CN103769601A - Preparing method of triangular flaky nanometer silver particles - Google Patents
Preparing method of triangular flaky nanometer silver particles Download PDFInfo
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- CN103769601A CN103769601A CN201410029136.5A CN201410029136A CN103769601A CN 103769601 A CN103769601 A CN 103769601A CN 201410029136 A CN201410029136 A CN 201410029136A CN 103769601 A CN103769601 A CN 103769601A
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Abstract
The invention relates to a preparing method of triangular flaky nanometer silver particles. The preparing method comprises the following steps that S1, silver trifluoroacetate, PVP (polyvinyl pyrrolidone) and phenylcarbinol are placed into a reaction kettle and are mixed, and a mixture is obtained after the materials are uniformly stirred; S2, metal salts are added into the mixture, and settled solution is obtained through stirring at room temperature; S3, the settled solution is heated to 120 to 150 DEG C in the reaction kettle, the reaction lasts a period of time, and a reaction product is obtained; S4, reaction products are subjected to centrifugal separation and are washed, and then, the triangular flaky nanometer silver particles are obtained. The preparing method provided by the invention has the advantages that the process is simple and convenient, the cost is low, and the preparing method is suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of preparation method of triangle sheet nano-Ag particles.
Background technology
Triangle sheet nano-Ag particles is a kind of leg-of-mutton flake nano structure, it is as a kind of special anisotropic structure, there is unique optical property, its surface plasma body resonant vibration (surface plasmon resonance, SPR) absorption spectrum has four utmost points and the strong interior bipolar SPR of face peak in outer four utmost points of weak face, face, is widely used in the aspects such as SERS (SERS) detection, near-field optical probe, biology sensor.So far, the synthetic method of reported in literature has template, electrochemical synthesis, photo-induction inducing defecation by enema and suppository and chemical reduction method, wherein, conventional with chemical direct-reduction process.In the preparation method who has reported, comparatively easy with two reducing process, this method carries out under water bath condition, using hydrogen peroxide as oxidant, uses sodium borohydride, trisodium citrate to reduce to silver nitrate.But there is the defect that output is lower and can not produce in enormous quantities in the method.
Summary of the invention
In view of this, provide the preparation method of triangle sheet nano-Ag particles of the low and applicable large-scale production of a kind of simple process, cost real in necessary.
A preparation method for triangle sheet nano-Ag particles, it comprises: S1: trifluoroacetic acid silver, polyvinylpyrrolidone (PVP) and phenmethylol are placed in a reactor and are mixed, after stirring, obtain a mixture; S2: add slaine in described mixture, at room temperature stir and obtain settled solution; S3: described settled solution is heated to 120～150 degrees Celsius in reactor, and reaction a period of time obtains a product; And S4: will obtain triangle sheet nano-Ag particles after described product centrifugation and washing.
Compared to prior art, the preparation method of triangle sheet nano-Ag particles provided by the present invention adopts slaine to regulate and control the output of triangle sheet nano-Ag particles, can obtain high yield.And in reaction, use phenmethylol simultaneously as solvent and reducing agent, simple to operate, be applicable to large-scale production.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of the triangle sheet nano-Ag particles that obtains in first embodiment of the invention.
Fig. 2 is the front transmission electron microscope picture of the triangle sheet triangular plate shape nano-Ag particles in Fig. 1.
Fig. 3 is the side transmission electron microscope picture of the triangle sheet triangular plate shape nano-Ag particles in Fig. 2.
Fig. 4 is the electron diffraction diagram of the triangle sheet triangular plate shape nano-Ag particles in Fig. 2.
The specific embodiment
Describe the preparation method of embodiment of the present invention triangle sheet nano-Ag particles in detail below with reference to accompanying drawing.
Refer to Fig. 1, the invention provides a kind of preparation method of triangle sheet nano-Ag particles, it comprises the following steps:
S1: trifluoroacetic acid silver, polyvinylpyrrolidone (PVP) and phenmethylol are placed in a reactor and are mixed, obtain a mixture after stirring;
S2: add slaine in described mixture, at room temperature stir and obtain settled solution;
S3: described settled solution is heated to 120～150 degrees Celsius in reactor, and reaction a period of time obtains a product; And
S4: will obtain triangle sheet nano-Ag particles after described product centrifugation and washing.
In step S1, the quality of described trifluoroacetic acid silver is 19～20 milligrams.Described PVP molecular weight is 10000 left and right, and its quality is 0.04～0.06 gram.Described phenmethylol is 4～6 milliliters.In the present embodiment, preferably, the quality of described trifluoroacetic acid silver is 20 milligrams, 0.09 mM; The quality of described PVP is 50 milligrams; Described phenmethylol is 5 milliliters.The time that described mixture is stirred is 10～20 minutes, is preferably 15 minutes.Agitating mode to described mixture is not limit, and is chosen as magneton and stirs, after putting into reactor by stirring magneton, as for stirring on magnetic stirring apparatus.The specification of described reactor is relevant with the amount of mixture, and in the present embodiment, the specification of reactor is 12 milliliters.
