CN113084154A - Method for efficiently purifying nano silver wires - Google Patents

Method for efficiently purifying nano silver wires Download PDF

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Publication number
CN113084154A
CN113084154A CN202110334736.2A CN202110334736A CN113084154A CN 113084154 A CN113084154 A CN 113084154A CN 202110334736 A CN202110334736 A CN 202110334736A CN 113084154 A CN113084154 A CN 113084154A
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CN
China
Prior art keywords
silver wire
solvent
nano silver
pvp
acetone
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Pending
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CN202110334736.2A
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Chinese (zh)
Inventor
杨棚竣
甘李
周明
杨建文
唐波
胡典勤
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Chongqing Xiyu New Material Technology Co ltd
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Chongqing Xiyu New Material Technology Co ltd
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Priority to CN202110334736.2A priority Critical patent/CN113084154A/en
Publication of CN113084154A publication Critical patent/CN113084154A/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
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14Treatment of metallic powder
    • 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
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • B22F1/0547Nanofibres or nanotubes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B11/00Obtaining noble metals
    • C22B11/04Obtaining noble metals by wet processes

Abstract

The invention discloses a method for efficiently purifying a nano silver wire, which is characterized by comprising the following steps: the method comprises the following five steps. According to the method for efficiently purifying the nano silver wire, the solubility or the dissolving capacity of the surface PVP of the nano silver wire in different solvents is different, and a multiphase interface is formed by adding different organic solvents, so that the PVP is dissolved in another solvent or a plurality of solvents more quickly, and the separation such as particle removal and the like of the nano silver wire is caused by the interface driving force for dissolving more quickly; by using the non-acetone organic solvent which does not dissolve PVP and is insoluble in water, water and the organic solvent are used in the purification, the silver wire coated with the PVP is only dissolved in water and is not dissolved in the solvent, the silver wire and the nanoparticles have different surface areas and different surface energies, so that more silver surfaces are exposed after the PVP of the silver wire is dissolved, more interface driving forces are obtained, the silver wire can quickly enter the organic solvent, the silver wire and the silver particles are separated, and the purification efficiency is effectively improved.

