CN107983970A - A kind of preparation method of Cu-Ag Nanoalloys - Google Patents
A kind of preparation method of Cu-Ag Nanoalloys Download PDFInfo
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- CN107983970A CN107983970A CN201711187394.6A CN201711187394A CN107983970A CN 107983970 A CN107983970 A CN 107983970A CN 201711187394 A CN201711187394 A CN 201711187394A CN 107983970 A CN107983970 A CN 107983970A
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
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Abstract
A kind of preparation method of Cu Ag Nanoalloys, belongs to Nanoalloy preparing technical field.The present invention using the gentle ascorbic acid of reproducibility or citric acid as reducing agent, it is environmentally friendly, there is good operability;The present invention is using the accurate sample introduction speed for controlling solution of micro-sampling pump so that in the reaction process of Ag in-stiu coatings Cu, Ag+Reaction system is added with fixed speed, it is ensured that the structure-controllable of the Cu Ag Nanoalloys of core shell structure, has good repeatability;The present invention adds suitable PVP as dispersant in the reaction system, reduces the agglomeration of particle, increases reaction active sites of the Ag in the in-situ reducing on Cu surfaces, improve combined coefficient.The method of the present invention is simple, and whole process is completed in air atmosphere, and reaction condition is gentle.
Description
Technical field
The invention belongs to Nanoalloy preparing technical field, and in particular to a kind of preparation method of Cu-Ag Nanoalloys.
Background technology
Copper system Nanoalloy has the advantages that the physicochemical properties that cost is low, stability is good, special because of it, catalysis,
The fields such as antibacterial, lubricant and electronic material are all widely used.Wherein, copper nano material have good electric conductivity and compared with
Low electron mobility, has been widely used in electrically-conducting paint, conducting wire material and electrode material.Particularly in flexible device
In the preparation of part, using Nanometer Copper as electrocondution slurry, applied to the printing of electronic circuit on flexible or extendable substrate, obtain
Nanometer Copper conducting wire show good flexibility and conductive stability.However, the heat endurance of Cu nano materials and anti-oxidant energy
Power is poor so that and the research of the Nanoalloy material of copper system receives the attention of more and more research workers, such as Cu-Ag,
The Nanoalloys such as Cu-Ni, Cu-Sn.Wherein, Cu-Ag Nanoalloys are a kind of common copper system Nanoalloy material, at present, Cu-
Ag Nanoalloys are typically to be carried out in the protective atmosphere of argon gas or nitrogen, and Cu simple substance is (as being hydrated by strong reductant
Hydrazine, boron Cymag or potassium borohydride) reduction obtains, efficient although the reaction time is short, hydrazine hydrate, boron Cymag etc. are strong
Reducing agent is poisonous, has harm to human body and environment.
Document (Y.Wei, S.Chen, Y.Lin, Z.Yang, L.Liu, Cu-Ag core-shell nanowires for
electronic skin with a petal molded microstructure,Journal of Materials
Chemistry C3 (37) (2015) 9594-9602.) the line style Cu-Ag alloys of core shell structure a kind of are reported, preparation process is adopted
Reducing agent is used as by the use of hydrazine hydrate.Document (H.Wang, C.Wu, Y.Huang, F.Sun, N.Lin, A.M.Soomro, Z.Zhong,
X.Yang,X.Chen,J.Kang,D.Cai,One-Pot Synthesis of Superfine Core-Shell Cu@metal
Nanowires for Highly Tenacious Transparent LED Dimmer,ACS applied materials&
Interfaces (2016)) one kind is reported using acetylacetone,2,4-pentanedione as reducing agent reduction CuCl2To prepare the side of Cu alloys
Method.Document (T.Dung Chinh, D.Thi My Dung, H.Kim Khanh, E.Fribourg-Blanc, D.Mau Chien,
Synthesis of Cu core Ag shell nanoparticles using chemical reduction method,
Advances in Natural Sciences-Nanoscience and Nanotechnology 6 (2) (2015)) report
A kind of method for preparing alloy as reducing agent using sodium borohydride.However, the reducing agent used in the above method is to human body
There is harm with environment.
