CN101775594A - Method for preparing silver nano material on surfaces of silicon wafers - Google Patents
Method for preparing silver nano material on surfaces of silicon wafers Download PDFInfo
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- CN101775594A CN101775594A CN201010106584A CN201010106584A CN101775594A CN 101775594 A CN101775594 A CN 101775594A CN 201010106584 A CN201010106584 A CN 201010106584A CN 201010106584 A CN201010106584 A CN 201010106584A CN 101775594 A CN101775594 A CN 101775594A
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Abstract
The invention discloses a method for preparing silver nano material on the surfaces of silicon wafers, which belongs to the field of nano material preparation. The surface of a silicon wafer is firstly cleaned, the silicon wafer is then put into the mixed solution of hydrofluoric acid and silver nitrate, and is processed for 1 to 2 minutes in room temperature, the silicon wafer is taken out, washed by deionized water and then naturally aired, and thereby the silver nano material growing on the surface of the silicon wafer can be obtained. The condition of the preparation method is simple, high temperature is not needed, the outfield auxiliary equipment is not needed, stabilizer, surfactant and organic solvent do not need to be added, a template is not needed, the reaction time is short, and the cost is low.
Description
Technical field
The present invention relates to a kind ofly prepare the method for silver nano material at silicon chip surface, belong to field of nano material preparation by chemical process.
Background technology
Nanometer silver is a kind of emerging functional materials, has very high specific surface area and surfactivity, is widely used as catalytic material, antistatic material, low temperature superconducting material and bio-sensing modulator material etc.
The preparation method of nanometer silver is a lot, comprises chemical reduction method, microemulsion method, outfield auxiliary law, electrochemical process, template etc.
Chemical reduction method generally is meant under liquid-phase condition, method with the silver-colored compound nanometer silver material of reductive agent reduction, existing chemical reduction method normally adds dispersion agent in solution, with hydrazine hydrate, sodium borohydride, inferior sodium phosphate, glucose, xitix, hydrogen peroxide etc. are made the compound of reductive agent reduction silver, as document " Sun Y.G.; Mayers B.; Herricks T.; etal.Polyol synthesis of uniform silver nanowires:A plausible growth mechanism and the supportingevidence.Nano Letters; 2003; 3 (7): 955-960 " and " Sun Y.G., Xia Y.N.Shape-controlled synthesis of goldand silver nanoparticles.Science, 2002,298 (5601): 2176-2179 ".The nanoparticle of present used chemical reduction method preparation is easy to reunite, usually need to add some special organic compound such as tensio-active agent, polymkeric substance or title complex as coating (stablizer) passivation nanoparticle surface, stop may reunite between the nanoparticle.
Because nanoparticle is easy to reunite, therefore, microemulsion (reverse micelle) method is used to preparation size homogeneous, the controlled nano particle of particle diameter as a kind of soft template technology.Microemulsion is usually by water in the microemulsion method, tensio-active agent is with the tertiary mixture of oil or by water, tensio-active agent, the quaternary mixture of cosurfactant and oil is formed, this method can be synthesized the nano material of specific dimensions and pattern, can be in the water nuclear of reverse micelle the nucleation of crystal grain and growth limitation, as document " Bagwe R.P.; Khilar K.C.Effectsof intermicellar exchange rate on the formation of silver nanoparticles in reverse microemulsionsof AOT.Langmuir; 2000; 16 (3): 905-910 " and " May S.; Ben-Shaul A.Molecular theory of thesphere-to-rod transition and the second CMC in aqueous micellar solutions.Journal of PhysicalChemistry B; 2001,105 (3): 630-640 ".Yet micro-emulsion method for preparing nano silver also comes with some shortcomings.For example, need to add a large amount of tensio-active agents and organic solvent in this system, synthetic cost is higher.In addition, the tensio-active agent of interpolation needs to separate operational difficulty with nano silver particles with organic solvent.
Outfield auxiliary law such as microwave assisting method etc. also are used to prepare the nano material of silver.The penetrativity of microwave is strong, and homogeneous heating has volume heating effect fast, and the advantages such as speed of reaction of fast lifting system at short notice have easy, quick, nanocrystal with microwave application in nano material synthetic and are easy to advantages such as nucleation.Microwave-assisted prepares silver nano material method such as document " Liu F.K.; Huang P.W., Chang Y.C., et al.Microwave-assisted synthesis of silvernanorods.Journal of Materials Research; 2004,19 (2): 469-473 ".Yet the outfield householder method needs airfield equipment, simultaneously, the nano particle diameter that this method the obtains relative broad that distributes, desire obtains often difficulty relatively of the silver nano-particle of small size, narrow distribution or cluster.
