CN106238718A - The method of Processing Ag nano wire and nano silver wire - Google Patents
The method of Processing Ag nano wire and nano silver wire Download PDFInfo
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- CN106238718A CN106238718A CN201610562026.4A CN201610562026A CN106238718A CN 106238718 A CN106238718 A CN 106238718A CN 201610562026 A CN201610562026 A CN 201610562026A CN 106238718 A CN106238718 A CN 106238718A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention proposes the method for Processing Ag nano wire.The method includes: exist protectant under the conditions of, make the solution containing described nano silver wire contact with silver halide lytic agent, in order to remove silver halide.Thus, it is possible to conveniently and effectively remove the impurity particle in nano silver wire product, such that it is able to improve the electricity of nano silver wire, mechanics and optical property.
Description
Technical field
The present invention relates to Material Field, in particular it relates to the method for Processing Ag nano wire and nano silver wire.
Background technology
Transparent conductor can apply to such as contact panel (touch panel), liquid crystal display (liquid because of it
Crystal display), thin film photocell (thin film photovoltaic cells) and organic light emitting diode device
Fields such as (organic light emitting diode devices), its demand increases year by year.At present, electrically conducting transparent material
Material is main with tin indium oxide (indium tin oxide, ITO).But the transparent conductor containing ITO is due to material cause, its property
There is many restrictions in energy and yield.Therefore, occur in that at present using nano silver wire substitute ITO as conductive material prepare transparent
Conductor.Compared with ITO, nano silver wire not only has good optics, electricity and mechanical property, also has metal nanometer line ratio
Surface area is big and the feature such as quantum size effect.The method of synthesis of silver nano-wire mainly has alcohol full-boiled process, hydro-thermal method, template at present
With the method such as self-assembly method, polyol process.
But, the current method of Processing Ag nano wire and the nano silver wire of acquisition still have much room for improvement.
Summary of the invention
The present invention be based on inventor on the fact that and the discovery of problem and understanding make:
At present, utilize nano silver wire prepared by the method for polyol process, generally there is conductivity, the transparency is poor etc. asks
Topic.Inventor finds through further investigation and great many of experiments, and this is due to the nano silver wire of the method synthesis, deposits in its product
At many impurity particles.Inventor confirms through great many of experiments, in above-mentioned impurity particle, is mainly composed of silver halide.Silver halide
Electric conductivity and the transparency are the most poor, therefore result in nano silver wire second-rate of the method synthesis.And the life of silver halide
Become, cause as nucleation controlling agent mainly due to needing interpolation halide salt in building-up process.The most current is polynary
In the method for alcohol reduction preparation of silver nano wire, it is difficult to avoid the generation of above-mentioned impurity particle, centrifugation can only be passed through in the later stage
Etc. method, impurity particle is separated.But, separation process is the most time-consuming, in addition it is also necessary to controlled by many conditions,
And separating effect is unsatisfactory.
It is contemplated that at least solve one of technical problem present in prior art.To this end, the present invention proposes process
The method of nano silver wire.According to embodiments of the invention, the method includes: exist protectant under the conditions of, make containing described
The solution of nano silver wire contacts with silver halide lytic agent, in order to remove silver halide.Thus, it is possible to conveniently and effectively remove silver nanoparticle
Impurity particle in line product, such that it is able to improve the electricity of nano silver wire, mechanics and optical property.
According to embodiments of the invention, described protective agent is polyvinylpyrrolidone, polyvinyl alcohol, chloro-hexadecane base pyrrole
At least one pyridine and cetyl trimethylammonium bromide.Thus, it is possible to effectively protection nano silver wire is not molten by silver halide
Solve the corrosion of agent, such that it is able to improve the quality of the nano silver wire utilizing the method to process further.
According to embodiments of the invention, described protective agent is 1:100 with the mass ratio of the described solution containing nano silver wire
To 1:10000.Thus, it is possible to effectively play the effect of protection nano silver wire, protective agent excess it is possible to prevent again to cause waste
And affect the performance of nano silver wire.
According to embodiments of the invention, described silver halide lytic agent contains thiosulfate ion, thiocyanate, cyanogen root, ammonia
At least one base, ethylenediamine ion and EDTA.Thus, it is possible to improve silver halide lytic agent further to dissolve the effect of silver halide
Rate and effect.
According to embodiments of the invention, determine the amount of the described silver chloride lytic agent of addition according to the amount of described silver halide.