The content of the invention
The present invention for background technology there are the defects of, it is proposed that a kind of preparation method of Cu-Ag Nanoalloys.This method
Easy to operate, whole process is completed in air atmosphere, and reaction condition is gentle.
Technical scheme is as follows:
A kind of preparation method of Cu-Ag Nanoalloys, it is characterised in that specifically include following steps:
The preparation of step 1, Cu nano particles:
1.1 using soluble copper salt as solute, volume ratio 3:1 deionized water and absolute ethyl alcohol is prepared as solvent
Obtain the mixed liquor A that mass concentration is 0.02~0.05g/mL;
1.2 using mass ratio as (8~10):1 reducing agent and PVP (polyvinylpyrrolidone) is used as solute, deionized water
As solvent, the mixed liquid B for obtaining the mass concentration of solute as 0.1~0.3g/mL is prepared;Wherein, the reducing agent is anti-bad
Hematic acid or citric acid;
1.3 mixed liquor As for obtaining step 1.1 are transferred in three-neck flask, are stirred under 50~100 DEG C of water-baths, then
Use micro-sampling pump that mixed liquid B is added dropwise in mixed liquor A with the speed of 0.1~1mL/min, obtained mixed liquor C is 50
More than 20h is reacted in~100 DEG C of water-baths, until the color of solution is changed into dark brown;
After the completion of 1.4 reactions, filtering, obtained product is respectively washed 5~8 times using deionized water and ethanol, Ran Hou
Dry more than 24h at a temperature of 100~120 DEG C, obtains Cu nano particles in vacuum drying chamber;
The preparation of step 2, Cu-Ag Nanoalloys:
The 2.1 Cu nano particles for respectively obtaining citric acid, PVP (polyvinylpyrrolidone) and step 1 add ethylene glycol
With absolute ethyl alcohol in the mixed solvent, more than 30min is stirred, obtains mixed liquor D;Wherein, in mixed liquor D citric acid mass concentration
For 0.01~0.1g/mL, the mass concentration of PVP (polyvinylpyrrolidone) is 0.01~0.1g/mL, and the mass concentration of Cu is
The volume ratio of 0.1~0.2g/mL, ethylene glycol and absolute ethyl alcohol is 5:2;
2.2 with AgNO3For solute, deionized water is solvent, and preparation obtains AgNO3Solution;
2.3 use the AgNO that micro-sampling pump is prepared step 2.2 with the speed of 0.01~0.2mL/min3Solution is added dropwise
In the mixed liquor D obtained to step 2.1, after being added dropwise to complete, stirring reaction more than 4h, until reaction solution presentation is uniform black
Color;Wherein, the Cu and AgNO in mixed liquor D3Molar ratio be 1:(0.5~2);
After the completion of 2.4 reactions, filtering, obtained product is respectively washed 5~8 times using deionized water and ethanol, Ran Hou
Dry more than 24h at a temperature of 100~120 DEG C, obtains Cu-Ag Nanoalloys in vacuum drying chamber.
Further, soluble copper salt described in step 1.1 is copper chloride, copper sulphate or copper nitrate etc..
Further, mixing speed is more than 1000r/min in step 1.3.
Beneficial effects of the present invention are:
The present invention provides a kind of preparation method of Cu-Ag Nanoalloys, easy to operate, whole process is in air atmosphere
Complete, reaction condition is gentle.The present invention uses the gentle ascorbic acid of reproducibility or citric acid as reducing agent, to environment friend
It is good, there is good operability;The present invention is using the accurate sample introduction speed for controlling solution of micro-sampling pump so that Ag bags in situ
In the reaction process for covering Cu, Ag+Reaction system is added with fixed speed, it is ensured that the Cu-Ag Nanoalloys of core shell structure
Structure-controllable, has good repeatability;The present invention adds suitable PVP (polyvinylpyrrolidone) works in the reaction system
For dispersant, the agglomeration of particle is reduced, reaction active sites of the Ag in the in-situ reducing on Cu surfaces is increased, improves conjunction
Into efficiency.
