CN101590527A - A kind of preparation method of nano-porous silver - Google Patents
A kind of preparation method of nano-porous silver Download PDFInfo
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- CN101590527A CN101590527A CNA2009100164161A CN200910016416A CN101590527A CN 101590527 A CN101590527 A CN 101590527A CN A2009100164161 A CNA2009100164161 A CN A2009100164161A CN 200910016416 A CN200910016416 A CN 200910016416A CN 101590527 A CN101590527 A CN 101590527A
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Abstract
The invention belongs to field of nano material preparation, relate in particular to a kind of preparation method of nano-porous silver.The present invention adopts rapid solidification and takes off the method that alloying combines and prepares nano-porous silver, at first pure metallic aluminum, silver is heated to molten state; Then, utilize inert gas that alloy liquid is blown out fast, make liquid metal rapid solidification on the high speed copper roller rotating of fusion, prepare alloy strip; At last, in sour corrosion solution, take off Alloying Treatment; Corrosion process is washed till neutrality with nano-porous silver after finishing in distilled water.This method selects for use the lower etchant solution of concentration can obtain nano-porous silver, and operating procedure is easy, suitability for mass industrialized production.This method also can be according to the kind of the composition and the etchant solution of foundry alloy, the structure and the size of regulation and control nano-porous silver.
Description
Technical field
Invention belongs to field of nano material preparation, relates in particular to a kind of preparation method of nano-porous silver.
Background technology
Nano porous metal is the material with nano-scale hole, and its aperture size is that several nanometers are to the hundreds of nanometer.At present, taking off alloying is to prepare the main method of cavernous structure nano porous metal at random.The object of choosing mostly is the solid solution alloy of binary, and by selecting suitable caustic solution, with wherein comparatively active dissolving metal, the metallic atom of remaining comparatively inertia is through the final nano-porous structure that forms co-continuous of diffusion reorganization.Wherein, the report of relevant porous gold is more in the nano porous metal preparation field.Calendar year 2001, Jonah Erlebacher (Erlebacher J, Aziz M, Karma A, et al.Nature, 2001,410 (22): 450-453.) Ag-32at.%Au and Ag-24at.%Au are taken off after the alloy, made thickness and be about the nanoporous gold thin film that 700nm, aperture size are about 10nm with red fuming nitric acid (RFNA).2004, people (Ding Y, Kim Y, Erlebacher J.Advanced Materials, 2004,16 (21): 1897-1900.) use 70wt.%HNO such as Ding Yi
3Ag, Au mass fraction be 50% the color leaf of commercially available platinum and carried out taking off alloy treatment, made thickness and be about 100nm, aperture size is about the nanoporous gold thin film of 20nm.2005, people (Dursun A such as Dursun Aziz, Pugh D, Corcoran S.Journal of theElectrochemical Society, 2005,152 (2): B65-B72.) with the mode of electrolytic etching Ag-20at.%Au, Ag-25at.%Au and Ag-30at.%Au have been carried out taking off alloy, the electrolyte that adopts in the corrosion process is the HClO of 0.1mol/L
4Yet, less about the preparation of nano-porous silver report, and mainly concentrate on the preparation method of the electrochemistry metal deposition-dissolution mechanism of complex process, Chinese (Jia, F.L. such as Fa-Long Jia; Yu, C.F.; Deng, K.J.; Zhang, L.Z.J.Phys.Chem.C 2007,111, and 8424.) utilize commercial galvanizing solution on silver electrode, to deposit one deck Zn film, utilize the Ag-Zn alloy thin layer of its formation, prepare attached to the suprabasil nano-porous silver thin layer of silver; (Yeh, F.H. such as the I-Wen Sun of TaiWan, China; Tai, C.C.; Huang, J.F.; Sun, I.W.J.Phys.Chem.B 2006,110, and 5215.) in the ZnCl-EMIC ionic liquid, also utilize similar electrochemical production to go out the nano-porous silver film.Adopt this Zn-Ag surface alloying/take off Alloying Treatment to prepare porous silver, its cost height, technology more complicated, the composition of Zn-Ag alloy is difficult to accurately control, and often only forms the nanoporous shape thin layer attached to fine and close substrate surface.
Summary of the invention
The objective of the invention is to overcome above-mentioned the deficiencies in the prior art, the preparation method of the nano-porous silver that a kind of cost is low, technology is simple, nano-porous structure is controlled is provided.
The present invention realizes in the following manner.
A kind of preparation method of nano-porous silver adopts rapid solidification and takes off the method that alloying combines to prepare nano-porous silver, it is characterized in that may further comprise the steps:
1, pure metallic aluminum, silver are heated to molten state, foundry alloy liquid is fully mixed;
2, utilize inert gas that alloy liquid is blown out fast, make liquid metal rapid solidification on the high speed copper roller rotating of fusion, prepare alloy strip;
3, in acid solution, take off Alloying Treatment; Corrosion process is washed till neutrality with nano-porous silver after finishing in distilled water; At last, sample dries and preserves.
