CN104014807A - Silver nanocrystalline preparation method with surface raman enhancing effect - Google Patents
Silver nanocrystalline preparation method with surface raman enhancing effect Download PDFInfo
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- CN104014807A CN104014807A CN201410230477.9A CN201410230477A CN104014807A CN 104014807 A CN104014807 A CN 104014807A CN 201410230477 A CN201410230477 A CN 201410230477A CN 104014807 A CN104014807 A CN 104014807A
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Abstract
The invention relates to a silver nanocrystalline chemical preparation method with a surface raman enhancing effect. The method includes the steps of dissolving polyvinylpyrrolidone in deionized water to prepare a water solution, adding strong alkali and a glucose solution to the water solution, fully stirring the mixture so as to evenly disperse the strong alkali and the glucose solution, dropwise adding a silver nitrate water solution to the mixture, moving reaction liquid into a reaction kettle to react, and washing and drying the reaction product so as to obtain solver nanometer sol. According to the method, raw materials are cheap; the method is environmentally friendly; silver nanocrystalline particles in the uniform size can be obtained, and the nanometer particles have the remarkable raman enhancing effect on PVP and pyridine.
Description
Technical field
The invention belongs to material chemistry technical field, relate to a kind of preparation method with the silver nanoparticle crystalline substance of surface Raman enhancement effect.
Background technology
Compare with body material, metal nanoparticle has the physics and chemistry character of many uniquenesses, wherein the most noticeable is exactly the surface plasma resonance characteristic of metallic nano crystal, based on surface plasma resonance effect, metallic nano crystal has been widely used in the aspects such as bio-sensing and surface Raman enhancement.Wherein SERS (SERS), as a kind of species analysis technology, can reach overdelicate detection in the fields such as analysis, environment and catalysis.It is active that alkali metal, noble metal and part transition metal have good surface Raman enhancement, and wherein the enhancing effect of silver nanoparticle crystalline substance is best, and gold and copper take second place.Because substrate is unstable, poor effects limit such as repeatability the business application of SERS.Preparation size is even, and shape is controlled, high stability, repeatable strong SERS active substrate are the primary goals that Raman strengthens research.Silver sol is current most widely used active substrate, and its preparation method is simple, has plasma resonance to absorb in visible region, and size and shape ratio is easier to control.The conventional method of synthetic silver nano-grain is to prepare in organic solvent, solvent organic molecule strengthens in test and can have a certain impact at follow-up Raman, so thereby being necessary to find a kind of method eco-friendly, that the aqueous solution is prepared silver nanoparticle colloidal sol facilitates follow-up Raman to strengthen test.
Summary of the invention
For overcoming the deficiencies in the prior art, the invention provides a kind of preparation method with the silver nanoparticle crystalline substance of surface Raman enhancement effect.
A preparation method with the silver nanoparticle crystalline substance of surface Raman enhancement effect, is characterized in that, comprises the following steps:
(1) 0.5～1.5 gram of polyvinylpyrrolidone is dissolved in the deionized water of 15～25 milliliters, is mixed with the polyvinylpyrrolidone aqueous solution;
(2) in above-mentioned solution, adding 5～15 ml concns is the sodium hydroxide solution of 0.05～0.15mol/L and 5～15 milliliters, and the glucose solution of 0.1～0.3mol/L, fully stirs and make to be uniformly dispersed with glass bar;
(3) in solution, drip liquor argenti nitratis ophthalmicus again;
(4) reactant liquor is moved to reaction kettle for reaction;
(5) product obtains silver nanoparticle colloidal sol through washing and drying;
(6) silver nanoparticle colloidal sol uniform load, on slide, strengthens test for follow-up Raman.
Liquor argenti nitratis ophthalmicus concentration described in step (3) is 0.04～0.05mol/L, adds 15～25 milliliters, slowly splashes into can observe solution after liquor argenti nitratis ophthalmicus and become immediately black gray expandable.
Temperature in reactor described in step (4) is 130～150 ℃, and the reaction time is 5～7 hours.
Washing and drying described in step (5), for adding deionized water high speed centrifugation, repeats 3 ~ 4 times; Dry as to heat at 350～450 ℃ 1 hour under vacuum condition.