Description

Method for efficiently purifying nano silver wires
Technical Field
The invention relates to the technical field of nano silver wire purification, in particular to a method for efficiently purifying a nano silver wire.
Background
A nanowire is a line of nanometer scale (1 nm ═ 10^ -9 meters), which can be defined as a one-dimensional structure with limits below 100 nm in the lateral direction (without limits in the longitudinal direction), and can be used to make ultra-small circuits as an important component of nanotechnology. The silver nanowires have excellent light transmittance and flexibility resistance due to a nano-scale size effect, in addition to excellent conductivity of silver. Therefore, the material is considered to be the most possible material for replacing the traditional ITO transparent electrode, provides possibility for realizing flexible and bendable LED display, touch screens and the like, and has a great deal of research on applying the material to thin-film solar cells;
after the silver nanowires are synthesized, a series of impurity particles such as particles, short rods or thick wires exist, the performance of the transparent conductive film coated on the silver nanowires is greatly related to the purification after the silver nanowires are synthesized, the surfaces of the silver nanowires after the silver nanowires are synthesized are coated with the pvp, and the conductivity of the obtained silver nanowires is seriously affected due to the existence of more impurities, so that the performance of the silver nanowires is greatly reduced, and therefore the silver nanowires coated with the pvp need to be purified.
Disclosure of Invention
The invention aims to provide a method for efficiently purifying a nano silver wire so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for efficiently purifying a nano silver wire is characterized by comprising the following steps: the method comprises the following five steps:
the method comprises the following steps: preparing 80% of acetone organic solvent according to a certain proportion;
step two: obtaining a toluene solvent, a hydrocarbon solvent and a carbon tetrachloride solvent;
step three: putting the PVC-coated nano silver wire into a prepared acetone organic solvent, and oscillating to perform mixed reaction on the acetone organic solvent and the PVC-coated nano silver wire;
step four: adding distilled water after the acetone organic solvent reacts with the PVC-coated nano silver wire, and dissolving the silver wire in water through oscillation reaction;
step five: the toluene solvent, the hydrocarbon solvent and the carbon tetrachloride solvent silver wire are respectively added for reaction, the silver wire coated with the pvp is insoluble in the solvent, and the pvp is dissolved in another solvent or a plurality of solvents more quickly, so that the silver nanowire is subjected to particle removal and the like for separation.
Further, the acetone organic solution was prepared by weighing 101.5ml of acetone into a cylinder according to the specific gravity of acetone equal to 0.788 in 100ml of distilled water and a measuring cylinder, and shaking to prepare an 80% acetone organic solution, wherein the volume formula of the required acetone was (100 × 80%)/1000 × 0.788 — 101.5 ml.
Further, after the surface of the synthesized nano silver wire is coated with PVP and contacted with an acetone organic solvent, a multiphase interface is generated, and the surface of the nano silver wire is larger than that of particles and short rods.
Further, the pvc-coated silver wire is dissolved in water by adding distilled water in a volume 3 to 6 times that of the acetone organic solvent and shaking or shaking using a shaker.
Furthermore, the added toluene solvent, hydrocarbon solvent and carbon tetrachloride solvent make the solubility or dissolving capacity of the pvp on the surface of the nano silver wire different in different solvents through different solvents, make the dissolution of the pvp faster in various solvents, and the faster interface driving force of the dissolution causes the de-graining separation of the nano silver wire.
Compared with the prior art, the invention has the beneficial effects that: according to the method for efficiently purifying the nano silver wire, different organic solvents are added by utilizing different solubilities or dissolving capacities of the surface PVP of the nano silver wire in different solvents to form a multiphase interface, the specific surface of the nano silver wire is large, compared with particles and short rods, PVP is dissolved in another solvent or solvents more quickly, and the particle removal and other separation of the nano silver wire are caused by the interface driving force for dissolving more quickly; by utilizing the non-acetone organic solvent which can not dissolve PVP and is insoluble in water, toluene, benzene, carbon tetrachloride and the like, because a large amount of PVP is coated on the surface of the synthesized silver, water and the organic solvent are used for purification, the silver wire coated with the PVP is only soluble in water and is insoluble in the solvent, the silver wire and the nano particles have different surface areas and different surface energies, more silver surfaces are exposed after the PVP of the silver wire is dissolved, more interface driving force is obtained, the silver wire can quickly enter the organic solvent, the silver wire and the silver particles are separated, and the purification efficiency is effectively improved.
Drawings
FIG. 1 is a schematic flow chart of the method for efficiently purifying the silver nanowires of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "front", "rear", "both ends", "one end", "the other end", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "connected," and the like are to be construed broadly, such as "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1
Referring to fig. 1, an embodiment of the present invention: a method for efficiently purifying a nano silver wire is characterized by comprising the following steps: the method comprises the following five steps:
the method comprises the following steps: preparing 80% of acetone organic solvent according to a certain proportion;
step two: obtaining a toluene solvent, a hydrocarbon solvent and a carbon tetrachloride solvent;
step three: putting the PVC-coated nano silver wire into a prepared acetone organic solvent, and oscillating to perform mixed reaction on the acetone organic solvent and the PVC-coated nano silver wire;
step four: adding distilled water after the acetone organic solvent reacts with the PVC-coated nano silver wire, and dissolving the silver wire in water through oscillation reaction;
step five: the toluene solvent, the hydrocarbon solvent and the carbon tetrachloride solvent silver wire are respectively added for reaction, the silver wire coated with the pvp is insoluble in the solvent, and the pvp is dissolved in another solvent or a plurality of solvents more quickly, so that the silver nanowire is subjected to particle removal and the like for separation.
Further, the preparation method of the acetone organic solution is that 100ml of distilled water is put into a measuring cylinder according to the specific gravity of acetone equal to 0.788, 101.5ml of acetone raw material is weighed by an electronic scale and is led into the measuring cylinder to be mixed with the distilled water, and the acetone is uniformly mixed with the distilled water in a shaking mode, so that the 80% acetone organic solution can be prepared, the volume formula of the needed acetone is (100 x 80%)/1000 x 0.788 ═ 101.5ml, the amount of the acetone can be conveniently obtained through the formula calculation, and the acetone can be conveniently weighed.
Further, the surface of the silver nanowire after synthesis is coated with PVP, and after the silver nanowire is contacted with an acetone organic solvent, substances insoluble in the acetone organic solvent can be separated out, so that a multiphase interface can be generated, and the surface of the silver nanowire is larger than that of particles and short rods, so that the silver nanowire can be initially separated from the particles.
Further, the pvc-coated silver wire is dissolved in water by adding distilled water in a volume 3 to 6 times that of the acetone organic solvent and shaking or shaking using a shaker.
Furthermore, the added toluene solvent, hydrocarbon solvent and carbon tetrachloride solvent make the solubility or dissolving capacity of the pvp on the surface of the nano silver wire different in different solvents through different solvents, so that the dissolution of the pvp can be faster under the condition of various solvents, and the faster dissolving interface driving force causes the nano silver wire to remove particles and other impurities for separation, thereby effectively improving the purification efficiency.
Example 2
When the purification is carried out, the prepared acetone organic solvent is guided into a prepared container with scale marks, so that the dosage can be conveniently mastered according to the scale marks, then putting the synthesized nano silver wire coated with PVP into a container to make the nano silver wire contact with an acetone organic solvent for reaction, shaking the container for 2-3min to make the nano silver wire fully contact with the acetone organic solvent, adding distilled water, the amount of the distilled water is required to be taken into account when the distilled water is introduced, then the container is kept stand for 3-4min, then the toluene solvent, the hydrocarbon solvent and the carbon tetrachloride solvent are respectively added in sequence, through rocking the nanometer silver line that makes the cladding have PVP and various solvents carry out misce bene, through the reaction of PVP and various solvents, can separate silver line and silver particle for quick relatively, utilize microporous filter to filter, can effectual improvement purification effect.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (5)