The preparation method of above-mentioned nano-porous silver is characterized in that the inert gas in the step 2 is a kind of of argon gas, nitrogen.Acid solution in the step 3 is a kind of in hydrochloric acid, the sulfuric acid solution.Al-Ag alloy and 0.1～37wt.% hydrochloric acid solution or 0.1～98wt.% sulfuric acid solution were room temperature to 90 ℃ reaction 1～4 hour in the step 3.The ratio of greater inequality of acid solution is 5wt.% in the step 3.The freezing rate of Al-Ag alloy is 10 in the step 2
2～10
6K/s.The content of Ag is 10～60% (atomic percents) in the step 1, and all the other are Al, and total amount is 100%.
Concrete operations are as follows: aforementioned fine aluminium and fine silver metal are joined in the smelting furnace, be heated to molten condition, make its alloying through fully stirring.Blow out fast under 0.05～1MPa pressure with the liquid metal of inert gas with fusion, Quench on the high speed copper roller rotating makes alloy with 10
2～10
6K/s speed is solidified, and obtaining thickness is 10～200 μ m, and width is 1～50mm, and length is 0.5～50cm alloy strip.Wherein the content of Ag is 10～60% (atomic percents), and all the other are Al, and total amount is 100%.Above-mentioned alloy strip joined in the sour corrosion solution take off Alloying Treatment, handled 1～4 hour, filter out the solution metal band then, be washed till the pH test paper with distilled water and be neutral, take out at last and place.
Method of the present invention is compared with existing nano-porous silver preparation technology, has the following advantages:
(1) this method is selected the foundry alloy of Al-Ag alloy as nano-porous silver for use, can reduce the cost of preparation nano-porous silver greatly.(2) this method selects for use the lower common etchant solution of concentration can obtain nano-porous silver, and operating procedure is easy, suitability for mass industrialized production.(3) this method can be according to the kind of the composition and the etchant solution of foundry alloy, the structure and the size of regulation and control nano-porous silver.
The specific embodiment
Provide three most preferred embodiments of the present invention below:
Embodiment one
(1) according to atomic percent 15%Ag, all the other are the proportioning of Al, and the Al-Ag alloy is put into smelting furnace.Alloy is heated to molten condition, makes its alloying through fully stirring.Blow out fast under 0.1MPa pressure with the liquid of argon gas fusion, Quench on the high speed copper roller rotating, obtaining thickness is 20～40 microns, and width is 2～5 millimeters, and length is 1～20 centimetre alloy thin band.
(2) 25 ℃ down with 5wt.% hydrochloric acid solution reaction 0.5 hour, then be heated to 90 ℃ of reactions 0.5 hour to not significantly the reaction bubble produce, stop to heat.
(3) reacted product is collected, washed repeatedly to chemical attack solution clean fully (wide pH value test paper check flushing distilled water is neutral) with distilled water.Under 25 ℃, dry then and preserve.Aperture, hole wall size are about 90～100 nanometers, and pore structure evenly distributes.
Embodiment two
(1) according to atomic percent 35%Ag, all the other are the proportioning of Al, and the Al-Ag alloy is put into smelting furnace.Alloy is heated to molten condition, makes its alloying through fully stirring.Blow out fast under 0.1MPa pressure with the liquid of argon gas fusion, Quench on the high speed copper roller rotating, obtaining thickness is 30～50 microns, and width is 2～5 millimeters, and length is 5～20 centimetres alloy thin band.
(2) 25 ℃ down with 5wt.% sulfuric acid solution reaction 1 hour, then be heated to 90 ℃ of reactions 1 hour to not significantly the reaction bubble produce, stop to heat.
(3) reacted product is collected, washed repeatedly to chemical attack solution clean fully (wide pH value test paper check flushing distilled water is neutral) with distilled water.Under 25 ℃, dry then and preserve.This nano-porous silver aperture, hole wall size are about 190～210 nanometers, and the continuity of hole wall is further strengthened.
Embodiment three
(1) according to atomic percent 60%Ag, all the other are the proportioning of Al, and the Al-Ag alloy is put into smelting furnace.Alloy is heated to molten condition, makes its alloying through fully stirring.Blow out fast under 0.1MPa pressure with the liquid of nitrogen fusion, Quench on the high speed copper roller rotating, obtaining thickness is 30～60 microns, and width is 2～5 millimeters, and length is 5～30 centimetres alloy thin band.
(2) 25 ℃ down with 37wt.% hydrochloric acid solution reaction 1 hour, then be heated to 90 ℃ of reactions 2 hours to not significantly the reaction bubble produce, stop to heat.