In step S2, described slaine is at least one in molysite and aluminium salt.That is, in step S2, can only add a kind of slaine, also can add two kinds of slaines simultaneously.As, can only add molysite or aluminium salt, also can add molysite and aluminium salt simultaneously.In the time adding molysite and aluminium salt, the mol ratio of molysite and aluminium salt is 1:2～2:1 simultaneously.Described molysite is the soluble-salt of iron, can be ferric nitrate or ferric sulfate.The soluble-salt that described aluminium salt is aluminium can be aluminum nitrate or aluminum sulfate.The amount of the molysite adding or aluminium salt is 0.002～0.01 mM, is preferably 0.0025～0.005 mM.In the present embodiment, preferably, add ferric nitrate and aluminum nitrate simultaneously.Add molysite or/and continue after aluminium salt to stir, until obtain the solution of clarification.
In step S3, after reactor is covered, put into heating furnace and heat, when temperature reaches after 120～150 degrees Celsius, be incubated 4～6 hours, make to react and obtain product between the material in reactor.
In step S4, product is placed in to centrifuge tube, put into centrifuge and carry out centrifugation.The rotating speed of centrifuge is 10000 revs/min.After centrifugation, pour out centrifuge tube clear liquid at the middle and upper levels, be precipitated thing.Use ethanol and deionized water to wash successively sediment, adopt ethanol or deionized water and sediment after centrifuge separating, washing when washing, centrifugal speed is 10000 revs/min.Through repeatedly washing, after centrifugation, obtain triangle sheet nano-Ag particles.
The productive rate of the change of reaction condition to product pattern and triangle sheet nano-Ag particles etc. has considerable influence.With specific embodiment, the present invention is further described below:
Embodiment 1:
The preparation method of the triangle sheet nano-Ag particles of the present embodiment has following steps:
Step 1, by the polyvinylpyrrolidone of the trifluoroacetic acid silver of 0.09mmol and 0.05g (PVP, molecular weight M
w≈ 10,000) be dissolved in the phenmethylol of 5 milliliters, at room temperature stir 10 minutes, now solution is colourless;
Step 2, the ferric nitrate of the aluminum nitrate of 0.0025mmol and 0.0025mmol is joined in the mixed system of above-mentioned steps one, continue to be stirred to aluminum nitrate and dissolve completely;
Step 3: the reactant liquor that step 2 is obtained is placed in reactor, in insulating box, 120 degrees Celsius of reactions obtained product after 6 hours.
Step 4: after adding washing through centrifugation, obtain end product.
Refer to Fig. 1, the product major part that the present embodiment is prepared into is the triangle sheet nano-Ag particles of 100 nanometer ~ 200 nanometers, contains part spheroidal particle simultaneously.The content of product intermediate cam flake nano silver particle is higher.Refer to Fig. 2 and Fig. 3, triangle sheet nano-Ag particles can be regular triangle sheet structure, and its length of side is approximately 150 nanometers, and thickness is 80 nanometer left and right.Fig. 4 is the electron diffraction diagram of triangle sheet nano-Ag particles.
Embodiment 2:
The preparation method's of the present embodiment triangular nano silver particle remainder is identical with embodiment 1, and difference is: the slaine adding in step 2 is aluminum nitrate, and its mole is 0.0025mmol.Product is the triangle sheet triangular plate shape nano-Ag particles of 100 nanometer ~ 200 nanometers, contains part spheroidal particle simultaneously, and the productive rate of product intermediate cam flake nano silver particle is lower than embodiment 1.
Embodiment 3:
The preparation method's of the triangle sheet nano-Ag particles of the present embodiment remainder is identical with embodiment 1, and difference is: the slaine adding in step 2 is aluminum nitrate, and its mole is 0.005mmol.The product finally obtaining is the triangle sheet nano-Ag particles of 100 nanometer ~ 200 nanometers, and the productive rate of product intermediate cam flake nano silver particle is 70% left and right.
Embodiment 4:
The preparation method's of the triangle sheet nano-Ag particles of the present embodiment remainder is identical with embodiment 1, and difference is: the slaine adding in step 2 is aluminum sulfate, and mole is 0.0025mmol.The product finally obtaining is the triangle triangle sheet nano-Ag particles of 100 nanometer ~ 200 nanometers, and sheet productive rate is lower, is only 10% left and right, contains a large amount of spheric granules in product.
Embodiment 5:
The preparation method's of the triangle sheet nano-Ag particles of the present embodiment remainder is identical with embodiment 1, and difference is: the slaine adding in step 2 is ferric nitrate, and its mole is 0.0025mmol.The product finally obtaining is the triangle sheet nano-Ag particles of 100 nanometer ~ 300 nanometers, and the obtuse angle of some triangle sheet nano-Ag particles is larger.The productive rate of product intermediate cam flake nano silver particle is 40% left and right.
Embodiment 6:
The preparation method's of the triangle sheet nano-Ag particles of the present embodiment remainder is identical with embodiment 1, and difference is: the slaine adding in step 2 is ferric sulfate, and its mole is 0.0025mmol.The product finally obtaining is the triangle sheet nano-Ag particles of 100 nanometer ~ 300 nanometers, and its laminated structure obtuse angle is larger.In product, the productive rate of laminated structure is 10% left and right.
