CN101498037A - Method for preparing single crystal silver nano-wire by plant biomass reduction - Google Patents
Method for preparing single crystal silver nano-wire by plant biomass reduction Download PDFInfo
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- CN101498037A CN101498037A CNA200910110902XA CN200910110902A CN101498037A CN 101498037 A CN101498037 A CN 101498037A CN A200910110902X A CNA200910110902X A CN A200910110902XA CN 200910110902 A CN200910110902 A CN 200910110902A CN 101498037 A CN101498037 A CN 101498037A
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Abstract
The invention relates to a method of preparing single-crystal and silver-nanometer rice noodles by reducing plant biomass, in particular to a method of preparing one-dimensional nanometer material. The invention provides a method of preparing the single-crystal and silver-nanometer rice noodles by reducing the plant biomass, which has the advantages that the technology is simple, convenient, rapid, economic and environment-friendly and has warm reaction conditions. The method comprises the following steps: adding 0.5g to 4.0g of plant leave dry powder to 50mL of distilled water to be boiled and cooled to a room temperature before being filtered; measuring filtrate to 50mL by the distilled water to obtain a plant leave extracting solution with the concentration of 10-80 g/L; mixing the plant leave extracting solution with a silver nitrate solution with the molar concentration of 0.5-8mmol/L and adding the solution into a water bath table concentrator for an oscillatory reaction so as to obtain a single-crystal and silver-nanometer rice noodle product.
Description
Technical field
The present invention relates to a kind of preparation method of monodimension nanometer material, especially a kind of method of utilizing plant biomass reduction to prepare monocrystal silver nano line.
Background technology
Monodimension nanometer material, as nano wire, nano belt, nanofiber, nanometer rod, nanotube etc., because it has physicochemical property such as unique optics, electricity, magnetics, catalysis, therefore strengthen aspects such as fluorescence spectrum, surface enhanced Raman spectroscopy (SERS), super large-scale integration (ULSC), chemical/biological sensors, nano-probe, nano composite material and have broad application prospects on photoconductive fiber, surface.Integrated and microminiaturized along with photoelectric component, the metal nanometer line with excellent conduction and heat conductivility more and more is subjected to people's attention and attention, and in numerous metals, the conductivity of silver is best, and nano silver wire is also so become hot of research and development.The method for preparing at present nano silver wire is more, mainly contains template preparation method, solution reaction method etc.But above method is in the shortcoming that exists easy contaminate environment, reduction temperature height, cost height, preparation process complexity in varying degrees.For example, patent ZL02159098.2 (solution reaction method) has used chemical reagent such as butyl (tetra) titanate, methyl ethyl diketone, DMF in the process of preparation nano silver wire, not only increased production cost greatly, and can cause certain pollution to environment; The temperature range of patent ZL200510060864.3 (solution reaction method), CN1709791A (solution reaction method), CN101220506A (solution reaction method) preparation nano silver wire is respectively 140～200 ℃, 100～150 ℃, 100～200 ℃, exists the shortcoming that preparation temperature is higher, energy consumption is big; Patent ZL02151277.9 (template preparation method) then exists the shortcoming of preparation were established complexity.People such as Yugang Sun by introducing the Pt nano particle as crystal seed, are protective material with Polyvinylpyrolidone (PVP) (PVP) then, utilize ethylene glycol reduction Silver Nitrate to prepare high quality, high yield nano silver wire [Nano Lett., 2002,2,165.].This is to prepare the comparatively easy method of nano silver wire at present, but this method has following shortcoming: (1) this process has been used the chemical reagent PVP and the ethylene glycol of easy contaminate environment; (2) reduction temperature higher relatively (160 ℃); (3) with expensive Pt nano particle as crystal seed, preparation cost is higher; (4) nano silver wire of gained and on-monocrystalline.
Summary of the invention
The object of the present invention is to provide a kind of technology both simple and efficient, the plant biomass reduction that utilizes of economic again environmental protection, reaction conditions gentleness prepares the method for monocrystal silver nano line.
The present invention includes following steps:
1) 0.5～4.0g leaf dry powder is added 50mL distilled water and boil, be cooled to the room temperature after-filtration, filtrate is settled to 50mL with distilled water, and getting concentration is the leaf extracting solution of 10～80g/L;
2) be that the silver nitrate solution of 0.5～8mmol/L mixes with the leaf extracting solution of step 1) gained and volumetric molar concentration, place the shaking bath oscillatory reaction, the product monocrystal silver nano line.