(3) reacted product is collected, washed repeatedly to chemical attack solution clean fully (wide pH value test paper check flushing distilled water is neutral) with distilled water.Under 25 ℃, dry then and preserve.This nano-porous silver hole wall size is about 400～600 nanometers, and whole nano-porous silver band homogeneous, continuous.
Claims (6)
1, a kind of preparation method of nano-porous silver adopts rapid solidification and takes off the method that alloying combines to prepare nano-porous silver, it is characterized in that may further comprise the steps:
(1) pure metallic aluminum, silver are heated to molten state, foundry alloy liquid is fully mixed;
(2) utilize inert gas that alloy liquid is blown out fast, make liquid metal rapid solidification on the high speed copper roller rotating of fusion, prepare alloy strip;
(3) in sour corrosion solution, take off Alloying Treatment; Corrosion process is washed till neutrality with nano-porous silver after finishing in distilled water; At last, sample dries and preserves.
2, the preparation method of nano-porous silver according to claim 1 is characterized in that the inert gas in the step 2 is a kind of of argon gas, nitrogen; Inert gas pressure is 0.05-1MPa.
3, the preparation method of nano-porous silver according to claim 1 is characterized in that acid solution in the step 3 is a kind of in hydrochloric acid, the sulfuric acid solution.
4, according to the preparation method of claim 1 or 3 described nano-porous silvers, it is characterized in that in the step 3 Al-Ag alloy and 0.1～37wt.% hydrochloric acid solution or with the 0.1-98wt.% sulfuric acid solution room temperature to 90 ℃ reaction 1～4 hour.
5, the preparation method of nano-porous silver according to claim 1 is characterized in that the ratio of greater inequality of acid solution is 5wt.% in the step 3; The freezing rate of Al-Ag alloy strip is 10 in the step 2
2～10
6K/s.
6, the preparation method of nano-porous silver according to claim 1, the atom percentage content that it is characterized in that Ag in the Al-Ag alloy is 10-60%, all the other are Al.
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101912970A (en) * | 2010-08-25 | 2010-12-15 | 中南大学 | Method for preparing spherical porous silver powder |
| CN102191400A (en) * | 2011-05-06 | 2011-09-21 | 上海大学 | Dealloying preparation method of nanoporous metal under static magnetic field |
| CN102191399A (en) * | 2011-05-04 | 2011-09-21 | 上海大学 | Dealloying preparation method capable of greatly reducing the size of a nanoporous metal skeleton |
| CN102296349A (en) * | 2011-07-06 | 2011-12-28 | 上海大学 | De-alloying preparation method of nanometer porous metal substrate with surface enhanced Raman scattering activity |
| CN103255441A (en) * | 2013-05-20 | 2013-08-21 | 北京科技大学 | Method for preparing nano porous silver based on Ag-based amorphous alloy |
| CN104372300A (en) * | 2014-11-03 | 2015-02-25 | 济南大学 | Preparation method of thickness-controllable nano-porous metal thin film |
| CN104831197A (en) * | 2015-04-30 | 2015-08-12 | 河北工业大学 | Preparation method for nanometer porous copper silver |
| CN105076206A (en) * | 2014-05-09 | 2015-11-25 | 中国人民解放军63971部队 | Magnetic porous nano silver antibacterial material, preparation method and application |
| CN105420532A (en) * | 2015-11-19 | 2016-03-23 | 辽宁石油化工大学 | Metal-hole antibacterial metallic silver at nanoscale and preparation method of metallic silver |
| CN107012438A (en) * | 2017-04-18 | 2017-08-04 | 电子科技大学 | A kind of preparation method of the reinforced porous silver-colored magnesium alloy film of heat endurance |
| CN107052612A (en) * | 2017-04-25 | 2017-08-18 | 哈尔滨工业大学深圳研究生院 | High-temp solder based on metallic tin filled and process silver and preparation method thereof |
| CN107326209A (en) * | 2017-07-05 | 2017-11-07 | 北京科技大学 | The preparation method of noble metal and magnesium-yttrium-transition metal nano wire and mesh nanometer material |
| CN109860638A (en) * | 2019-01-07 | 2019-06-07 | 湖南大学 | A kind of nanoporous Ag2Al material, preparation method and application |
| CN110306061A (en) * | 2019-08-06 | 2019-10-08 | 攀钢集团研究院有限公司 | The method that vananum prepares vanadium metal |
| CN111347056A (en) * | 2020-03-12 | 2020-06-30 | 东莞理工学院 | Preparation method of nano silver powder |