Brief description of the drawings
Fig. 1 is the XRD spectrum for the Cu nano particles that embodiment step 1 obtains;
Fig. 2 is the XRD spectrum for the Cu-Ag Nanoalloys that embodiment obtains;
Fig. 3 is the SEM of the Cu nano particles (a) that embodiment step 1 obtains and the Cu-Ag Nanoalloys (b) that step 2 obtains
Figure;
Fig. 4 is the EDS for the Cu-Ag Nanoalloys that embodiment obtains;
Fig. 5 is the schematic diagram of the preparation method of Cu-Ag Nanoalloys provided by the invention.
Embodiment
With reference to the accompanying drawings and examples, technical scheme is described in detail.
A kind of preparation method of Cu-Ag Nanoalloys, it is characterised in that specifically include following steps:
The preparation of step 1, Cu nano particles:
1.1 using soluble copper salt as solute, volume ratio 3:1 deionized water and absolute ethyl alcohol is prepared as solvent
Obtain the mixed liquor A that mass concentration is 0.02~0.05g/mL;
1.2 using mass ratio as (8~10):1 reducing agent and PVP (polyvinylpyrrolidone) is used as solute, deionized water
As solvent, the mixed liquid B for obtaining the mass concentration of solute as 0.1~0.3g/mL is prepared;Wherein, the reducing agent is anti-bad
Hematic acid or citric acid;
1.3 mixed liquor As for obtaining step 1.1 are transferred in three-neck flask, are stirred under 50~100 DEG C of water-baths, then
Use micro-sampling pump that mixed liquid B is added dropwise in mixed liquor A with the speed of 0.1~1mL/min, obtained mixed liquor C is 50
More than 20h is reacted in~100 DEG C of water-baths, until the color of solution is changed into dark brown;
After the completion of 1.4 reactions, filtering, obtained product uses cleaning 5~8 times successively respectively of deionized water and ethanol, directly
It is in neutrality to eluate, then dries more than 24h at a temperature of 100~120 DEG C in vacuum drying chamber, obtain Cu nano particles;
The preparation of step 2, Cu-Ag Nanoalloys:
2.1 using volume ratio as 5:As solvent, it is 0.01 to add mass concentration for 2 ethylene glycol and the mixed liquor of absolute ethyl alcohol
The citric acid of~0.1g/mL and the PVP of 0.01~0.1g/mL, are uniformly mixed, and the step 1 for then adding 0.1~0.2g/mL obtains
The Cu nano particles arrived, stir more than 30min, obtain mixed liquor D;
2.2 with AgNO3For solute, deionized water is solvent, and preparation obtains AgNO3Solution;
2.3 use the AgNO that micro-sampling pump is prepared step 2.2 with the speed of 0.01~0.2mL/min3Solution is added dropwise
In the mixed liquor D obtained to step 2.1, after being added dropwise to complete, stirring reaction more than 4h, until reaction solution presentation is uniform black
Color;Wherein, the Cu and AgNO in mixed liquor D3Molar ratio be 1:(0.5~2);
After the completion of 2.4 reactions, filtering, obtained product is respectively washed 5~8 times using deionized water and ethanol, Ran Hou
Dry more than 24h at a temperature of 100~120 DEG C, obtains Cu-Ag Nanoalloys in vacuum drying chamber.
