixed solution of 30% hydrogen peroxide, with pure water this sheet glass to be rinsed well with sheet glass in volume ratio;
2) sheet glass that step 1) was handled is 7.0 at pH, and concentration is to soak 10 minutes in the aqueous solution of polymine of branching of 5mg/ml, and is clean with pure water rinsing;
3) then sheet glass being soaked in pH is 3.5, and concentration is the polyacrylic acid solution 10 minutes of 5mg/ml, and is clean with pure water rinsing again;
4) repeating step 2) and step 3) be 7 polyelectrolyte multilayer film to the double-deck number that obtains polyelectrolyte;
5) the double-deck number that step 4) is obtained is that 7 polyelectrolyte multilayer film is 2.0 at pH, and concentration is to soak 15 minutes in the aqueous solution of gold chloride of 5mM, and is clean with pure water rinsing; Be to soak 5 minutes in the aqueous solution of 10mM silver nitrate in concentration then, clean with pure water rinsing; This multilayer film that will obtain at last places baking oven, heats 1 hour down at 200 ℃, promptly obtains gold-silver alloy nanoparticles.
Embodiment 5:
1) be that 7: 3 mass percent is after 98% sulfuric acid and mass percent are to soak 30 fens kinds in the mixed solution of 30% hydrogen peroxide, with pure water this sheet glass to be rinsed well with sheet glass in volume ratio;
2) sheet glass that step 1) was handled is 7.0 at pH, and concentration is to soak 10 minutes in the aqueous solution of polymine of branching of 5mg/ml, and is clean with pure water rinsing;
3) then sheet glass being soaked in pH is 3.5, and concentration is the polyacrylic acid solution 10 minutes of 5mg/ml, and is clean with pure water rinsing again;
4) repeating step 2) and step 3) be 7 polyelectrolyte multilayer film to the double-deck number that obtains polyelectrolyte;
5) the double-deck number that step 4) is obtained is that 7 polyelectrolyte multilayer film is 2.0 at pH, and concentration is to soak 15 minutes in the aqueous solution of gold chloride of 5mM, and is clean with pure water rinsing; Be to soak 1 minute in the aqueous solution of 10mM silver nitrate in concentration then, clean with pure water rinsing; This multilayer film that will obtain at last places baking oven, heats 1 hour down at 200 ℃, promptly obtains gold-silver alloy nanoparticles.
Embodiment 6:
1) be that 7: 3 mass percent is after 98% sulfuric acid and mass percent are to soak 30 fens kinds in the mixed solution of 30% hydrogen peroxide, with pure water this sheet glass to be rinsed well with sheet glass in volume ratio;
2) sheet glass that step 1) was handled is 7.0 at pH, and concentration is to soak 10 minutes in the aqueous solution of polymine of linearity of 5mg/ml, and is clean with pure water rinsing;
3) then sheet glass being soaked in pH is 3.5, and concentration is the polyacrylic acid solution 10 minutes of 5mg/ml, and is clean with pure water rinsing again;
4) repeating step 2) and step 3) be 7 polyelectrolyte multilayer film to the double-deck number that obtains polyelectrolyte;
5) the double-deck number that step 4) is obtained is that 7 polyelectrolyte multilayer film is 2.0 at pH, and concentration is to soak 15 minutes in the aqueous solution of gold chloride of 5mM, and is clean with pure water rinsing; Be to soak 10 minutes in the aqueous solution of 10mM silver nitrate in concentration then, clean with pure water rinsing; This multilayer film that will obtain at last places baking oven, heats 1 hour down at 200 ℃, promptly obtains gold-silver alloy nanoparticles.
Embodiment 7:
1) be that 7: 3 mass percent is after 98% sulfuric acid and mass percent are to soak 30 fens kinds in the mixed solution of 30% hydrogen peroxide, with pure water this sheet glass to be rinsed well with sheet glass in volume ratio;
2) sheet glass that step 1) was handled is 7.0 at pH, and concentration is to soak 10 minutes in the aqueous solution of polymine of branching of 5mg/ml, and is clean with pure water rinsing;
3) then sheet glass being soaked in pH is 3.5, and concentration is the polymethyl acid solution 10 minutes of 5mg/ml, and is clean with pure water rinsing again;
4) repeating step 2) and step 3) be 7 polyelectrolyte multilayer film to the double-deck number that obtains polyelectrolyte;
5) the double-deck number that step 4) is obtained is that 7 polyelectrolyte multilayer film is 2.0 at pH, and concentration is to soak 15 minutes in the aqueous solution of gold chloride of 5mM, and is clean with pure water rinsing; Be to soak 10 minutes in the aqueous solution of 10mM silver nitrate in concentration then, clean with pure water rinsing; This multilayer film that will obtain at last places baking oven, heats 1 hour down at 200 ℃, promptly obtains gold-silver alloy nanoparticles.