1. A method for efficiently purifying nano silver wires is characterized by comprising the following steps: the method comprises the following five steps:
the method comprises the following steps: preparing 80% of acetone organic solvent according to a certain proportion;
step two: obtaining a toluene solvent, a hydrocarbon solvent and a carbon tetrachloride solvent;
step three: putting the PVC-coated nano silver wire into a prepared acetone organic solvent, and oscillating to perform mixed reaction on the acetone organic solvent and the PVC-coated nano silver wire;
step four: adding distilled water after the acetone organic solvent reacts with the PVC-coated nano silver wire, and dissolving the silver wire in water through oscillation reaction;
step five: the toluene solvent, the hydrocarbon solvent and the carbon tetrachloride solvent silver wire are respectively added for reaction, the silver wire coated with the pvp is insoluble in the solvent, and the pvp is dissolved in another solvent or a plurality of solvents more quickly, so that the silver nanowire is subjected to particle removal and the like for separation.
2. The method for efficiently purifying the nano silver wire according to claim 1, wherein the method comprises the following steps: the acetone organic solution is prepared by weighing 101.5ml of acetone into a cylinder according to the specific gravity of the acetone equal to 0.788, and then shaking to prepare the 80% acetone organic solution, wherein the volume formula of the required acetone is (100: 80%)/1000: 0.788: 101.5 ml.
3. The method for efficiently purifying the nano silver wire according to claim 1, wherein the method comprises the following steps: after the nano silver wire is synthesized, the surface is coated with PVP and is contacted with an acetone organic solvent, a multiphase interface is generated, and the surface of the nano silver wire is larger than particles and short rods.
4. The method for efficiently purifying the nano silver wire according to claim 1, wherein the method comprises the following steps: the pvc-coated silver wire is dissolved in water by adding distilled water in a volume 3 to 6 times that of the acetone organic solvent and shaking or shaking using a shaker.
5. The method for efficiently purifying the nano silver wire according to claim 1, wherein the method comprises the following steps: the added toluene solvent, hydrocarbon solvent and carbon tetrachloride solvent lead the solubility or dissolving capacity of the pvp on the surface of the nano silver wire to be different in different solvents through different solvents, lead the dissolution of the pvp to be faster in various solvents, and lead the nano silver wire to be separated by removing particles and the like through the interface driving force for dissolving the pvp faster.
CN202110334736.2A 2021-03-29 2021-03-29 Method for efficiently purifying nano silver wires Pending CN113084154A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120148861A1 (en) * 2010-12-09 2012-06-14 Whitcomb David R Nanowire preparation methods, compositions, and articles
CN105345022A (en) * 2015-10-22 2016-02-24 东华大学 Purification method for silver nanowire
CN106068166A (en) * 2014-03-07 2016-11-02 同和控股(集团)有限公司 The manufacture method of nano silver wire and nano silver wire and use the ink of this nano silver wire
CN107598152A (en) * 2017-08-30 2018-01-19 浙江科创新材料科技有限公司 A kind of method of purification of nano silver wire
CN109311087A (en) * 2016-06-02 2019-02-05 同和电子科技有限公司 Silver nanowires and its manufacturing method and silver nanowires ink and transparent conductive film
CN111217389A (en) * 2020-01-08 2020-06-02 苏州星烁纳米科技有限公司 Nanowire processing method and nanowire
CN111715877A (en) * 2020-05-22 2020-09-29 深圳市华科创智技术有限公司 Method for purifying nano silver wire
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Patent Citations (8)

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US20120148861A1 (en) * 2010-12-09 2012-06-14 Whitcomb David R Nanowire preparation methods, compositions, and articles
CN106068166A (en) * 2014-03-07 2016-11-02 同和控股(集团)有限公司 The manufacture method of nano silver wire and nano silver wire and use the ink of this nano silver wire
CN105345022A (en) * 2015-10-22 2016-02-24 东华大学 Purification method for silver nanowire
CN109311087A (en) * 2016-06-02 2019-02-05 同和电子科技有限公司 Silver nanowires and its manufacturing method and silver nanowires ink and transparent conductive film
CN107598152A (en) * 2017-08-30 2018-01-19 浙江科创新材料科技有限公司 A kind of method of purification of nano silver wire
FR3098134A1 (en) * 2019-07-02 2021-01-08 Commissariat A L'energie Atomique Et Aux Energies Alternatives Process for the purification of metallic nanowires
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CN111715877A (en) * 2020-05-22 2020-09-29 深圳市华科创智技术有限公司 Method for purifying nano silver wire

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Application publication date: 20210709

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