Embodiment
A kind of preparation method of Cu-Ag Nanoalloys, specifically includes following steps:
The preparation of step 1, Cu nano particles:
1.1 using copper chloride as solute, volume ratio 3:1 deionized water and absolute ethyl alcohol is obtained as solvent, preparation
Mass concentration is the mixed liquor A of 0.025g/mL;
1.2 using mass ratio as 10:1 ascorbic acid and PVP (polyvinylpyrrolidone) is used as solute, deionized water conduct
Solvent, prepares the mixed liquid B for obtaining the mass concentration of solute as 0.1g/mL;
1.3 mixed liquor As for obtaining step 1.1 are transferred in three-neck flask, with the speed of 1000r/min under 70 DEG C of water-baths
Degree stirring, then uses micro-sampling pump that mixed liquid B is added dropwise in mixed liquor A with the speed of 0.1mL/min, obtained mixing
Liquid C reacts 20h in 70 DEG C of water-baths, until the color of solution is changed into dark brown;
After the completion of 1.4 reactions, filtering, obtained product is cleaned 8 times successively respectively using deionized water and ethanol, until washing
Go out liquid to be in neutrality, then dry more than 24h at a temperature of 120 DEG C in vacuum drying chamber, obtain Cu nano particles;
The preparation of step 2, Cu-Ag Nanoalloys:
2.1 using volume ratio as 5:As solvent, adding mass concentration is for 2 ethylene glycol and the mixed liquor of absolute ethyl alcohol
The citric acid of 0.05g/mL and the PVP of 0.015g/mL, are uniformly mixed, and then add the Cu nanometers that the step 1 of 0.1g/mL obtains
Particle, with speed stirring 30min of 1000r/min or so, obtains mixed liquor D;
2.2 with AgNO3For solute, deionized water is solvent, and preparation obtains the AgNO of 0.025g/mL3Solution;
2.3 use the AgNO that micro-sampling pump is prepared step 2.2 with the speed of 0.05mL/min3Solution is added dropwise to step
In 2.1 obtained mixed liquor D, after being added dropwise to complete, stirring reaction more than 4h, until uniform black is presented in reaction solution;Wherein,
Cu and AgNO in mixed liquor D3Molar ratio be 1:1;
After the completion of 2.4 reactions, filtering, obtained product is respectively washed 8 times using deionized water and ethanol, then in vacuum
Dry more than 24h at a temperature of 120 DEG C, obtains the Cu-Ag Nanoalloys of core shell structure in drying box.
Fig. 1 is the XRD spectrum for the Cu nano particles that embodiment step 1 obtains;As shown in Figure 1, have Cu's in collection of illustrative plates
(111), (200), (220), (311) characteristic peak (JCPDS 65-9743), show that the Cu nano particles that step 1 obtains are the center of area
Cubic structure.Fig. 2 is the XRD spectrum for the Cu-Ag Nanoalloys that embodiment obtains;As shown in Figure 2, in collection of illustrative plates have Ag (111),
(200), the characteristic peak (JCPDS 65-2871) of (220), (311), (222), while also have the characteristic peak of Cu, show the present invention
Embodiment has successfully obtained Cu-Ag Nanoalloys using the method for solution reduction, and combined coefficient is high.
Fig. 3 is the SEM of the Cu nano particles (a) that embodiment step 1 obtains and the Cu-Ag Nanoalloys (b) that step 2 obtains
Figure;From the figure 3, it may be seen that Cu nano particles become large-sized after the processing of embodiment step 2, and formed on the surface of Cu nano particles
Fine and close Ag clads.
Fig. 4 is the EDS for the Cu-Ag Nanoalloys that embodiment obtains;As shown in Figure 4, the Cu-Ag nanometers that embodiment obtains are closed
Gold is core shell structure.
Fig. 5 is the schematic diagram of the preparation method of Cu-Ag Nanoalloys provided by the invention.