The present invention has synthesized the silver nanoparticle crystalline substance of the uniform-dimension of 50 nanometer left and right in aqueous systems, and the method is easy and simple to handle, nontoxic, favorable repeatability, with low cost.Raw material of the present invention is cheap, and technique is simple, can prepare the silver nanoparticle colloidal sol of size uniform, and the structure and morphology of material is controlled stable, and the Raman of pyridine and PVP is strengthened to successful.
Accompanying drawing explanation
Fig. 1 is for adopting the electron scanning micrograph of the synthetic silver nanoparticle crystalline substance of the present invention (embodiment 1).
Fig. 2 is for adopting the Raman enhancement effect of the synthetic silver nanoparticle crystalline substance of the present invention (embodiment 1) to PVP, and wherein 1 is the Raman collection of illustrative plates of PVP, and the 2nd, PVP is at the Raman collection of illustrative plates on the brilliant surface of silver nanoparticle.
Fig. 3 is for adopting the Raman enhancement effect of the synthetic silver nanoparticle crystalline substance of the present invention (embodiment 1) to pyridine, and wherein 1 is the Raman collection of illustrative plates of pyridine, and the 2nd, pyridine is at the Raman collection of illustrative plates on the brilliant surface of silver nanoparticle.
The specific embodiment
Embodiment 1:
The synthetic method of silver nanoparticle colloidal sol
First 1.0g PVP is dissolved in the deionized water of 20ml; In above-mentioned solution, add successively 10ml, NaOH solution and the 10ml of 0.1mol/L, the glucose solution of 0.2mol/L, stirs with glass bar; Add 20ml, the liquor argenti nitratis ophthalmicus of 0.05mol/L, can observe solution and become immediately black gray expandable; Above-mentioned reactant liquor is added in the reactor of 100ml to 140 ℃ of reaction 6h.Product is added after the centrifugal 10min of deionized water 10000r, remove supernatant, continue to add pure deionized water to continue centrifugal, repeat this process 3 ~ 4 times; By the powder sample obtaining 400 ℃ of annealing 1h under vacuum condition.Powder sample is loaded on slide uniformly, drip certain density PVP and pyridine solution, it is carried out to the test of Raman enhancement effect.
Fig. 1 shows that synthetic size is at the silver nanoparticle colloidal sol of 50nm; Fig. 2 shows the Raman enhancement effect that synthetic silver nanoparticle crystalline substance is good to PVP, and wherein 1 is the Raman collection of illustrative plates of PVP, and the 2nd, PVP is at the Raman collection of illustrative plates on the brilliant surface of silver nanoparticle; Fig. 3 shows the Raman enhancement effect that synthetic silver nanoparticle crystalline substance is good to pyridine, and wherein 1 is the Raman collection of illustrative plates of pyridine, the 2nd, and pyridine is at the Raman collection of illustrative plates on the brilliant surface of silver nanoparticle.
Embodiment 2:
First 0.5g PVP is dissolved in the deionized water of 20ml; In above-mentioned solution, add successively 5ml, NaOH solution and the 5ml of 0.1mol/L, the glucose solution of 0.2mol/L, stirs with glass bar; Add 20ml, the liquor argenti nitratis ophthalmicus of 0.05mol/L, can observe solution and become immediately black gray expandable; Above-mentioned reactant liquor is added in the reactor of 100ml to 150 ℃ of reaction 6h.Product is added after the centrifugal 10min of deionized water 10000r, remove supernatant, continue to add pure deionized water to continue centrifugal, repeat this process 3 ~ 4 times; By the powder sample obtaining 350 ℃ of annealing 1h under vacuum condition.Powder sample is loaded on slide uniformly, drip certain density PVP and pyridine solution, it is carried out to the test of Raman enhancement effect.Prepared nanoparticle size, in 40 nanometer left and right, all has certain humidification to PVP and pyridine.
