CN101344484B - Nano-silver film preparation method for high-efficiency detecting biomacromolecule and microbe - Google Patents
Nano-silver film preparation method for high-efficiency detecting biomacromolecule and microbe Download PDFInfo
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- CN101344484B CN101344484B CN2008100588709A CN200810058870A CN101344484B CN 101344484 B CN101344484 B CN 101344484B CN 2008100588709 A CN2008100588709 A CN 2008100588709A CN 200810058870 A CN200810058870 A CN 200810058870A CN 101344484 B CN101344484 B CN 101344484B
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Abstract
The invention discloses a method which prepares a nano silver film used for detecting biological macromolecules and microorganisms in high efficiency, the method adds solid particles of silver nitrate(AgNo3) and solid particles of polyvinyl alcohol (PVA) into high-purity water with the electric conductance less than 0.2 microseconds per centimeter and heats the high-purity water until the solid particles are completely dissolved, a mixture solution with all dissolved solid particles is taken as an electrolyte, and one surface of a substance that has a negative charge and two even surfaces without slopes is fixed on a container wall and led to contact with the electrolyte. Two silver rods with the purity equal to or more than 99.5 percent are inserted into the electrolyte, direct current voltage of 25 to 50 V is applied, electricity is supplied for 1 to 3 hours, the electrolyte and a substrate are then positioned in a heliophobe place for 12 to 24 hours, and then the substrate is takenout and dried. When used for the detection of biological macromolecules and microorganisms, the method has the remarkable advantages of good stability, favor for longtime storage, convenient use in any time and acquisition of stable Raman spectrum.
Description
Technical field
The present invention relates to the nanometer silverskin of a kind of efficient detection biomacromolecule and microorganism, belong to the nanometer applied technical field.
Background technology
The Surface enhanced raman spectroscopy technology, because can detect individual molecule has obtained using widely at everyways such as physics, chemistry, biologies in recent years, a concrete problem of running in the detection of biomacromolecule, microorganism is: how to make the surface of preparation strengthen substrate, strengthen effective, good reproducibility.Existing surface commonly used strengthens silver substrate elargol, silver-colored island and nanometer silverskin.
Elargol is since last century, the seventies made with chemical reduction method, and technology of preparing reaches its maturity, and is widely used in the middle of the enhancing of Raman spectrum surface.But elargol is because nano-Ag particles disperses inhomogeneously in colloid, and the electric field humidification that is produced does not have other substrate good, so the enhancing effect is not fine.The disperse state of this Nano Silver just in addition, the repeatability of feasible Raman spectrum of working it out is quite bad, even the method that had human to add polycoagulant has afterwards been improved this defective, but general test biomacromolecule and microorganism the time, effect still is not very desirable.
The silver island is not long as the substrate time that the Raman spectrum surface strengthens, but the people of research also is a lot of now.As silver-colored island, his surperficial enhanced mechanism also is to produce owing to electric field action that the silver-colored particle that flocks together produces.But because silver-colored island is similar to the island of the dispersion in the life, very big of distance between two silver-colored islands, so it is not very desirable strengthening effect, though have the people to improve the enhancing effect now, up to the present strengthen effect and also be not enough to it as in the middle of the large-scale practical application by controlling the distance between the silver-colored island and the size on silver-colored island.
The nanometer silverskin is that a kind of surface of using always strengthens substrate, and commonly used at present has: with dull and stereotyped sputter of laser and electronation preparation two kinds.The method of the dull and stereotyped sputter of laser can be prepared the silverskin of uniform particles marshalling, and changes spacing between the nano-Ag particles by changing pitch-row on the flat board, strengthens effect preferably thereby seek.Utilize the repeated relatively good of nanometer silverskin Surface enhanced raman spectroscopy that the method for dull and stereotyped sputter makes; but because the silverskin of making majority is the individual layer silverskin; formed " hot spot-effect " or " hot link effect " is not clearly; effect is fine when doing the micromolecule particle; because the micromolecule particle can be easily and the nano-Ag particles combination; but when doing biomacromolecule particle or microorganism just dying; because biomacromolecule and microorganism is big or small indefinite; for size and the silverskin all fixed of spacing; can not allow a lot of particles to be detected well combine, so effect is very undesirable when doing the Surface enhanced raman spectroscopy that is similar to biomacromolecule and microorganism with nano-Ag particles.And the method for the dull and stereotyped sputter of laser will be used expensive devices such as high power laser, so the cost of preparation is quite high.The method of electronation can be prepared the nano particle silverskin of different shape, Leaves'Shape for example, the flower shape or the like, and can change and strengthen effect by changing shape and grain spacing, but also not have the silverskin of the method preparation of that a kind of electronation can obtain Surface enhanced raman spectroscopy widely biomacromolecule and microorganism.In addition, also having a problem is in big molecule of Raman spectrometer detection of biological and microorganism, these wait to separate side material itself with the fluorescence let us be difficult to obtain desirable Raman spectrum, the silverskin that existing all methods are made all can not well address this problem.So the cost that the problem that existing Surface enhanced raman spectroscopy substrate exists mainly contains can't obtain stable Raman spectrum, make substrate is very high, biomacromolecule and microorganism are not had universality, can't solve fluorescence problem of biomacromolecule and microorganism or the like.