Electrochemical process is according to electrochemical principle, in solution, produce unbound electron, for the reduction of silver ions provides condition, as document " Zhang Y.H.; Chen F., Zhuang J.H., et al.Synthesis of silver nanoparticles via electrochemicalreduction on compact zeolite film modified electrodes.ChemicalCommunications; 2002, (23): 2814-2815 ".This method needs electrochemical appliance, simultaneously, when the electrolysis Ag-containing compound aqueous solution, needs to add a certain amount of coordination agent usually.
Template, be with anodised aluminium (AAO), nanotube, mesoporous SiO2, DNA, tensio-active agent such as PVP, AOT and CTAB etc. prepare nano wire and nanometer rod as template, as document " Malandrino G.; Finocchiaro S.T.; FragalaI.L.Silver nanowires by a sonoself-reduction template process.Journal of MaterialsChemistry; 2004; 14 (18): 2726-2728 " and " Behrens S.; Wu J., Habicht W., et al.Silver nanoparticle andnanowire formation by microtubule templates.Chemistry of Materials, 2004,16 (16): 3085-3090 ".The template advantage be can strict control nano wire pattern, shortcoming is that nanowire size is limited by template size, the different size nano wire need prepare different templates, yields poorly, cost is too high.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing silver nano material at silicon chip surface, belong to chemical reduction method, overcome existing chemical reduction method and need add coating, it is the deficiency of stablizer, overcome the deficiency that microemulsion method need add tensio-active agent and organic solvent, overcome the outfield auxiliary law and needed the outfield utility appliance, deficiency as microwave generating apparatus, having overcome electrochemical process needs the deficiency of electrochemical appliance, overcome the deficiency of the extra templates of template need, simple to operate, with low cost.
The present invention solves its technical problem, and the technical scheme that is adopted is as follows:
A kind ofly prepare the method for silver nano material, may further comprise the steps at silicon chip surface:
Step 1: silicon chip surface is cleaned, cleaning sequence to silicon chip is to clean 5-10 minute with the acetone concussion, cleaned 5-10 minute with the ethanol concussion then, mixed solution of hydrogen peroxide with 98% sulfuric acid and 30% cleaned 5-10 minute again, and the volumetric ratio of described 98% sulfuric acid and 30% hydrogen peroxide is 3: 1.
Step 2: the silicon chip that will clean is put into the Silver Nitrate mixing solutions that hydrofluoric acid that concentration is 2.3mol/L-4.6mol/L and concentration are 0.01mol/L-0.04mol/L, room temperature treatment 0.5-2 minute.
Step 3: take out silicon chip, with drying naturally after the rinsed with deionized water.
The invention has the beneficial effects as follows: it is silver nano material about tens to 100 microns that the present invention can prepare length.Compare with existing silver nano material preparation method, this preparation method condition is simple, does not need high temperature, do not need the outfield utility appliance, do not need to add stablizer, tensio-active agent and organic solvent, do not need template, reaction times is short, therefore greatly reduces cost.
Description of drawings
Fig. 1 is the stereoscan photograph of the silver nano material of embodiment 1 preparation.
Fig. 2 is that the XRD of the silver nano material of embodiment 1 preparation can spectrogram.
Fig. 3 is the stereoscan photograph of the silver nano material of embodiment 2 preparations.
Fig. 4 is the stereoscan photograph of the silver nano material of embodiment 3 preparations.
Fig. 5 is the stereoscan photograph of the silver nano material of embodiment 4 preparations.
Fig. 6 is the stereoscan photograph of the silver nano material of embodiment 5 preparations.
Embodiment
Embodiment 1
Silicon chip was cleaned 5 minutes with acetone concussion, cleaned 5 minutes with the ethanol concussion then, with the mixed solution of hydrogen peroxide cleaning of 98% sulfuric acid and 30% 5 minutes, the volumetric ratio of described 98% sulfuric acid and 30% hydrogen peroxide was 3: 1 again.The silicon chip that cleaned is put into the hydrofluoric acid of 2.3mol/L and the Silver Nitrate mixing solutions of 0.02mol/L, room temperature treatment 2 minutes.Take out silicon chip, with drying naturally after the rinsed with deionized water.The stereoscan photograph of the silver nano material that on silicon chip, prepares as shown in Figure 1, as can be seen from the figure, the silver nano material of preparation is dendritic, maximum diameter 870 nanometers, 23.15 microns of maximum lengths.The EDS energy spectrogram of the silver nano material for preparing on silicon chip as shown in Figure 2, as can be seen from the figure, choose 1: 009 on silver nano material, the atom content (Atom%) of this some place element (Element) silver (Ag) is 69.02%, illustrates that it is a silver nano material.