Embodiment 8:
1) be that 7: 3 mass percent is after 98% sulfuric acid and mass percent are to soak 30 fens kinds in the mixed solution of 30% hydrogen peroxide, with pure water this sheet glass to be rinsed well with sheet glass in volume ratio;
2) sheet glass that step 1) was handled is 7.0 at pH, and concentration is to soak 10 minutes in the aqueous solution of polymine of linearity of 5mg/ml, and is clean with pure water rinsing;
3) then sheet glass being soaked in pH is 3.5, and concentration is the polymethyl acid solution 10 minutes of 5mg/ml, and is clean with pure water rinsing again;
4) repeating step 2) and step 3) be 7 polyelectrolyte multilayer film to the double-deck number that obtains polyelectrolyte;
5) the double-deck number that step 4) is obtained is that 7 polyelectrolyte multilayer film is 2.0 at pH, and concentration is to soak 15 minutes in the aqueous solution of gold chloride of 5mM, and is clean with pure water rinsing; Be to soak 10 minutes in the aqueous solution of 10mM silver nitrate in concentration then, clean with pure water rinsing; This multilayer film that will obtain at last places baking oven, heats 1 hour down at 200 ℃, promptly obtains gold-silver alloy nanoparticles.
Curve 1-3 among Fig. 2 is respectively embodiment 5,4, the ultraviolet-visible absorption spectroscopy of 1 gold-silver alloy nanoparticles that makes, show that the nano particle that makes has unimodal plasma and absorbs feature, its absworption peak is between monometallic Nano silver grain and golden nanometer particle, and along with the increase of the mol ratio of silver ion in the system and gold ion, absworption peak moves to short wavelength's direction.
Claims (1)
1. method for preparing gold-silver alloy nanoparticles in polyelectrolyte multilayer film is characterized in that step and condition are as follows:
1) be that 7: 3 mass percent is after 98% sulfuric acid and mass percent are to soak 30 fens kinds in the mixed solution of 30% hydrogen peroxide, with pure water this sheet glass to be rinsed well with sheet glass in volume ratio;
2) sheet glass that step 1) was handled is 5.0-9.0 at pH, and concentration is to soak 10 minutes in the aqueous solution of the polymine of branching of 5mg/ml or linear polymine, and is clean with pure water rinsing;
3) then, with step 2) to be soaked in pH be 3.0-7.0 for the sheet glass handled, and concentration is the polyacrylic acid of 5mg/ml or polymethyl acid solution 10 minutes, and water is rinsed well again;
4) repeating step 2) and step 3), polyelectrolyte multilayer film obtained;
5) polyelectrolyte multilayer film that step 4) is obtained is 2.0-3.0 at pH, and concentration is to soak 15 minutes in the aqueous solution of gold chloride of 5mM, and is clean with pure water rinsing; In the aqueous solution of 10mM silver nitrate, soaked 1-10 minute then, clean with pure water rinsing; This multilayer film that will obtain at last places baking oven, heats 1 hour down at 200 ℃, obtains gold-silver alloy nanoparticles.
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| US9718013B2 (en) * | 2012-02-27 | 2017-08-01 | Kx Technologies Llc | Formation and immobilization of small particles by using polyelectrolyte multilayers |
| CN103543109B (en) * | 2013-08-12 | 2016-08-10 | 苏州大学 | LSPR sensing membrane for measuring mercury ions and preparation method thereof |
| CN103409750B (en) * | 2013-08-15 | 2015-08-19 | 南京邮电大学 | Array type Silver nanorod of a kind of finishing gold nano grain and preparation method thereof |
| CN103521754B (en) * | 2013-10-14 | 2017-02-15 | 厦门大学 | Method for preparing surface enhancement Raman spectroscopy substrate material |
| CN104999088B (en) * | 2015-07-03 | 2017-03-29 | 中国地质大学（北京） | A kind of golden nanometer particle redox graphene multilamellar film composite material and preparation method thereof |
| CN106483116B (en) * | 2016-09-27 | 2019-12-06 | 东南大学 | Preparation method of hollow-core optical fiber SERS probe based on self-assembly of two silver nanoparticles |
| CN108267428A (en) * | 2016-12-30 | 2018-07-10 | 北京大学深圳研究生院 | Portable reinforced surface plasma resonance biosensor |
| CN111272727B (en) * | 2018-12-05 | 2021-09-03 | 同济大学 | Substrate material for detecting chiral compounds |
| CN109794175A (en) * | 2018-12-26 | 2019-05-24 | 浙江大学 | Graphene oxide composite membrane with pH responsiveness and preparation method and use thereof |
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| CN1772363A (en) * | 2004-11-11 | 2006-05-17 | 中国科学院化学研究所 | Method for preparing hollow sphere and composite hollow sphere by template method |
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