Thus, it is possible to prevent silver halide from removing not exclusively, or silver halide lytic agent excess and corrode nano silver wire.
According to embodiments of the invention, described silver halide lytic agent is 1:1 to 2:1 with the mol ratio of described silver halide.By
This, can improve efficiency and the effect utilizing the method Processing Ag nano wire further.
According to embodiments of the invention, described contact is under agitation carried out.It is somebody's turn to do thus, it is possible to improve further to utilize
The efficiency of method Processing Ag nano wire and effect.
Time of contact according to embodiments of the invention, the described solution containing nano silver wire and described silver halide lytic agent
It it is 5～120 minutes.Thus, it is possible to make silver halide lytic agent fully react with silver halide impurity particle.
According to embodiments of the invention, the method farther includes: (a) is to the silver nanoparticle containing described silver halide lytic agent
Line solution is centrifuged processing, and retains precipitation；B () adds water in described precipitation and stirs, carry out the aqueous solution of described precipitation
Secondary centrifuging processes；And (c) is repeated several times step (b).Thus, it is possible to remove silver halide lytic agent.
In another aspect of this invention, the present invention proposes a kind of nano silver wire.According to embodiments of the invention, described silver
Nano wire utilizes foregoing method to process and obtain.
Accompanying drawing explanation
Fig. 1 shows the optical microscope photograph of the embodiment of the present invention 1 nano silver wire before treatment；
Fig. 2 shows the optical microscope photograph of the nano silver wire after the embodiment of the present invention 1 process；
Fig. 3 shows the optical microscope photograph of the embodiment of the present invention 2 nano silver wire before treatment；And
Fig. 4 shows the optical microscope photograph of the nano silver wire after the embodiment of the present invention 2 process.
Detailed description of the invention
Embodiments of the invention are described below in detail, and the example of described embodiment is shown in the drawings, the most from start to finish
Same or similar label represents same or similar element or has the element of same or like function.Below with reference to attached
The embodiment that figure describes is exemplary, is only used for explaining the present invention, and is not considered as limiting the invention.
In one aspect of the invention, a kind of method that the present invention proposes Processing Ag nano wire.Reality according to the present invention
Executing example, the method includes: exist protectant under the conditions of, make the solution (nano silver wire solution) containing nano silver wire and halogenation
Silver lytic agent contact, in order to remove silver halide.Thus, it is possible to conveniently and effectively remove the impurity particle in nano silver wire, thus
The electricity of nano silver wire, mechanics and optical property can be improved.
Understanding for convenience, the principle that the method removes silver halide first below is briefly described:
In the present invention, in the silver halide lytic agent of employing, containing forming complex with the silver ion in silver halide
B-Anion.Therefore, after silver halide lytic agent being joined in the nano silver wire solution containing silver halide impurity, halogenation
Silver lytic agent can occur to react as follows with silver halide:
AgX+B-=[AgB]-+X-
Wherein, X is halide anion, for example, it is possible to be Cl, Br or I at least one.Enforcement according to the present invention
Example, silver halide lytic agent can contain thiosulfate ion, thiocyanate, cyanogen root, amino, ethylenediamine ion and EDTA extremely
One of few.Above-mentioned ion or group have preferably and silver ion carries out the ability of complexation, thus, it is possible to improve halogenation further
Silver lytic agent dissolves efficiency and the effect of silver halide.
According to embodiments of the invention, in the method, addition can be determined according to the amount of silver halide in nano silver wire
The amount of silver chloride lytic agent.Thus, it is possible to prevent silver halide from removing not exclusively, or silver halide lytic agent excess and corrode silver and receive
Rice noodle.Concrete, silver halide lytic agent can be (2～1) with the mol ratio of silver halide: 1.In the method, the amount of silver halide
Can be determined according to the amount of the nucleation controlling agent that can produce silver halide impurity added in nano silver wire synthetic method.Send out
A person of good sense finds through further investigation and great many of experiments, and the composition of the impurity particle contained in nano silver wire product is complex,
Outside removing silver halide, possibly together with other compositions.But utilize above-mentioned silver halide lytic agent that nano silver wire solution is processed, permissible
Making the nano silver wire quality after process significantly improve, the nano silver wire surface after process is relatively smooth, and to the Yin Na after processing
The physical property of rice noodle detects, and its electric conductivity, light transmission all improve a lot, and can meet and prepare wanting of transparent conductor
Ask.This is likely due to silver halide lytic agent during reacting with silver halide, reduces owing to having dissolved silver halide precipitation
The size of impurity particle, hence in so that impurity particle waits routine operation to remove easily by washing is centrifugal, and reduces impurity
Active force between granule and nano silver wire so that impurity particle is not easy to be attached on nano silver wire.Therefore, this Processing Ag is received
The method of rice noodle only needs to add silver halide lytic agent, can obtain the effect preferably removing impurity particle, and without analyzing
All the components in impurity particle, and process one by one for each composition.