Claims (2)
1. a kind of preparation method of Cu-Ag Nanoalloys, it is characterised in that comprise the following steps:
The preparation of step 1, Cu nano particles:
1.1 using soluble copper salt as solute, and as solvent, preparation obtains mass concentration as 0.02 for deionized water and absolute ethyl alcohol
The mixed liquor A of~0.05g/mL;
1.2 using mass ratio as (8~10):1 reducing agent and PVP obtains solute as solute, deionized water as solvent, preparation
Mass concentration be 0.1~0.3g/mL mixed liquid B;Wherein, the reducing agent is ascorbic acid or citric acid;
1.3 stir the mixed liquor A that step 1.1 obtains under 50~100 DEG C of water-baths, then use micro-sampling pump with 0.1~
Mixed liquid B is added dropwise in mixed liquor A by the speed of 1mL/min, obtained mixed liquor C reacted in 50~100 DEG C of water-baths 20h with
On;
After the completion of 1.4 reactions, filtering, obtained product is cleaned using deionized water and ethanol, dry, obtains Cu nano particles;
The preparation of step 2, Cu-Ag Nanoalloys:
The 2.1 Cu nano particles for respectively obtaining citric acid, PVP and step 1 add ethylene glycol and absolute ethyl alcohol in the mixed solvent,
More than 30min is stirred, obtains mixed liquor D;Wherein, the mass concentration of citric acid is 0.01~0.1g/mL in mixed liquor D, PVP's
Mass concentration is 0.01~0.1g/mL, and the mass concentration of Cu is 0.1~0.2g/mL;
2.2 with AgNO3For solute, deionized water is solvent, and preparation obtains AgNO3Solution;
2.3 use the AgNO that micro-sampling pump is prepared step 2.2 with the speed of 0.01~0.2mL/min3Solution is added dropwise to step
In 2.1 obtained mixed liquor D, after being added dropwise to complete, stirring reaction more than 4h;Wherein, the Cu and AgNO in mixed liquor D3Mole
Than for 1:(0.5~2);
After the completion of 2.4 reactions, filtering, obtained product is cleaned using deionized water and ethanol, dry, obtains Cu-Ag nanometers of conjunctions
Gold.
2. the preparation method of Cu-Ag Nanoalloys according to claim 1, it is characterised in that solvable described in step 1.1
Property mantoquita is copper chloride, copper sulphate or copper nitrate.
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Cited By (6)
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CN108977923A (en) * | 2018-06-27 | 2018-12-11 | 佛山市南海区佳妍内衣有限公司 | A kind of functional polyalkylene ester fiber |
CN108995327A (en) * | 2018-06-27 | 2018-12-14 | 佛山市南海区佳妍内衣有限公司 | A kind of composite polar fleece fabric |
CN114603153A (en) * | 2022-03-19 | 2022-06-10 | 昆明理工大学 | Preparation method of bimetallic particles formed by self-assembly of nano copper and silver |
CN114700497A (en) * | 2022-03-18 | 2022-07-05 | 昆明理工大学 | Preparation method of pomegranate-shaped structure Cu-Ag alloy |
CN114799195A (en) * | 2022-03-10 | 2022-07-29 | 昆明理工大学 | Preparation method of self-assembled micro-nano structure Cu-Ag nano particles |
CN114799195B (en) * | 2022-03-10 | 2024-06-25 | 昆明理工大学 | Preparation method of self-assembled micro-nano structure Cu-Ag nano particles |
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Cited By (8)
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CN108977923A (en) * | 2018-06-27 | 2018-12-11 | 佛山市南海区佳妍内衣有限公司 | A kind of functional polyalkylene ester fiber |
CN108995327A (en) * | 2018-06-27 | 2018-12-14 | 佛山市南海区佳妍内衣有限公司 | A kind of composite polar fleece fabric |
CN114799195A (en) * | 2022-03-10 | 2022-07-29 | 昆明理工大学 | Preparation method of self-assembled micro-nano structure Cu-Ag nano particles |
CN114799195B (en) * | 2022-03-10 | 2024-06-25 | 昆明理工大学 | Preparation method of self-assembled micro-nano structure Cu-Ag nano particles |
CN114700497A (en) * | 2022-03-18 | 2022-07-05 | 昆明理工大学 | Preparation method of pomegranate-shaped structure Cu-Ag alloy |
CN114700497B (en) * | 2022-03-18 | 2024-03-29 | 昆明理工大学 | Preparation method of Cu-Ag alloy with pomegranate-like structure |
CN114603153A (en) * | 2022-03-19 | 2022-06-10 | 昆明理工大学 | Preparation method of bimetallic particles formed by self-assembly of nano copper and silver |
CN114603153B (en) * | 2022-03-19 | 2024-01-23 | 昆明理工大学 | Preparation method of bimetal particles formed by self-assembly of nano copper and silver |
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