Described leaf is preferably sausage leaf etc.; Preferably keep 1～10min to be cooled to room temperature again after boiling.
By volume, the leaf extracting solution: silver nitrate solution is preferably 1: 1, and described water-bath is preferably 20～40 ℃ water bath with thermostatic control, and the time of oscillatory reaction is preferably 12～72h in the shaking table.
The length of products therefrom monocrystal silver nano line is generally 0.2～60 μ m, and mean diameter is generally 20～100nm.
Technology of the present invention is simple, need not to add other chemical reagent except that Silver Nitrate, reaction conditions gentleness, the not only simple and efficient but also economic environmental protection of preparation method.The nano silver wire of preparation favorable dispersity, stability in the aqueous solution is high, strengthens in optics, electricity and the materialogy fields such as fluorescence spectrum, surface enhanced Raman spectroscopy being with a wide range of applications on preparation, nano-device assembling, chemical/biological sensors, nano-probe, the surface of conductive and heat-conductive, nano composite material such as antibiotic.
Description of drawings
Fig. 1 is transmission electron microscope (TEM) figure of the nano silver wire of embodiment 1 preparation.In Fig. 1, scale is 0.5 μ m.
Fig. 2 is selected area electron diffraction (SAED) figure of the nano silver wire of embodiment 1 preparation.
Fig. 3 is the TEM figure of the nano silver wire of embodiment 2 preparations.
Fig. 4 is the TEM figure of the nano silver wire of embodiment 3 preparations.
Fig. 5 is the TEM figure of the nano silver wire of embodiment 4 preparations.In Fig. 5, scale is 1 μ m.
Fig. 6 is the TEM figure of the nano silver wire of embodiment 5 preparations.In Fig. 6, scale is 500nm.
Embodiment
The invention will be further described below by embodiment.
Accurately take by weighing the ground sausage leaf dried powder of 2.0g, add 50mL distilled water and boil back maintenance 5min, liquid to be boiled is cooled to the room temperature after-filtration, and filtrate is settled to 50mL with distilled water, and getting concentration is the sausage leaf extract of 40g/L; The silver nitrate solution of getting this extracting solution of 25mL and 25mL, volumetric molar concentration and be 2mmol/L mixes, and places water bath with thermostatic control shaking table (30 ℃, 150rpm) oscillatory reaction 24h, get final product length 0.5～15 μ m, the nano silver wire of mean diameter 52.7nm.Fig. 1 provides the TEM picture of the nano silver wire of present embodiment preparation, and the generation of nano silver wire is as can be seen from Figure 1 arranged.Fig. 2 provides the SAED picture of the nano silver wire of present embodiment preparation, and as can be seen from Figure 2 diffraction pattern is regularly arranged spot, thereby the nano silver wire of proof gained is a monocrystalline.
Embodiment 2
Accurately take by weighing the ground sausage leaf dried powder of 2.0g, add 50mL distilled water and boil back maintenance 5min, liquid to be boiled is cooled to the room temperature after-filtration, and filtrate is settled to 50mL with distilled water, and getting concentration is the sausage leaf extract of 40g/L; The silver nitrate solution of getting this extracting solution of 50mL and 50mL, volumetric molar concentration and be 2mmol/L mixes, and places water bath with thermostatic control shaking table (30 ℃, 150rpm) oscillatory reaction 48h, get final product length 0.5～30 μ m, the nano silver wire of mean diameter 85.4nm.Fig. 3 is the TEM picture of the nano silver wire of present embodiment preparation, the as can be seen from Figure 3 generation of many nano silver wires.
Embodiment 3
Accurately take by weighing the ground sausage leaf dried powder of 2.0g, add 50mL distilled water and boil back maintenance 5min, liquid to be boiled is cooled to the room temperature after-filtration, and filtrate is settled to 50mL with distilled water, and getting concentration is the sausage leaf extract of 40g/L; The silver nitrate solution of getting this extracting solution of 25mL and 25mL, volumetric molar concentration and be 3mmol/L mixes, and places water bath with thermostatic control shaking table (30 ℃, 150rpm) oscillatory reaction 52h, get final product length 0.3～60 μ m, the nano silver wire of mean diameter 67.6nm.Fig. 4 is the TEM picture of the nano silver wire of present embodiment preparation, the as can be seen from Figure 4 generation of a large amount of nano silver wires.
