CN108817417A - Preparation method of sphere-like nano silver sheet cluster - Google Patents

Preparation method of sphere-like nano silver sheet cluster Download PDF

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Publication number
CN108817417A
CN108817417A CN201810867437.3A CN201810867437A CN108817417A CN 108817417 A CN108817417 A CN 108817417A CN 201810867437 A CN201810867437 A CN 201810867437A CN 108817417 A CN108817417 A CN 108817417A
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China
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solution
nano silver
preparation
cluster
weighs
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CN201810867437.3A
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Chinese (zh)
Inventor
王悦辉
杨星
谢辉
赵玉珍
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University of Electronic Science and Technology of China Zhongshan Institute
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University of Electronic Science and Technology of China Zhongshan Institute
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Priority to CN201810867437.3A priority Critical patent/CN108817417A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

Abstract

The invention discloses a preparation method of a sphere-like nano silver sheet cluster, which is characterized by comprising the following steps: mixing silver nitrate with the concentration of 0.8-6% and citric acid with the concentration of 0.3-2.0%, stirring for 5-10 minutes, adding ferrous sulfate with the concentration of 1.6-8.0% into the mixed solution, magnetically stirring for 1-2 hours at the stirring speed of 550 r/min, and after the reaction is finished, performing centrifugal washing on the product to obtain the spheroidal nano silver sheet cluster. The preparation method is simple and easy to operate, the reaction is carried out in aqueous solution at room temperature, no special additive or template is used, the reaction time is short, the cost and the energy consumption are low, and the industrial production can be realized.