Embodiment 3:
First 1.5g PVP is dissolved in the deionized water of 20ml; In above-mentioned solution, add successively 15ml, NaOH solution and the 15ml of 0.1mol/L, the glucose solution of 0.2mol/L, stirs with glass bar; Add 20ml, the liquor argenti nitratis ophthalmicus of 0.05mol/L, can observe solution and become immediately black gray expandable; Above-mentioned reactant liquor is added in the reactor of 100ml to 130 ℃ of reaction 6h.Product is added after the centrifugal 10min of deionized water 10000r, remove supernatant, continue to add pure deionized water to continue centrifugal, repeat this process 3 ~ 4 times; By the powder sample obtaining 450 ℃ of annealing 1h under vacuum condition.Powder sample is loaded on slide uniformly, drip certain density PVP and pyridine solution, it is carried out to the test of Raman enhancement effect.Prepared nanoparticle size, in 60 nanometer left and right, all has certain humidification to PVP and pyridine.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.Person skilled in the art obviously can easily make various modifications to these embodiment, and General Principle described herein is applied in other embodiment and needn't passes through performing creative labour.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and the improvement of making for the present invention and modification all should be within protection scope of the present invention.
Claims (4)
1. a preparation method with the silver nanoparticle crystalline substance of surface Raman enhancement effect, is characterized in that, comprises the following steps:
(1) 0.5～1.5 gram of polyvinylpyrrolidone is dissolved in the deionized water of 15～25 milliliters, is mixed with the polyvinylpyrrolidone aqueous solution;
(2) in above-mentioned solution, adding 5～15 ml concns is the sodium hydroxide solution of 0.05～0.15mol/L and 5～15 milliliters, and the glucose solution of 0.1～0.3mol/L, fully stirs and make to be uniformly dispersed with glass bar;
(3) in solution, drip liquor argenti nitratis ophthalmicus again;
(4) reactant liquor is moved to reaction kettle for reaction;
(5) product obtains silver nanoparticle colloidal sol through washing and drying;
(6) silver nanoparticle colloidal sol uniform load, on slide, strengthens test for follow-up Raman.
2. the preparation method according to claim 1 with the silver nanoparticle crystalline substance of surface Raman enhancement effect, it is characterized in that, liquor argenti nitratis ophthalmicus concentration described in step (3) is 0.04～0.05mol/L, add 15～25 milliliters, slowly splash into and can observe solution after liquor argenti nitratis ophthalmicus and become immediately black gray expandable.
3. the preparation method according to claim 1 with the silver nanoparticle crystalline substance of surface Raman enhancement effect, is characterized in that, the temperature in the reactor described in step (4) is 130～150 ℃, and the reaction time is 5～7 hours.
4. the preparation method according to claim 1 with the silver nanoparticle crystalline substance of surface Raman enhancement effect, is characterized in that, the washing and drying described in step (5), for adding deionized water high speed centrifugation, repeats 3 ~ 4 times; Dry as to heat at 350～450 ℃ 1 hour under vacuum condition.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106248650A (en) * | 2016-08-22 | 2016-12-21 | 上海朗研光电科技有限公司 | Simple and effective Raman strengthens the preparation method of substrate |
| CN106853523A (en) * | 2016-12-29 | 2017-06-16 | 山东大学 | A kind of how dendritic gold and silver composite nano materials with excellent surface enhancing Raman scattering characteristic and preparation method thereof |
| CN107127352A (en) * | 2017-05-04 | 2017-09-05 | 温州大学 | A kind of preparation method of the nano silver wire of one-step synthesis at room temperature |
| CN107322005A (en) * | 2017-06-20 | 2017-11-07 | 北京大学 | A kind of SERS substrate fabrication method based on nano-Ag particles |
| CN107775013A (en) * | 2017-10-26 | 2018-03-09 | 中国科学技术大学 | Ag is nanocrystalline, its preparation method and its application |