Summary of the invention
The objective of the invention is to overcome the weak point that above-mentioned nanometer silverskin exists; and provide the nanometer silverskin of a kind of efficient detection biomacromolecule microorganism; its principle is to utilize electrolytic silver rod method to obtain nano-Ag particles, is that protective agent makes the nano-Ag particles of positively charged not take place to condense and directly be adsorbed on the electronegative medium in colloid with polyvinyl alcohol (PVA).The nanometer silverskin that adopts the method to prepare not only has good Raman spectrum to strengthen effect to micromolecule, and has good especially fluorescent quenching and surface to strengthen effect to biomacromolecule and microorganism.
The objective of the invention is to realize by following technical solution.Silver nitrate (AgNo
3) solid particle and polyvinyl alcohol (PVA) (PVA) solid particle join electricity lead＜high purity water of 0.2 μ S/cm in, being heated to 100 ℃ all dissolves solid particle, mixed liquor after the solid particle dissolving is as electrolytic solution, wherein, silver nitrate accounts for 0.005% to 0.015% of electrolyte quality, and polyvinyl alcohol (PVA) accounts for 0.025% to 0.1% of electrolyte quality.The electrolytic solution of making is poured in the clean container of not charged or positively charged, the clean electronegative two-sided smooth material that does not have a gradient tightly is fixed on as substrate makes it have only one side on the chamber wall with the electrolytic solution contact.The silver rod of two purity 〉=99.5% is inserted in the electrolytic solution respectively as both positive and negative polarity, add the 30V DC voltage then in the above, switched on 1～3 hour.The electrolytic solution of electricity charged is placed on the place 12～24 hours of lucifuge, the nano-Ag particles combination that makes substrate have sufficient chance to go out with electrolysis together with substrate.Then substrate is taken out from electrolytic solution and dried, the one side that contacts with nano-Ag particles is the nanometer silverskin for preparing.
The invention has the beneficial effects as follows, good stability, process is to the test shows of the Surface enhanced raman spectroscopy of the difference of the sample on the same silverskin, and this silverskin has fabulous repeatability, the strong and peak position basically identical of the Raman peaks of each sample difference.The present invention is by scanning electronic microscope observation, and the mean grain size of nano-Ag particles is at 200nm.And the mean size of the nano-Ag particles that the electrolysis by scanning electron microscope observation goes out is 30nm, be far smaller than the nano particle on the silverskin, clustering phenomena has taken place in the nano-Ag particles on this explanation silverskin, single silver-colored particle aggregation about nearly ten becomes a big silver-colored particle on the silverskin, because this clustering phenomena, make the electric filed enhanced effect growth at double of Nano Silver, the effect that the surface strengthens is also just stronger.And can't obtain or strengthen the bad Surface enhanced raman spectroscopy of effect for traditional silverskin, as tobacco mosaic virus (TMV), Escherichia coli, staphylococcus, the human body haemocyte, serum etc., this silverskin all shows the repeatability of good surface-enhanced Raman effects and high-quality, this be because size of nano-Ag particles on the silverskin and spacing in the data area of existing optimization model, but not to be fixed under a certain size, distribute but present the irregular grains of sand shape that is similar to, this has the chance of an a lot of and silver-colored particle combination just for macromolecular particle and microorganism, these materials to be detected are understood and oneself are searched out suitable silver-colored particle, thereby above being adsorbed on, produce maximum electric filed enhanced effect, detected by Raman spectrometer.In addition at room temperature, the nanometer silverskin for preparing is kept in the high purity water, can makes things convenient for use at any time, the effective time of preserving silverskin is more than half a year.And this Nano Silver film preparation condition is simple, spends cheaply, has popularizing value widely.
Embodiment
Embodiment one is 20.0mg silver nitrate (AgNo
3) solid particle and 70.0mg polyvinyl alcohol (PVA) (PVA) solid particle join the 200ml electricity lead＜high purity water of 0.2 μ S/cm in, being heated to 100 ℃ all dissolves solid particle, the electrolytic solution of making is poured in the square plastic container, get 4 microslides and clean respectively three times with the concentrated sulphuric acid and high concentration of hydrogen kali, the back is washed three times with high purity water.The microslide of wash clean tightly is fixed on makes it have only one side in the square container with electrolytic solution contact.The silver rod of two purity 〉=99.5% is inserted in the electrolytic solution as both positive and negative polarity, add the 25V DC voltage then in the above, switched on 1 hour.The electrolytic solution of electricity charged was placed on the lucifuge place 12 hours together with microslide, the nano-Ag particles combination that makes microslide have sufficient chance to go out with electrolysis.Then microslide is taken out from electrolytic solution and dried, the one side that contacts with nano-Ag particles is the nanometer silverskin for preparing.