As can be seen from the above-described embodiment, in the preparation method of triangle sheet nano-Ag particles provided by the present invention, adding of slaine has obvious impact to the method.The kind of slaine and addition, affect output and the concrete pattern of triangle sheet nano-Ag particles.
The preparation method of triangle sheet nano-Ag particles provided by the present invention; adopt chemical direct-reduction process; using phenmethylol as solvent with a kind of weak reducing agent; take polyvinylpyrrolidone as surfactant with protective agent; reduction trifluoroacetic acid silver; whole reaction is carried out in reactor, adds metallic aluminium salt or/and metal molysite carries out the regulation and control of triangle sheet nano-Ag particles pattern.This preparation method is simple to operate, can disposablely produce in enormous quantities, reproducible, and has realized use metal cation and carried out the regulation and control of triangle sheet nano-Ag particles.
In addition, those skilled in the art also can do other and change in spirit of the present invention, and these variations of doing according to spirit of the present invention certainly, all should be included in the present invention's scope required for protection.
Claims (10)
1. a preparation method for triangle sheet nano-Ag particles, comprises the following steps:
S1: trifluoroacetic acid silver, polyvinylpyrrolidone and phenmethylol are placed in a reactor and are mixed, obtain a mixture after stirring;
S2: add slaine in described mixture, at room temperature stir and obtain settled solution;
S3: described settled solution is heated to 120～150 degrees Celsius in reactor, and reaction a period of time obtains a product; And
S4: will obtain triangle sheet nano-Ag particles after described product centrifugation and washing.
2. the preparation method of triangle sheet nano-Ag particles as claimed in claim 1, is characterized in that, in step S1, the quality of described trifluoroacetic acid silver is 19～20 milligrams; Described polyvinylpyrrolidonemolecules molecules amount is 10000 left and right, and its quality is 0.04～0.06 gram; Described phenmethylol is 4～6 milliliters.
3. the preparation method of triangle sheet nano-Ag particles as claimed in claim 1, is characterized in that, in described step S2, slaine is at least one in molysite and aluminium salt.
4. the preparation method of triangle sheet nano-Ag particles as claimed in claim 3, is characterized in that, describedly in described mixture, adds the step of slaine to be: in described mixture, add molysite and aluminium salt.
5. the preparation method of triangle sheet nano-Ag particles as claimed in claim 4, is characterized in that, the mol ratio of described molysite and aluminium salt is 1:2～2:1.
6. the preparation method of triangle sheet nano-Ag particles as claimed in claim 3, is characterized in that, the soluble-salt that described molysite is iron comprises ferric nitrate and ferric sulfate.
7. the preparation method of triangle sheet nano-Ag particles as claimed in claim 3, is characterized in that, the soluble-salt that described aluminium salt is aluminium, comprises aluminum nitrate and aluminum sulfate.
8. the preparation method of triangle sheet nano-Ag particles as claimed in claim 1, is characterized in that, in step S3, when temperature reaches after 120～150 degrees Celsius, is incubated 4～6 hours.
9. the preparation method of triangle sheet nano-Ag particles as claimed in claim 1, it is characterized in that, in step S4, product is placed in to centrifuge tube, put into centrifuge and carry out centrifugation, the rotating speed of centrifuge is 10000 revs/min, after centrifugation, pour out centrifuge tube clear liquid at the middle and upper levels, be precipitated thing.
10. the preparation method of triangle sheet nano-Ag particles as claimed in claim 9, is characterized in that, in step S4, uses ethanol and deionized water to wash successively sediment, adopts ethanol or deionized water and sediment after centrifuge separating, washing when washing.
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| CN107486026A (en) * | 2017-08-18 | 2017-12-19 | 清华大学 | Seperation film of stable against biological contamination and preparation method thereof |
| CN110220869A (en) * | 2019-07-17 | 2019-09-10 | 北京师范大学 | A kind of method of mercury ion in detection water |
| CN110548880A (en) * | 2019-09-11 | 2019-12-10 | 南京牧科纳米科技有限公司 | Method and equipment for preparing metal nanosheets |
| CN110899722A (en) * | 2019-12-26 | 2020-03-24 | 无锡晶睿光电新材料有限公司 | Thin single crystal flake silver powder synthesized by chemical method and preparation method thereof |
| CN113084184A (en) * | 2021-03-25 | 2021-07-09 | 吉林大学 | Nano silver sheet and preparation method thereof |
| CN114226711A (en) * | 2021-12-31 | 2022-03-25 | 江苏纳美达光电科技有限公司 | Silver nanoparticles and method for preparing same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113084184A (en) * | 2021-03-25 | 2021-07-09 | 吉林大学 | Nano silver sheet and preparation method thereof |
| CN114226711A (en) * | 2021-12-31 | 2022-03-25 | 江苏纳美达光电科技有限公司 | Silver nanoparticles and method for preparing same |
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