| CN107838435A (en) * | 2017-11-16 | 2018-03-27 | 中国计量大学 | A kind of preparation method of the silver nano flower-like with surface Raman enhancement effect |
| CN110449595A (en) * | 2019-07-11 | 2019-11-15 | 四川大学 | The method and hydrophobicity gold, silver nano particle of step preparation hydrophobicity gold, silver nano particle in a kind of aqueous solution |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1583332A (en) * | 2004-06-08 | 2005-02-23 | 陈丽琼 | Nanometer silver sol and preparing method thereof |
| CN1653907A (en) * | 2005-01-27 | 2005-08-17 | 浙江大学 | Method for preparing nanometer silver solution and nanometer silver powder by using high polymer as stabilizer |
| US20070056402A1 (en) * | 2005-09-14 | 2007-03-15 | Samsung Electro-Machanics Co. Ltd. | Metal nanoparticles and method for manufacturing thereof |
| CN102133645A (en) * | 2011-03-04 | 2011-07-27 | 华南理工大学 | Preparation method of environment-friendly micron-size triangular silver sheet |
| CN102198512A (en) * | 2011-05-13 | 2011-09-28 | 同济大学 | Method for preparing nano silver dispersed by glucose reduction complexing agent |
| CN102197826A (en) * | 2010-03-25 | 2011-09-28 | 上海亿金纳米科技有限公司 | Novel large-scale method for preparing alkalescent nano-silver solution |
| US20130008287A1 (en) * | 2011-07-08 | 2013-01-10 | Benq Materials Corporation | Method for preparing nano silver particles |
-
2014
- 2014-05-28 CN CN201410230477.9A patent/CN104014807A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1583332A (en) * | 2004-06-08 | 2005-02-23 | 陈丽琼 | Nanometer silver sol and preparing method thereof |
| CN1653907A (en) * | 2005-01-27 | 2005-08-17 | 浙江大学 | Method for preparing nanometer silver solution and nanometer silver powder by using high polymer as stabilizer |
| US20070056402A1 (en) * | 2005-09-14 | 2007-03-15 | Samsung Electro-Machanics Co. Ltd. | Metal nanoparticles and method for manufacturing thereof |
| CN102197826A (en) * | 2010-03-25 | 2011-09-28 | 上海亿金纳米科技有限公司 | Novel large-scale method for preparing alkalescent nano-silver solution |
| CN102133645A (en) * | 2011-03-04 | 2011-07-27 | 华南理工大学 | Preparation method of environment-friendly micron-size triangular silver sheet |
| CN102198512A (en) * | 2011-05-13 | 2011-09-28 | 同济大学 | Method for preparing nano silver dispersed by glucose reduction complexing agent |
| US20130008287A1 (en) * | 2011-07-08 | 2013-01-10 | Benq Materials Corporation | Method for preparing nano silver particles |
Non-Patent Citations (1)
| Title |
|---|
| 刘艳娥等: "水热法制备球形纳米银粒子及其表征", 《材料导报》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106248650A (en) * | 2016-08-22 | 2016-12-21 | 上海朗研光电科技有限公司 | Simple and effective Raman strengthens the preparation method of substrate |
| CN106853523A (en) * | 2016-12-29 | 2017-06-16 | 山东大学 | A kind of how dendritic gold and silver composite nano materials with excellent surface enhancing Raman scattering characteristic and preparation method thereof |
| CN106853523B (en) * | 2016-12-29 | 2019-01-22 | 山东大学 | A kind of preparation method of the racemosus shape gold and silver composite nano materials with Surface enhanced Raman scattering characteristic |
| CN107127352A (en) * | 2017-05-04 | 2017-09-05 | 温州大学 | A kind of preparation method of the nano silver wire of one-step synthesis at room temperature |
| CN107322005A (en) * | 2017-06-20 | 2017-11-07 | 北京大学 | A kind of SERS substrate fabrication method based on nano-Ag particles |
| CN107775013A (en) * | 2017-10-26 | 2018-03-09 | 中国科学技术大学 | Ag is nanocrystalline, its preparation method and its application |
| CN107775013B (en) * | 2017-10-26 | 2020-01-03 | 中国科学技术大学 | Ag nanocrystal, preparation method and application thereof |
| CN107838435A (en) * | 2017-11-16 | 2018-03-27 | 中国计量大学 | A kind of preparation method of the silver nano flower-like with surface Raman enhancement effect |
| CN110449595A (en) * | 2019-07-11 | 2019-11-15 | 四川大学 | The method and hydrophobicity gold, silver nano particle of step preparation hydrophobicity gold, silver nano particle in a kind of aqueous solution |
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Application publication date: 20140903 |