| CN113186428A (en) * | 2021-04-27 | 2021-07-30 | 安徽工业大学 | Preparation method of layer-pleated nano-porous silver alloy |
| CN113182525A (en) * | 2021-04-27 | 2021-07-30 | 安徽工业大学 | Preparation method of nano porous silver powder |
| WO2021179677A1 (en) * | 2020-03-12 | 2021-09-16 | 赵远云 | Preparation method for powder material and use thereof |
| CN113416974A (en) * | 2021-03-22 | 2021-09-21 | 辽宁石油化工大学 | Method for rapidly preparing efficient porous silver electrocatalyst |
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2009
- 2009-06-19 CN CNA2009100164161A patent/CN101590527A/en active Pending
Cited By (27)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101912970A (en) * | 2010-08-25 | 2010-12-15 | 中南大学 | Method for preparing spherical porous silver powder |
| CN102191399A (en) * | 2011-05-04 | 2011-09-21 | 上海大学 | Dealloying preparation method capable of greatly reducing the size of a nanoporous metal skeleton |
| CN102191400A (en) * | 2011-05-06 | 2011-09-21 | 上海大学 | Dealloying preparation method of nanoporous metal under static magnetic field |
| CN102296349A (en) * | 2011-07-06 | 2011-12-28 | 上海大学 | De-alloying preparation method of nanometer porous metal substrate with surface enhanced Raman scattering activity |
| CN103255441A (en) * | 2013-05-20 | 2013-08-21 | 北京科技大学 | Method for preparing nano porous silver based on Ag-based amorphous alloy |
| CN103255441B (en) * | 2013-05-20 | 2015-06-10 | 北京科技大学 | Method for preparing nano porous silver based on Ag-based amorphous alloy |
| CN105076206A (en) * | 2014-05-09 | 2015-11-25 | 中国人民解放军63971部队 | Magnetic porous nano silver antibacterial material, preparation method and application |
| CN104372300A (en) * | 2014-11-03 | 2015-02-25 | 济南大学 | Preparation method of thickness-controllable nano-porous metal thin film |
| CN104831197A (en) * | 2015-04-30 | 2015-08-12 | 河北工业大学 | Preparation method for nanometer porous copper silver |
| CN104831197B (en) * | 2015-04-30 | 2017-06-16 | 河北工业大学 | A kind of preparation method of nano porous copper silver |
| CN105420532A (en) * | 2015-11-19 | 2016-03-23 | 辽宁石油化工大学 | Metal-hole antibacterial metallic silver at nanoscale and preparation method of metallic silver |
| CN107012438A (en) * | 2017-04-18 | 2017-08-04 | 电子科技大学 | A kind of preparation method of the reinforced porous silver-colored magnesium alloy film of heat endurance |
| CN107052612A (en) * | 2017-04-25 | 2017-08-18 | 哈尔滨工业大学深圳研究生院 | High-temp solder based on metallic tin filled and process silver and preparation method thereof |
| CN107326209B (en) * | 2017-07-05 | 2018-11-27 | 北京科技大学 | The preparation method of noble metal and magnesium-yttrium-transition metal nano wire and mesh nanometer material |
| CN107326209A (en) * | 2017-07-05 | 2017-11-07 | 北京科技大学 | The preparation method of noble metal and magnesium-yttrium-transition metal nano wire and mesh nanometer material |
| CN109860638B (en) * | 2019-01-07 | 2021-12-03 | 湖南大学 | Nano-porous Ag2Al material, preparation method and application |
| CN109860638A (en) * | 2019-01-07 | 2019-06-07 | 湖南大学 | A kind of nanoporous Ag2Al material, preparation method and application |
| CN110306061A (en) * | 2019-08-06 | 2019-10-08 | 攀钢集团研究院有限公司 | The method that vananum prepares vanadium metal |
| WO2021179677A1 (en) * | 2020-03-12 | 2021-09-16 | 赵远云 | Preparation method for powder material and use thereof |
| CN111347056A (en) * | 2020-03-12 | 2020-06-30 | 东莞理工学院 | Preparation method of nano silver powder |
| CN111347056B (en) * | 2020-03-12 | 2022-08-23 | 东莞理工学院 | Preparation method of nano silver powder |
| JP2023510987A (en) * | 2020-03-12 | 2023-03-15 | 遠雲 趙 | Method for preparing powder material and its application |
| JP7550475B2 (en) | 2020-03-12 | 2024-09-13 | 遠雲 趙 | Powder material preparation method and its application |
| CN113416974A (en) * | 2021-03-22 | 2021-09-21 | 辽宁石油化工大学 | Method for rapidly preparing efficient porous silver electrocatalyst |
| CN113186428A (en) * | 2021-04-27 | 2021-07-30 | 安徽工业大学 | Preparation method of layer-pleated nano-porous silver alloy |
| CN113182525A (en) * | 2021-04-27 | 2021-07-30 | 安徽工业大学 | Preparation method of nano porous silver powder |
| CN113182525B (en) * | 2021-04-27 | 2022-07-26 | 安徽工业大学 | Preparation method of nano porous silver powder |
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