Description

A kind of preparation method of near-spherical nano silver slice cluster
Technical field
The present invention relates to a kind of preparation methods of Silver Clusters, with the preparation side for being a kind of near-spherical nano silver slice cluster Method.
Background technique
Nano silver is a kind of very important precious metal material, and the characteristic of nano silver and its size and shape are closely related, Therefore, the morphology and size control research of nano silver is always one of the hot spot of nano materials research.
Currently, spherical nano-Ag particles and nano-silver thread control synthesis have obtained good progress, and realize production Industry.But control synthesizing nano-silver piece still has certain difficulty.In general, with polyvinylpyrrolidone, cetyl bromination Ammonium or diisooctyl sodium sulfosuccinate etc. are coating material, are prepared using Photoinduced conversion method, template and solwution method etc. Nano silver slice.Wherein Photoinduced conversion method and template operation are more complicated, and yield is lower.Solwution method yield is high, at low cost, It is the current main method studied and apply.105268995 A of Chinese patent CN(A kind of preparation method of nano silver slice)In adopt It is raw material with silver nitrate, polyvinylpyrrolidone is coating material, sodium borohydride is reducing agent, water-soluble in 0-60 DEG C of polyalcohol Reaction prepares nano silver slice in liquid.105127448 A of Chinese patent CN(A kind of room temperature preparation of overlarge area nano silver slice Method)In report with silver nitrate, PVP, FeSO4With dilute H2SO4For raw material, magnetic agitation reaction 3-6h prepares nanometer at room temperature Silver strip.
Nano material has self assembly characteristic due to special surface features.The self assembly of nano material refers to surface The nano particle basic structural unit of characteristic, which passes through, spontaneously forms or is collected as a stabilization, tool under non-covalent interaction There is the structure of certain regular geometric appearance.Self assembling process is not a large amount ofAtom, ion, weak force is simple between molecule Superposition, but spontaneous generation simultaneously be associated with and gathers to form that one is close and orderly or standard has between several body The structural body of sequence is a kind of whole complicated synergistic effect.It can be obtained using the self assembly characteristic of nano material a variety of multiple Miscellaneous structural body, to assign material special function.108190957 A of Chinese patent CN(A kind of flower-shaped cerous molybdate nanometer rods The preparation method of cluster)In report and prepared using sodium molybdate, cerous nitrate, polyethylene glycol and water as raw material in 90 DEG C of water-bath 0.5-8h Flower-shaped cerous molybdate nanometer rods cluster.
It is many about the report for preparing nano silver slice method at present, but nano silver slice self-assembled structures research report compared with Few, the especially research in terms of the synthesis of near-spherical nano silver slice cluster has not been reported.
Summary of the invention
It is an object of the invention to by regulation, a kind of simple process is provided, operation is easy, low-cost type ball The preparation method of shape nano silver slice cluster.Reaction is carried out in the aqueous solution of room temperature condition, without special additive, template, instead Short between seasonable, cost and energy consumption are low, it can be achieved that industrialized production.
The present invention uses following technical scheme:
A kind of preparation method of near-spherical nano silver slice cluster, which is characterized in that include the following steps:
(1)It weighs silver nitrate solid to be dissolved in water ion water, is configured to silver nitrate solution;
(2)It weighs citric acid solid to be dissolved in deionized water, is configured to surface modification agent solution;
(3)It weighs ferrous sulfate solid to be dissolved in deionized water, is configured to inhibitor solution;
(4)At room temperature, by step(2)The solution of preparation is added to(1)In, after stirring 5-10 minutes, by step(3)System Standby solution is added rapidly in above-mentioned mixed solution, under the mixing speed of 550 r/min, magnetic agitation 1-2 hours;
(5)After the reaction was completed, product is centrifuged, first with deionized water centrifuge washing 3 times, then with ethanol washing 2 times, i.e., Near-spherical nano silver slice cluster is obtained, the spherical nano silver slice cluster is distributed in deionized water and is saved.
The preparation method of above-mentioned near-spherical nano silver slice cluster, it is characterised in that:
In the mixed solution, silver nitrate concentration 0.8%-6%;Citric acid concentration is 0.3%-2.0%;Ferrous sulfate concentration is 1.6%-8.0%。
Use ferrous sulfate for reducing agent and inhibitor in the present invention, Fe2+By Ag+It is reduced into Ag, Fe2+Then it is oxidized to Fe3+;Citric acid is adsorbed on Ag particular crystal plane as coating material, meanwhile, citric acid also has reduction reaction and regulation system Middle Fe2+The effect of reducing power can control Ag atomic nucleation and growth rate in system, to be conducive to Ag nanometers of growth Piece.
Compared with prior art, the beneficial effects of the present invention are:
The present invention uses common silver nitrate, ferrous sulfate and citric acid for raw material, and magnetic agitation has synthesized spherical at room temperature Nano silver slice cluster.Spherical nano silver slice cluster diameter 200-500 nm, by thickness 10-30 nm, size 70-150 nm's Nano silver slice is self-assembly of.