Inventor finds through great many of experiments, although above-mentioned silver halide lytic agent can effectively dissolve silver halide, but also holds
Easily nano silver wire is caused corrosion.Therefore, according to embodiments of the invention, can be before adding silver halide lytic agent, in advance
Protective agent is added in nano silver wire solution.Specifically, protective agent can include polyvinylpyrrolidone, polyvinyl alcohol, chloro
Cetyl pyridinium and cetyl trimethylammonium bromide etc..Such as, according to a particular embodiment of the invention, can add
Before silver halide lytic agent, in the solution containing nano silver wire, add polyvinylpyrrolidone (PVP) in advance.Inventor passes through
Great many of experiments finds, polyvinylpyrrolidone can be that nano silver wire offer is effectively protected, and utilizes polyol reduction method
The growth adding PVP to promote nano silver wire is needed during the nano silver wire of preparation.Therefore, many for using when nano silver wire
When unit's alcohol reducing process prepares, it is not necessary to remove the PVP contained in product (containing the solution of nano silver wire), can directly produce
Thing adds silver halide lytic agent and carries out the removing of silver halide.Thus, it is possible to effectively protection nano silver wire is not by halogenation
The corrosion of silver lytic agent, such that it is able to improve the quality of the nano silver wire utilizing the method to process further.Inventor is through excessive
Amount experiment finds, protective agent can be 1:(100～10000 with the mass ratio of the solution containing nano silver wire).Thus, it is possible to have
Effect plays the effect of protection nano silver wire, is possible to prevent again protective agent excess cause waste and affect the performance of nano silver wire.
It will be appreciated to those of skill in the art that when in the solution containing nano silver wire containing PVP, PVP can be selected as guarantor
Protect agent, when PVP amount is not enough, only need to additionally add a part, make protective agent full with the mass ratio of the solution containing nano silver wire
The above-mentioned scope of foot.
It will be appreciated to those of skill in the art that owing to nano silver wire has less diameter and bigger length,
Therefore it is susceptible to reunite.And after nano silver wire is reunited, it is difficult to dispersed in medium (such as water equal solvent) again, because of
Among this transparent conductor prepared, it is difficult to ensure the dispersed of nano silver wire, thus affect electric conductivity in transparent conductor with
And the unification of optical property.Inventor is found surprisingly that, nano silver wire is processed by the method utilizing the present invention to propose, not only
The impurity particle on nano silver wire surface can be removed, and the nano silver wire obtained will not be reunited, additionally it is possible to be dispersed in
In medium, thereby may be ensured that the quality of the transparent conductor of follow-up preparation.
According to embodiments of the invention, in order to improve the efficiency and effect utilizing the method Processing Ag nano wire further
Really, mixing can be stirred, in order to protective agent adsorbs equably after being joined in nano silver wire solution by protective agent
Nano silver wire surface, thus prevent silver halide lytic agent from nano silver wire is caused corrosion in subsequent step.Silver halide is molten
After solution agent addition contains in protectant nano silver wire solution, it is stirred so that silver halide lytic agent fully and is attached to silver
The silver halide contact of nanowire surface, such that it is able to make silver halide lytic agent fully react with silver halide.Thus, it is possible to further
Improve efficiency and the effect utilizing the method Processing Ag nano wire.
According to embodiments of the invention, nano silver wire solution was not particularly limited with the time of contact of silver halide lytic agent,
As long as can make silver halide lytic agent fully and silver halide generation complex reaction dissolved impurity granule.According to the present invention's
Specific embodiment, can under conditions of stirring, make silver halide lytic agent with containing protectant nano silver wire solution reaction 5～
120 minutes.Thus, it is possible to make silver halide lytic agent fully react with silver halide.