Embodiment 2
Silicon chip was cleaned 8 minutes with acetone concussion, cleaned 8 minutes with the ethanol concussion then, with the mixed solution of hydrogen peroxide cleaning of 98% sulfuric acid and 30% 8 minutes, the volumetric ratio of described 98% sulfuric acid and 30% hydrogen peroxide was 3: 1 again.The silicon chip that cleaned is put into the hydrofluoric acid of 2.3mol/L and the Silver Nitrate mixing solutions of 0.01mol/L, room temperature treatment 1 minute.Take out silicon chip, with drying naturally after the rinsed with deionized water.The stereoscan photograph of the silver nano material for preparing on silicon chip as shown in Figure 3.
Embodiment 3
Silicon chip was cleaned 10 minutes with acetone concussion, cleaned 10 minutes with the ethanol concussion then, with the mixed solution of hydrogen peroxide cleaning of 98% sulfuric acid and 30% 10 minutes, the volumetric ratio of described 98% sulfuric acid and 30% hydrogen peroxide was 3: 1 again.The silicon chip that cleaned is put into the hydrofluoric acid of 3.5mol/L and the Silver Nitrate mixing solutions of 0.03mol/L, room temperature treatment 2 minutes.Take out silicon chip, with drying naturally after the rinsed with deionized water.The stereoscan photograph of the silver nano material for preparing on silicon chip as shown in Figure 4.
Embodiment 4
Silicon chip was cleaned 5 minutes with acetone concussion, cleaned 5 minutes with the ethanol concussion then, with the mixed solution of hydrogen peroxide cleaning of 98% sulfuric acid and 30% 5 minutes, the volumetric ratio of described 98% sulfuric acid and 30% hydrogen peroxide was 3: 1 again.The silicon chip that cleaned is put into the hydrofluoric acid of 4.6mol/L and the Silver Nitrate mixing solutions of 0.02mol/L, room temperature treatment 1 minute.Take out silicon chip, with drying naturally after the rinsed with deionized water.The stereoscan photograph of the silver nano material for preparing on silicon chip as shown in Figure 5.
Embodiment 5
Silicon chip was cleaned 10 minutes with acetone concussion, cleaned 10 minutes with the ethanol concussion then, with the mixed solution of hydrogen peroxide cleaning of 98% sulfuric acid and 30% 10 minutes, the volumetric ratio of described 98% sulfuric acid and 30% hydrogen peroxide was 3: 1 again.The silicon chip that cleaned is put into the hydrofluoric acid of 4.6mol/L and the Silver Nitrate mixing solutions of 0.04mol/L, room temperature treatment 2 minutes.Take out silicon chip, with drying naturally after the rinsed with deionized water.The stereoscan photograph of the silver nano material for preparing on silicon chip as shown in Figure 6.
Claims (2)
1. one kind prepares the method for silver nano material at silicon chip surface, it is characterized in that: may further comprise the steps:
Step is cleaned silicon chip surface.
Step 2: the silicon chip that will clean is put into the Silver Nitrate mixing solutions that hydrofluoric acid that concentration is 2.3mol/L-4.6mol/L and concentration are 0.01mol/L-0.04mol/L, room temperature treatment 0.5-2 minute.
Step 3: take out silicon chip, with drying naturally after the rinsed with deionized water.