Preparation method of the invention is simple, easily operated, reaction is to carry out in the aqueous solution of room temperature condition, add without special Add agent, template, the reaction time is short, and cost and energy consumption are low, it can be achieved that industrialized production.
Detailed description of the invention
Fig. 1 is the electron scanning micrograph of product in the embodiment of the present invention 1.
Fig. 2 is the X ray diffracting spectrum of product in the embodiment of the present invention 1.
Fig. 3 is the electron scanning micrograph of product in the embodiment of the present invention 2.
Fig. 4 is the electron scanning micrograph of product in the embodiment of the present invention 3.
Fig. 5 is the electron scanning micrograph of product in the embodiment of the present invention 4.
Fig. 6 is the electron scanning micrograph of product in the embodiment of the present invention 5.
Fig. 7 is the electron scanning micrograph of product in the embodiment of the present invention 6.
Fig. 8 is the electron scanning micrograph of product in the embodiment of the present invention 7.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below with reference to the embodiment of the present invention, to this hair Technical solution in bright embodiment is clearly and completely described.Described embodiments are some of the embodiments of the present invention, and The embodiment being not all of.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creative work Under the premise of every other embodiment obtained, shall fall within the protection scope of the present invention.
Embodiment 1:
(1)It weighs 4 grams of silver nitrates and is dissolved in 100 milliliters and go in water ion water, be configured to silver nitrate solution;
(2)It weighs 0.75 gram of citric acid to be dissolved in 50 ml deionized waters, is configured to surface modification agent solution;
(3)It weighs 5 grams of ferrous sulfate to be dissolved in 100 ml deionized waters, is configured to inhibitor solution;
(4)At room temperature, by step(2)The solution of preparation is added to(1)In, it stirs after five minutes, by step(3)Preparation Solution be added rapidly in above-mentioned mixed solution, under the mixing speed of 550 r/min, magnetic agitation 2 hours;
(5)After the reaction was completed, product is centrifuged, first with deionized water centrifuge washing 3 times, then with ethanol washing 2 times, i.e., Near-spherical nano silver slice cluster is obtained, the spherical nano silver slice cluster is distributed in deionized water and is saved;
(6)The electron scanning micrograph of product prepared by the present embodiment is as shown in Figure 1, it can be seen that product is spherical receives Rice silver strip cluster, cluster diameter 200-500 nm, by thickness 10-30 nm, the nano silver slice self assembly shape of size 70-150 nm At;
(7) X-ray diffractogram of product prepared by the present embodiment shows made as shown in Fig. 2, contrast with silver-colored standard diagram Standby product is silver.
Embodiment 2:
(1)It weighs 5 grams of silver nitrates and is dissolved in 100 milliliters and go in water ion water, be configured to silver nitrate solution;
(2)It weighs 1.0 grams of citric acids to be dissolved in 50 ml deionized waters, is configured to surface modification agent solution;
(3)It weighs 5 grams of ferrous sulfate to be dissolved in 100 ml deionized waters, is configured to inhibitor solution;
(4)At room temperature, by step(2)The solution of preparation is added to(1)In, it stirs after five minutes, by step(3)Preparation Solution be added rapidly in above-mentioned mixed solution, under the mixing speed of 550 r/min, magnetic agitation 2 hours;
(5)After the reaction was completed, product is centrifuged, first with deionized water centrifuge washing 3 times, then with ethanol washing 2 times, i.e., Near-spherical nano silver slice cluster is obtained, the spherical nano silver slice cluster is distributed in deionized water and is saved;
(6)The electron scanning micrograph of product prepared by the present embodiment is as shown in Figure 3, it can be seen that product is spherical receives Rice silver strip cluster, cluster diameter 200-500 nm, by thickness 10-30 nm, the nano silver slice self assembly shape of size 70-150 nm At.
Embodiment 3:
(1)It weighs 5 grams of silver nitrates and is dissolved in 100 milliliters and go in water ion water, be configured to silver nitrate solution;
(2)It weighs 1.5 grams of citric acids to be dissolved in 50 ml deionized waters, is configured to surface modification agent solution;
(3)It weighs 5 grams of ferrous sulfate to be dissolved in 100 ml deionized waters, is configured to inhibitor solution;
(4)At room temperature, by step(2)The solution of preparation is added to(1)In, it stirs after five minutes, by step(3)Preparation Solution be added rapidly in above-mentioned mixed solution, under the mixing speed of 550 r/min, magnetic agitation 2 hours;
(5)After the reaction was completed, product is centrifuged, first with deionized water centrifuge washing 3 times, then with ethanol washing 2 times, i.e., Near-spherical nano silver slice cluster is obtained, the spherical nano silver slice cluster is distributed in deionized water and is saved;
(6)The electron scanning micrograph of product prepared by the present embodiment is as shown in Figure 4, it can be seen that product is spherical receives Rice silver strip cluster, cluster diameter 200-500 nm, by thickness 10-30 nm, the nano silver slice self assembly shape of size 70-150 nm At.
Embodiment 4:
(1)It weighs 5 grams of silver nitrates and is dissolved in 100 milliliters and go in water ion water, be configured to silver nitrate solution;
(2)It weighs 2.0 grams of citric acids to be dissolved in 50 ml deionized waters, is configured to surface modification agent solution;