According to embodiments of the invention, after silver halide lytic agent fully reacts with silver halide, containing protectant silver
Nanowire solution reacts complex, halide ion and the remaining silver halide generated containing silver ion and silver halide lytic agent
The impurity components such as lytic agent.In order to improve the effect utilizing the method Processing Ag nano wire further, the method can also enter one
Step includes the step removing silver halide lytic agent.Owing to silver halide lytic agent dissolubility in water is higher, and silver ion is formed
Complex and halide ion can also be dissolved in water, therefore, removing above-mentioned impurity component can be by simple centrifugation
Realize.Specifically, according to embodiments of the invention, the removing of above-mentioned impurity can realize through the following steps:
(a) centrifugal treating
According to embodiments of the invention, in this step, the nano silver wire solution containing silver halide lytic agent is carried out from
The heart processes, and retains precipitation.Centrifugal treating can make the nano silver wire of solid-state divide with the solvent (water) in solution and soluble impurity
From, nano silver wire forms precipitation after centrifugal treating.In this step, the parameter such as the time of centrifugal treating, rotating speed is by especially
Limiting, those skilled in the art can be carried out according to parameters such as the content of nano silver wire, the diameter of nano silver wire, length in solution
Design, as long as can be by nano silver wire by being centrifugation down.
B () repeated centrifugation processes
Inventor finds through great many of experiments, owing to nano silver wire has less diameter and bigger length, many
Easily adsorbing a part of solution between root nano silver wire, therefore silver ion complex, halide ion and remaining silver halide are molten
Solve agent to be difficult to be processed by single spin separate with nano silver wire.According to embodiments of the invention, can be formed in centrifugal treating
Precipitation in add water and stir, then the aqueous solution formed is carried out secondary centrifuging process, retains precipitation, and this is repeated several times
Process.By repeatedly centrifugal treating, can fully remove absorption silver ion complex between nano silver wire, halide ion with
And the impurity such as remaining silver halide lytic agent, such that it is able to improve the effect utilizing the method Processing Ag nano wire further.Close
In the number of times that repeated centrifugation processes, those skilled in the art can be adjusted according to practical situation.Specifically, according to the present invention
Embodiment, can by repeated centrifugation process 2～3 times, complete the removing of above-mentioned impurity.
In sum, the method for Processing Ag nano wire proposed by the invention have following advantages at least one:
1, with low cost, the reagent used is common agents, and required raw material sources extensively and is readily available.
2, the method is easy and simple to handle, it is not necessary to loaded down with trivial details step can realize the raising of nano silver wire quality, and processing procedure
Quickness and high efficiency, processing technique will not impact nano silver wire production process.
3, this processing method can effectively obtain the nano silver wire that quality is higher, and processing procedure is not result in nano silver wire
Reunion, it is possible to be effectively improved conduction and the light transmission of nano silver wire.
4, the method can complete the process of nano silver wire without the extra production equipment that adds, and does not receives existing production silver
The technological process of rice noodle impacts, beneficially large-scale promotion application.
In another aspect of this invention, the present invention proposes a kind of nano silver wire.According to embodiments of the invention, this silver is received
Rice noodle utilizes foregoing method to process and obtain.Therefore, this nano silver wire has and utilizes foregoing side
Method processes whole features and the advantage that the nano silver wire obtained is had, and does not repeats them here.Generally speaking, this nano silver wire
Have the advantages such as low production cost, electric conductivity height, good, the nano wire not reunion of light transmission at least one.
Below by specific embodiment, the present invention will be described, it will be appreciated to those of skill in the art that following
The purpose that is merely to illustrate that of specific embodiment, and limit the scope of the present invention never in any form.It addition, below
Embodiment in, unless stated otherwise, the material and facility used is all commercially available.If in embodiment below
In, concrete treatment conditions and processing method are not expressly recited, then can use condition as known in the art and side
Method processes.In the examples below that, the nano silver wire of process is to use conventional polyol reducing process to prepare.
Embodiment 1
The preparation process of nano silver wire is with method disclosed in documents below:
Xiping Zeng,et al,Structural dependence of silver nanowires on
polyvinyl pyrrolidone(PVP)chain length,Nanotechnology,Volume 25,Number 49,
2014
With reference to Fig. 1, a diameter of about 80nm of prepared nano wire, and diameter Distribution is uniform, a length of 30 μm.And it is micro-
Microscopic observation is to impurity particle containing about 5% in nano silver wire.Take in the solution that 100ml synthesis obtains and add 0.1wt%
PVP, be uniformly mixed, add 0.1wt% thiosulfuric acid sodium salt, stir and react 10 minutes.Subsequently, to adding sulfur
The solution of sodium thiosulfate is centrifuged processing, rotating speed 5000rpm, centrifugation time 20min.Retain precipitation, add 100ml water the most molten
Repeating above-mentioned centrifugally operated 3 times after solution, the final precipitation obtained is dissolved in water and is configured to aqueous solution, in order to complete the place of nano silver wire
Reason.With reference to Fig. 2, treated nano silver wire purity has and the most significantly improves, and examines under a microscope less than the most miscellaneous
Matter granule, and the holding of nano silver wire surface topography is good, is not corroded and soilless sticking phenomenon.