2. according to the described preparation method of claim 1, it is characterized in that: the detailed process of in the described step 1 silicon chip surface being cleaned is: cleaned 5-10 minute with the acetone concussion, cleaned 5-10 minute with the ethanol concussion then, mixed solution of hydrogen peroxide with 98% sulfuric acid and 30% cleaned 5-10 minute again, and the volumetric ratio of described 98% sulfuric acid and 30% hydrogen peroxide is 3: 1.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2473352C2 (en) * | 2011-04-21 | 2013-01-27 | Закрытое акционерное общество "Институт прикладной нанотехнологии" | Intra-articular fluid simulator formulation and method for preparing intra-articular fluid additive |
| CN103116019A (en) * | 2013-01-16 | 2013-05-22 | 宁波大学 | Preparation method of immune base and antigen or antibody immunoassay method |
| CN103451632A (en) * | 2013-04-22 | 2013-12-18 | 深圳信息职业技术学院 | Micro-nano silver, copper or silver-copper alloy film and preparation method thereof |
| CN103741122A (en) * | 2014-01-20 | 2014-04-23 | 厦门大学 | Chemical plating method for preparing smooth and sharp AFM-TERS (Atomic Force Microscopy-Tip-Enhanced Raman Spectroscopy) needle point |
| CN104593756A (en) * | 2015-02-10 | 2015-05-06 | 江西赛维Ldk太阳能高科技有限公司 | Coating silicon-based material as well as preparation method and coating treatment liquid thereof |
| CN105039942A (en) * | 2015-08-18 | 2015-11-11 | 西安交通大学 | Preparation method of silver dendrite and silicon tip nanocomposite with cactus structure |
| CN106735295A (en) * | 2016-12-12 | 2017-05-31 | 中南大学 | A kind of two-dimensional layer Au nanometer sheet materials and preparation method thereof |
| CN109192793A (en) * | 2018-09-07 | 2019-01-11 | 深圳信息职业技术学院 | A kind of preparation method of silicon solar cell silver electrode |
| CN114012103A (en) * | 2021-10-21 | 2022-02-08 | 云南省产品质量监督检验研究院 | Method for preparing silver nanoparticles with controllable size on silicon surface |
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2010
- 2010-02-04 CN CN201010106584A patent/CN101775594A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2473352C2 (en) * | 2011-04-21 | 2013-01-27 | Закрытое акционерное общество "Институт прикладной нанотехнологии" | Intra-articular fluid simulator formulation and method for preparing intra-articular fluid additive |
| CN103116019A (en) * | 2013-01-16 | 2013-05-22 | 宁波大学 | Preparation method of immune base and antigen or antibody immunoassay method |
| CN103116019B (en) * | 2013-01-16 | 2015-03-18 | 宁波大学 | Preparation method of immune base and antigen or antibody immunoassay method |
| CN103451632A (en) * | 2013-04-22 | 2013-12-18 | 深圳信息职业技术学院 | Micro-nano silver, copper or silver-copper alloy film and preparation method thereof |
| CN103741122A (en) * | 2014-01-20 | 2014-04-23 | 厦门大学 | Chemical plating method for preparing smooth and sharp AFM-TERS (Atomic Force Microscopy-Tip-Enhanced Raman Spectroscopy) needle point |
| CN104593756A (en) * | 2015-02-10 | 2015-05-06 | 江西赛维Ldk太阳能高科技有限公司 | Coating silicon-based material as well as preparation method and coating treatment liquid thereof |
| CN105039942A (en) * | 2015-08-18 | 2015-11-11 | 西安交通大学 | Preparation method of silver dendrite and silicon tip nanocomposite with cactus structure |
| CN105039942B (en) * | 2015-08-18 | 2017-12-08 | 西安交通大学 | The preparation method of the silver-colored dendrite of cactus structure/silicon needle point nano composite material |
| CN106735295A (en) * | 2016-12-12 | 2017-05-31 | 中南大学 | A kind of two-dimensional layer Au nanometer sheet materials and preparation method thereof |
| CN106735295B (en) * | 2016-12-12 | 2018-11-23 | 中南大学 | A kind of two-dimensional layer Au nanometer sheet material and preparation method thereof |
| CN109192793A (en) * | 2018-09-07 | 2019-01-11 | 深圳信息职业技术学院 | A kind of preparation method of silicon solar cell silver electrode |
| CN114012103A (en) * | 2021-10-21 | 2022-02-08 | 云南省产品质量监督检验研究院 | Method for preparing silver nanoparticles with controllable size on silicon surface |
| CN114012103B (en) * | 2021-10-21 | 2023-03-07 | 云南省产品质量监督检验研究院 | Method for preparing silver nanoparticles with controllable size on silicon surface |
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Inventor after: He Yang Inventor after: Jiang Chengyu Inventor after: Yin Hengxu Inventor after: Zhang Feng Inventor after: Chen Jun Inventor after: Tian Mengjun Inventor after: Yuan Weizheng Inventor before: He Yang Inventor before: Yin Hengxu Inventor before: Tian Mengjun Inventor before: Jiang Chengyu Inventor before: Yuan Weizheng |
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Free format text: CORRECT: INVENTOR; FROM: HE YANG YIN HENGXU TIAN MENGJUN JIANG DENGYU YUAN WEIZHENG TO: HE YANG JIANG DENGYU YIN HENGXU ZHANG FENG CHEN JUN TIAN MENGJUN YUAN WEIZHENG |
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Application publication date: 20100714 |