(3)It weighs 9.5 grams of ferrous sulfate to be dissolved in 100 ml deionized waters, is configured to inhibitor solution;
(4)At room temperature, by step(2)The solution of preparation is added to(1)In, it stirs after five minutes, by step(3)Preparation Solution be added rapidly in above-mentioned mixed solution, under the mixing speed of 550 r/min, magnetic agitation 2 hours;
(5)After the reaction was completed, product is centrifuged, first with deionized water centrifuge washing 3 times, then with ethanol washing 2 times, i.e., Near-spherical nano silver slice cluster is obtained, the spherical nano silver slice cluster is distributed in deionized water and is saved;
(6)The electron scanning micrograph of product prepared by the present embodiment is as shown in Figure 5, it can be seen that product is spherical receives Rice silver strip cluster, cluster diameter 200-500 nm, by thickness 10-30 nm, the nano silver slice self assembly shape of size 70-150 nm At.
Embodiment 5:
(1)It weighs 15 grams of silver nitrates and is dissolved in 100 milliliters and go in water ion water, be configured to silver nitrate solution;
(2)It weighs 4.0 grams of citric acids to be dissolved in 50 ml deionized waters, is configured to surface modification agent solution;
(3)It weighs 6.5 grams of ferrous sulfate to be dissolved in 100 ml deionized waters, is configured to inhibitor solution;
(4)At room temperature, by step(2)The solution of preparation is added to(1)In, it stirs after five minutes, by step(3)Preparation Solution be added rapidly in above-mentioned mixed solution, under the mixing speed of 550 r/min, magnetic agitation 2 hours;
(5)After the reaction was completed, product is centrifuged, first with deionized water centrifuge washing 3 times, then with ethanol washing 2 times, i.e., Near-spherical nano silver slice cluster is obtained, the spherical nano silver slice cluster is distributed in deionized water and is saved;
(6)The electron scanning micrograph of product prepared by the present embodiment is as shown in Figure 5, it can be seen that product is spherical receives Rice silver strip cluster, cluster diameter 200-500 nm, by thickness 10-30 nm, the nano silver slice self assembly shape of size 70-150 nm At.
Embodiment 6:
(1)It weighs 5.0 grams of silver nitrates and is dissolved in 100 milliliters and go in water ion water, be configured to silver nitrate solution;
(2)It weighs 2.0 grams of citric acids to be dissolved in 50 ml deionized waters, is configured to surface modification agent solution;
(3)It weighs 5.0 grams of ferrous sulfate to be dissolved in 100 ml deionized waters, is configured to inhibitor solution;
(4)At room temperature, by step(2)The solution of preparation is added to(1)In, it stirs after five minutes, by step(3)Preparation Solution be added rapidly in above-mentioned mixed solution, under the mixing speed of 550 r/min, magnetic agitation 2 hours;
(5)After the reaction was completed, product is centrifuged, first with deionized water centrifuge washing 3 times, then with ethanol washing 2 times, i.e., Near-spherical nano silver slice cluster is obtained, the spherical nano silver slice cluster is distributed in deionized water and is saved;
(6)The electron scanning micrograph of product prepared by the present embodiment is as shown in Figure 5, it can be seen that product is spherical receives Rice silver strip cluster, cluster diameter 200-500 nm, by thickness 10-30 nm, the nano silver slice self assembly shape of size 70-150 nm At.
Embodiment 7:
(1)It weighs 5.0 grams of silver nitrates and is dissolved in 100 milliliters and go in water ion water, be configured to silver nitrate solution;
(2)It weighs 1.5 grams of citric acids to be dissolved in 50 ml deionized waters, is configured to surface modification agent solution;
(3)It weighs 9.5 grams of ferrous sulfate to be dissolved in 100 ml deionized waters, is configured to inhibitor solution;
(4)At room temperature, by step(2)The solution of preparation is added to(1)In, it stirs after five minutes, by step(3)Preparation Solution be added rapidly in above-mentioned mixed solution, under the mixing speed of 550 r/min, magnetic agitation 2 hours;
(5)After the reaction was completed, product is centrifuged, first with deionized water centrifuge washing 3 times, then with ethanol washing 2 times, i.e., Near-spherical nano silver slice cluster is obtained, the spherical nano silver slice cluster is distributed in deionized water and is saved;
(6)The electron scanning micrograph of product prepared by the present embodiment is as shown in Figure 5, it can be seen that product is spherical receives Rice silver strip cluster, cluster diameter 200-500 nm, by thickness 10-30 nm, the nano silver slice self assembly shape of size 70-150 nm At.
Above-described embodiment is merely illustrative of the technical solution of the present invention and is not intended to limit it, all without departing from the present invention Any modification of spirit and scope or equivalent replacement should all cover the range in technical solution of the present invention.
The invention discloses a kind of preparation methods of near-spherical nano silver slice cluster, it is characterised in that:It is 0.8%- by concentration 6% silver nitrate is mixed with the citric acid that concentration is 0.3%-2.0%, after stirring 5-10 minutes, the sulphur for being 1.6%-8.0% by concentration Sour ferrous iron is add to the above mixed solution under the mixing speed of 550 r/min, and magnetic agitation 1-2 hours, after the reaction was completed, Product is subjected to centrifuge washing, i.e. acquisition near-spherical nano silver slice cluster.Preparation method of the invention is simple, easily operated, anti- Should be in the aqueous solution of room temperature condition carry out, without special additive, template, the reaction time is short, cost and consume energy it is low, it can be achieved that Industrialized production.