Embodiment two is 25.0mg silver nitrate (AgNo
3) solid particle and 100.0mg polyvinyl alcohol (PVA) (PVA) solid particle join the 200ml electricity lead＜high purity water of 0.2 μ S/cm in, being heated to 100 ℃ all dissolves solid particle, the electrolytic solution of making is poured in the rectangle plastics beaker, get 8 cloudlet master slices and clean respectively three times with the concentrated sulphuric acid and high concentration of hydrogen kali, the back is washed three times with high purity water.The mica sheet of wash clean tightly is fixed on makes it have only one side in the square container with electrolytic solution contact.The silver rod of two purity 〉=99.5% is inserted in the electrolytic solution as both positive and negative polarity, add the 35V DC voltage then in the above, switched on 2 hours.The electrolytic solution of electricity charged was placed on the lucifuge place 18 hours together with mica sheet, the nano-Ag particles combination that makes mica sheet have sufficient chance to go out with electrolysis.Then mica sheet is taken out from electrolytic solution and dried, the one side of touching with silver-colored nano-Ag particles is the nanometer silverskin for preparing.
Embodiment three is 30.0mg silver nitrate (AgNo
3) solid particle and 150.0mg polyvinyl alcohol (PVA) (PVA) solid particle join the 200ml electricity lead＜high purity water of 0.2 μ S/cm in, being heated to 100 ℃ all dissolves solid particle, the electrolytic solution of making is poured in the rhombus plastic beaker, get 2 microslides and clean respectively three times with the concentrated sulphuric acid and high concentration of hydrogen kali, the back is washed three times with high purity water.The microslide of wash clean tightly is fixed on makes it have only one side in the rhombus container with electrolytic solution contact.The silver rod of two purity 〉=99.5% is inserted in the electrolytic solution as both positive and negative polarity, add the 50V DC voltage then in the above, switched on 3 hours.The electrolytic solution of electricity charged was placed on the lucifuge place 24 hours together with microslide, the nano-Ag particles combination that makes microslide have sufficient chance to go out with electrolysis.Then microslide is taken out from electrolytic solution and dried, the one side that contacts with nano-Ag particles is the nanometer silverskin for preparing.
Claims (1)
1. efficient detection biomacromolecule and microorganism Nano Silver membrane preparation method is characterized in that, silver nitrate (AgNo
3) solid particle and polyvinyl alcohol (PVA) (PVA) solid particle join electricity lead＜high purity water of 0.2 μ S/cm in, being heated to solid particle all dissolves, mixed liquor after the solid particle dissolving is as electrolytic solution, wherein, silver nitrate accounts for 0.005% to 0.015% of electrolyte quality, and polyvinyl alcohol (PVA) accounts for 0.025% to 0.1% of electrolyte quality; The electrolytic solution of making is poured in the container of not charged or positively charged, the electronegative two-sided smooth clean microslide that does not have a gradient or mica sheet tightly be fixed on as substrate make it have only one side on the chamber wall with the electrolytic solution contact, the silver rod of two purity 〉=99.5% is inserted in the electrolytic solution respectively as both positive and negative polarity, add 25～50V DC voltage then in the above, switched on 1～3 hour; The electrolytic solution of electricity charged is placed on the place 12～24 hours of lucifuge, the nano-Ag particles combination that makes substrate have sufficient chance to go out with electrolysis together with substrate; Then substrate is taken out from electrolytic solution and dried, the one side that contacts with nano-Ag particles is the nanometer silverskin for preparing.
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| CN101344484B true CN101344484B (en) | 2010-06-16 |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102183502B (en) * | 2011-01-14 | 2012-12-12 | 楚雄师范学院 | Method for preparing nano silver film with enhanced Raman scattering substrate based on microwave technique |
| CN102181891B (en) * | 2011-04-08 | 2012-11-07 | 温州大学 | Silver nanodendrite surface enhanced Raman scattering (SERS) substrate, and preparation method and application thereof |
| CN103063607B (en) * | 2011-10-20 | 2015-07-29 | 西北工业大学 | A kind of optical refractive index sensor based on meta-material absorber |
| CN104458694A (en) * | 2014-11-28 | 2015-03-25 | 中国科学院合肥物质科学研究院 | Method for enhancing Raman signals with nano super-crystal technology to identify microorganisms |
| CN107525795A (en) * | 2016-06-21 | 2017-12-29 | 天津大学 | Application of the polyvinyl alcohol composite hydrogel in using Raman spectrum detection rhodamine |
| CN107525794A (en) * | 2016-06-21 | 2017-12-29 | 天津大学 | Application of the polyvinyl alcohol-nano silver composite material in using Raman spectrum detection crystal violet |
| CN106280157A (en) * | 2016-08-11 | 2017-01-04 | 潘忠宁 | A kind of preparation method of AgNO3/PVA composite membrane |
| CN108760714A (en) * | 2018-03-05 | 2018-11-06 | 华南理工大学 | The method that noble metal quenching fluorescence is used in Raman spectrum |
| CN110559126A (en) * | 2019-08-13 | 2019-12-13 | 深圳恩必德电子科技有限公司 | waterproof and antibacterial perforated graphene eye patch and manufacturing process thereof |
| CN111175281A (en) * | 2020-02-24 | 2020-05-19 | 江苏师范大学 | Rapid detection method of flavoprotein prosthetic group based on surface enhanced Raman spectroscopy |
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