Embodiment 4
Accurately take by weighing the ground sausage leaf dried powder of 4.0g, add 50mL distilled water and boil back maintenance 10min, liquid to be boiled is cooled to the room temperature after-filtration, and filtrate is settled to 50mL with distilled water, and getting concentration is the sausage leaf extract of 80g/L; The silver nitrate solution of getting this extracting solution of 25mL and 25mL, volumetric molar concentration and be 8mmol/L mixes, and places water bath with thermostatic control shaking table (20 ℃, 150rpm) oscillatory reaction 72h, get final product length 0.5～20 μ m, mean diameter is the nano silver wire of 50.6nm.Fig. 5 as can be seen from Figure 5 has the generation of nano silver wire for the TEM picture of the nano silver wire of present embodiment preparation.
Embodiment 5
Accurately take by weighing the ground sausage leaf dried powder of 0.5g, add 50mL distilled water and boil back maintenance 1min, liquid to be boiled is cooled to the room temperature after-filtration, and filtrate is settled to 50mL with distilled water, and getting concentration is the sausage leaf extract of 10g/L; The silver nitrate solution of getting this extracting solution of 25mL and 25mL, volumetric molar concentration and be 0.5mmol/L mixes, and places water bath with thermostatic control shaking table (40 ℃, 150rpm) oscillatory reaction 12h, get final product length 0.3～12 μ m, the nano silver wire of mean diameter 42.4nm.Fig. 6 as can be seen from Figure 6 has the generation of nano silver wire for the TEM picture of the nano silver wire of present embodiment preparation.
Claims (6)
1. method of utilizing plant biomass reduction to prepare monocrystal silver nano line is characterized in that may further comprise the steps:
1) 0.5～4.0g leaf dry powder is added 50mL distilled water and boil, be cooled to the room temperature after-filtration, filtrate is settled to 50mL with distilled water, and getting concentration is the leaf extracting solution of 10～80g/L;
2) be that the silver nitrate solution of 0.5～8mmol/L mixes with the leaf extracting solution of step 1) gained and volumetric molar concentration, place the shaking bath oscillatory reaction, the product monocrystal silver nano line.
2. a kind of method of utilizing plant biomass reduction to prepare monocrystal silver nano line as claimed in claim 1 is characterized in that described leaf is the sausage leaf.
3. a kind of method of utilizing plant biomass reduction to prepare monocrystal silver nano line as claimed in claim 1 is characterized in that boiling the back and keeps 1～10min to be cooled to room temperature again.
4. a kind of method of utilizing plant biomass reduction to prepare monocrystal silver nano line as claimed in claim 1 is characterized in that by volume the leaf extracting solution: silver nitrate solution is 1: 1.
5. a kind of method of utilizing plant biomass reduction to prepare monocrystal silver nano line as claimed in claim 1 is characterized in that described water-bath is 20～40 ℃ water bath with thermostatic control.
6. a kind of method of utilizing plant biomass reduction to prepare monocrystal silver nano line as claimed in claim 1, the time that it is characterized in that oscillatory reaction in the shaking table is 12～72h.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101912976A (en) * | 2010-08-24 | 2010-12-15 | 厦门大学 | Method for preparing silver nano granules by reducing plant extract |
| CN103192091A (en) * | 2013-04-23 | 2013-07-10 | 湖南农业大学 | Method utilizing sloanea sinensis leaves for green synthesis of water-soluble nano-iron |
| CN103702785A (en) * | 2011-07-12 | 2014-04-02 | 于伽·纳拉杨·本德勒 | Novel nano gold and process for preparation |
| CN104148669A (en) * | 2014-08-29 | 2014-11-19 | 厦门大学 | Method for preparing bi-metal nanometer wire |
| CN105665737A (en) * | 2016-01-27 | 2016-06-15 | 陕西科技大学 | Biosynthesis method of nano Ag |