Embodiment 2
Nano silver wire preparation method with embodiment 1, except that, the consumption of temperature and PVP is adjusted, makes system
A diameter of about 60nm of the nano wire obtained, average length 20 μm.With reference to Fig. 3, can see the microscope photograph of nano silver wire
Go out, this nano silver wire contains the impurity particle of about 2%.Take the polyvinylpyrrolidone adding 0.1wt% in 100ml solution
(PVP), after stirring, after adding 0.01wt%EDTA stirring 10 minutes, being centrifuged separating, centrifugal treating parameter is with implementing
Example 1.Take precipitation and add centrifugation again after 100ml water stirs, to remove remaining EDTA, purification aftereffect after being repeated 3 times
Fruit is as shown in Figure 4.Treated nano silver wire purity has and the most significantly improves, and examines under a microscope less than the most miscellaneous
Matter granule, and the holding of nano silver wire surface topography is good, is not corroded and soilless sticking phenomenon.
Thus, it is possible to prove, method proposed by the invention, the nano silver wire for different-diameter, length is respectively provided with relatively
Good treatment effect, it is possible to effectively remove the nano silver wire pattern after the impurity particle on nano silver wire surface, and process and keep good
Good, soilless sticking phenomenon and without the phenomenon that is substantially corroded.
In the description of this specification, reference term " embodiment ", " some embodiments ", " specific embodiment ", " show
Example " or the description of " some examples " etc. means to combine this embodiment or example describes specific features, structure, material or feature
It is contained at least one embodiment or the example of the present invention.In this manual, the schematic representation of above-mentioned term is differed
Surely identical embodiment or example are referred to.And, the specific features of description, structure, material or feature can be any
One or more embodiments or example combine in an appropriate manner.
Although an embodiment of the present invention has been shown and described, it will be understood by those skilled in the art that: not
These embodiments can be carried out multiple change in the case of departing from the principle of the present invention and objective, revise, replace and modification, this
The scope of invention is limited by claim and equivalent thereof.
Claims (10)
1. the method for a Processing Ag nano wire, it is characterised in that including:
Exist protectant under the conditions of, make the solution containing described nano silver wire contact with silver halide lytic agent, in order to remove
Silver halide.
Method the most according to claim 1, it is characterised in that described protective agent includes polyvinylpyrrolidone, polyethylene
At least one alcohol, halogenated phosphates and cetyl trimethylammonium bromide.
Method the most according to claim 1, it is characterised in that described protective agent and the described solution containing nano silver wire
Mass ratio is 1:100 to 1:10000.
Method the most according to claim 1, it is characterised in that described silver halide lytic agent contain thiosulfate ion,
At least one thiocyanate, cyanogen root, amino, ethylenediamine ion and EDTA.
Method the most according to claim 1, it is characterised in that determine the described chlorination of addition according to the amount of described silver halide
The amount of silver lytic agent.
Method the most according to claim 5, it is characterised in that described silver halide lytic agent and the mol ratio of described silver halide
For 1:1 to 2:1.
Method the most according to claim 1, it is characterised in that described contact is under agitation carried out.
Method the most according to claim 1, it is characterised in that the described solution containing nano silver wire is molten with described silver halide
The time of contact solving agent is 5～120 minutes.
Method the most according to claim 1, it is characterised in that farther include:
A nano silver wire solution containing described silver halide lytic agent is centrifuged processing by (), retain precipitation；
B () adds water in described precipitation and stirs, the aqueous solution of described precipitation is carried out secondary centrifuging process；And
C () is repeated several times step (b).
10. a nano silver wire, it is characterised in that described nano silver wire is to utilize the method described in any one of claim 1～9
Carry out processing and obtaining.
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| WO2020019384A1 (en) * | 2018-07-27 | 2020-01-30 | 深圳市华科创智技术有限公司 | Silver nano ring preparation method |
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