Claims (2)

1. a kind of preparation method of near-spherical nano silver slice cluster, which is characterized in that include the following steps:
(1)It weighs silver nitrate solid to be dissolved in water ion water, is configured to silver nitrate solution;
(2)It weighs citric acid solid to be dissolved in deionized water, is configured to surface modification agent solution;
(3)It weighs ferrous sulfate solid to be dissolved in deionized water, is configured to inhibitor solution;
(4)At room temperature, by step(2)The solution of preparation is added to(1)In, after stirring 5-10 minutes, by step(3)System Standby solution is added rapidly in above-mentioned mixed solution, under the mixing speed of 550 r/min, magnetic agitation 1-2 hours;
(5)After the reaction was completed, product is centrifuged, first with deionized water centrifuge washing 3 times, then with ethanol washing 2 times, i.e., Near-spherical nano silver slice cluster is obtained, the spherical nano silver slice cluster is distributed in deionized water and is saved.
2. a kind of preparation method of spherical nano silver slice cluster according to claim 1, which is characterized in that
In the mixed solution, silver nitrate concentration 0.8%-6%;Citric acid concentration is 0.3%-2.0%;Ferrous sulfate concentration is 1.6%-8.0%。
CN201810867437.3A 2018-09-04 2018-09-04 Preparation method of sphere-like nano silver sheet cluster Pending CN108817417A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110330512A (en) * 2019-07-30 2019-10-15 山东大学 A kind of ag nano-cluster fluorescence nano stick and preparation method thereof and the application in white light LEDs
CN110681874A (en) * 2019-11-07 2020-01-14 西南大学 Preparation method and hydrogen evolution application of silver-nickel nanocluster
CN114733519A (en) * 2022-05-31 2022-07-12 电子科技大学中山学院 Preparation method of nano-silver/graphene/nano-titanium dioxide composite material
CN115283688A (en) * 2022-07-04 2022-11-04 电子科技大学 Method for preparing gold nanocluster by solid-phase dynamics control method
CN115502408A (en) * 2022-09-21 2022-12-23 四川工程职业技术学院 Preparation method of flower-like silver powder

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110330512A (en) * 2019-07-30 2019-10-15 山东大学 A kind of ag nano-cluster fluorescence nano stick and preparation method thereof and the application in white light LEDs
CN110330512B (en) * 2019-07-30 2021-05-14 山东大学 Silver nanocluster fluorescent nanorod, preparation method thereof and application thereof in white light LED
CN110681874A (en) * 2019-11-07 2020-01-14 西南大学 Preparation method and hydrogen evolution application of silver-nickel nanocluster
CN110681874B (en) * 2019-11-07 2022-05-31 西南大学 Preparation method and hydrogen evolution application of silver-nickel nanocluster
CN114733519A (en) * 2022-05-31 2022-07-12 电子科技大学中山学院 Preparation method of nano-silver/graphene/nano-titanium dioxide composite material
CN115283688A (en) * 2022-07-04 2022-11-04 电子科技大学 Method for preparing gold nanocluster by solid-phase dynamics control method
CN115283688B (en) * 2022-07-04 2024-03-26 电子科技大学 Method for preparing gold nanoclusters by using solid-phase kinetic control method
CN115502408A (en) * 2022-09-21 2022-12-23 四川工程职业技术学院 Preparation method of flower-like silver powder

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Application publication date: 20181116