| CN105817643A (en) * | 2016-05-06 | 2016-08-03 | 东北师范大学 | Method for preparing nano particles from waste generated after extraction of saponin from ginseng |
| CN106513707A (en) * | 2016-12-07 | 2017-03-22 | 鲁东大学 | Nano silver bacteriostatic agent biosynthesized through blueberry leaf extracting solution and preparation process of nano silver bacteriostatic agent |
| CN106862590A (en) * | 2017-02-24 | 2017-06-20 | 华中农业大学 | A kind of method of utilization Guangxi Du chaste tree blade extract biosynthesis Nano Silver |
| CN107309438A (en) * | 2017-07-14 | 2017-11-03 | 福建农林大学 | A kind of method that polysaccharide from Phyllanthus Emblica L prepares Nano Silver compound particle |
| CN109550974A (en) * | 2018-12-13 | 2019-04-02 | 华南理工大学 | A kind of preparation method using carnosic acid green syt nano silver |
| CN109909512A (en) * | 2017-12-12 | 2019-06-21 | 中国科学院深圳先进技术研究院 | A kind of silver nanowires and its green magnanimity preparation method |
| CN112705728A (en) * | 2021-01-18 | 2021-04-27 | 山西大同大学 | Green preparation method of silver nanorods |
| CN114505489A (en) * | 2020-10-27 | 2022-05-17 | 深圳市华科创智技术有限公司 | Preparation method of silver nanowires |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1203949C (en) * | 2002-12-31 | 2005-06-01 | 中国科学院上海光学精密机械研究所 | Method for synthesizing single crystal silver nano-wire |
| CN1709791A (en) * | 2005-07-05 | 2005-12-21 | 华东理工大学 | Method for preparing silver nano line |
| CN100450677C (en) * | 2006-11-28 | 2009-01-14 | 厦门大学 | Plant reduction method for preparing silver Nano granules and gold Nano granules |
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2009
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101912976A (en) * | 2010-08-24 | 2010-12-15 | 厦门大学 | Method for preparing silver nano granules by reducing plant extract |
| CN103702785A (en) * | 2011-07-12 | 2014-04-02 | 于伽·纳拉杨·本德勒 | Novel nano gold and process for preparation |
| CN103192091A (en) * | 2013-04-23 | 2013-07-10 | 湖南农业大学 | Method utilizing sloanea sinensis leaves for green synthesis of water-soluble nano-iron |
| CN103192091B (en) * | 2013-04-23 | 2015-04-08 | 湖南农业大学 | Method utilizing sloanea sinensis leaves for green synthesis of water-soluble nano-iron |
| CN104148669A (en) * | 2014-08-29 | 2014-11-19 | 厦门大学 | Method for preparing bi-metal nanometer wire |
| CN105665737A (en) * | 2016-01-27 | 2016-06-15 | 陕西科技大学 | Biosynthesis method of nano Ag |
| CN105817643A (en) * | 2016-05-06 | 2016-08-03 | 东北师范大学 | Method for preparing nano particles from waste generated after extraction of saponin from ginseng |
| CN105817643B (en) * | 2016-05-06 | 2019-02-19 | 东北师范大学 | A method of waste prepares nanoparticle after extracting saponin using ginseng |
| CN106513707B (en) * | 2016-12-07 | 2018-06-08 | 鲁东大学 | A kind of nano silver antibacterial agent and its preparation process using blueberry leaf extract biosynthesis |
| CN106513707A (en) * | 2016-12-07 | 2017-03-22 | 鲁东大学 | Nano silver bacteriostatic agent biosynthesized through blueberry leaf extracting solution and preparation process of nano silver bacteriostatic agent |
| CN106862590A (en) * | 2017-02-24 | 2017-06-20 | 华中农业大学 | A kind of method of utilization Guangxi Du chaste tree blade extract biosynthesis Nano Silver |
| CN107309438A (en) * | 2017-07-14 | 2017-11-03 | 福建农林大学 | A kind of method that polysaccharide from Phyllanthus Emblica L prepares Nano Silver compound particle |
| CN109909512A (en) * | 2017-12-12 | 2019-06-21 | 中国科学院深圳先进技术研究院 | A kind of silver nanowires and its green magnanimity preparation method |
| CN109550974A (en) * | 2018-12-13 | 2019-04-02 | 华南理工大学 | A kind of preparation method using carnosic acid green syt nano silver |
| CN114505489A (en) * | 2020-10-27 | 2022-05-17 | 深圳市华科创智技术有限公司 | Preparation method of silver nanowires |
| CN112705728A (en) * | 2021-01-18 | 2021-04-27 | 山西大同大学 | Green preparation method of silver nanorods |
| CN112705728B (en) * | 2021-01-18 | 2023-05-23 | 山西大同大学 | Green preparation method of silver nanorods |
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