CN111217389A - Nanowire processing method and nanowire - Google Patents

Nanowire processing method and nanowire Download PDF

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CN111217389A
CN111217389A CN202010016795.0A CN202010016795A CN111217389A CN 111217389 A CN111217389 A CN 111217389A CN 202010016795 A CN202010016795 A CN 202010016795A CN 111217389 A CN111217389 A CN 111217389A
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nanowire
nanowires
gas
solution
carbonate
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马金锁
王允军
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Suzhou Xingshuo Nanotech Co Ltd
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Suzhou Xingshuo Nanotech Co Ltd
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    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00—Selenium; Tellurium; Compounds thereof
    • C01B19/007—Tellurides or selenides of metals
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    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/0632—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with gallium, indium or thallium
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    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/08—Other phosphides
    • C01B25/082—Other phosphides of boron, aluminium, gallium or indium
    • C01B25/087—Other phosphides of boron, aluminium, gallium or indium of gallium or indium
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    • C01B32/00—Carbon; Compounds thereof
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/02—Silicon
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
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    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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    • C01G23/00—Compounds of titanium
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    • C01G23/047—Titanium dioxide
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    • C01P2004/00—Particle morphology
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    • C01P2004/02—Particle morphology depicted by an image obtained by optical microscopy
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    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer

Abstract

The invention discloses a method for processing nanowires, which comprises the steps of providing a nanowire solution; a gas is generated in the nanowire solution, which separates the nanowires from each other, or which prevents the nanowires from being doubled or knotted. This application is through producing gas in the nanowire solution, and gas can make the nanowire alternate segregation, when having the nanowire of knoing and/or doubling in the nanowire solution, gas can make the nanowire alternate segregation of doubling or knoing to the problem of metal nanowire in the purification process because of vibrating and stirring etc. operation appear knoing in a large number and doubling has been solved.

Description

Nanowire processing method and nanowire
Technical Field
The present application relates to the field of nanotechnology, and in particular, to a method for processing nanowires and nanowires.
Background
Currently prepared nanowires, e.g., silver nanowires, can contain many impurities, e.g., silver nanoparticles of different sizes.
Therefore, after the crude product containing silver nanowires is prepared, separation and purification are generally required, and the existing purification of silver nanowires mainly comprises washing the crude product of silver nanowires with acetone. Because acetone and water are miscible, but the silver nanowires in the crude product are coated with polyvinylpyrrolidone (PVP), and the silver nanowires coated with the polyvinylpyrrolidone (PVP) are insoluble in acetone, so that the excessive acetone can lead the silver nanowires to be aggregated and precipitated. By pumping away the acetone and water, the impurities (silver particles, PVP and unreacted ionic Cl) mixed in the acetone and water can be removed-,Br-,Ag+) And (5) removing. Then the silver nanowire sediment coated with PVP is redispersed in water, and the silver nanowires agglomerated together can be slowly redispersed in water by shaking and stirring. The above operation is repeated a plurality of times, for example, 3 times or more, and impurities in the silver nanowires can be removed.
However, in the experiment, it was found that during the re-dispersion of the silver nanowire precipitation like dough, it was found by an electron microscope that the silver nanowires were largely knotted and doubled due to operations such as shaking and stirring of the re-dispersion, especially for ultra-fine silver nanowires (particle size less than 40nm, more preferably, particle size less than 20 nm).
When the silver nanowires are used as the transparent electrode material, the knotted and/or doubled silver nanowires can scatter visible light, so that the transmittance of the transparent electrode material is reduced, the haze of the transparent electrode material is increased, and the optical performance of the transparent conductive material is reduced.
Therefore, in order to further meet the market requirement for higher photoelectric property of the silver nanowires, solving the problem of knotting and doubling of the silver nanowires in the purification process is an increasingly sought target by researchers and enterprises.
Disclosure of Invention
In view of the above problems, the present application provides a method for processing nanowires, which can solve the knotting and merging problems of nanowires.
One aspect of the present application provides a method for processing a nanowire, the method comprising the steps of:
providing a nanowire solution;
a gas is generated in the nanowire solution, which separates the nanowires from each other, or which prevents the nanowires from being doubled or knotted.
Preferably, the processing method further comprises the steps of:
knotted and/or doubled nanowires exist in the nanowire solution;
the gas separates the doubled or knotted nanowires from each other.
Preferably, the generating of the gas in the nanowire solution comprises:
physical and/or chemical methods generate the gas.
Preferably, the chemically generating a gas in the nanowire solution includes:
and adding a first reactant and a second reactant into the nanowire solution, wherein the first reactant and the second reactant react to generate gas.
Preferably, the first reactant is a carbonate and the second reactant is a weak acid.
Preferably, the carbonate salt comprises at least one of a normal carbonate salt, a basic carbonate salt or a bicarbonate salt.
Preferably, the carbonate includes at least one of sodium carbonate, sodium bicarbonate, lithium carbonate, lithium bicarbonate, magnesium carbonate, calcium carbonate, potassium carbonate, or potassium bicarbonate.
Preferably, the weak acid comprises a carboxylic acid.
Preferably, the carboxylic acid comprises acetic acid.
Preferably, the chemically generating a gas in the nanowire solution includes:
performing electrolytic treatment on the nanowire solution to generate gas; or
Performing photolysis treatment on the nanowire solution to generate gas;
preferably, a direct current is passed to the nanowire solution.
Preferably, the generating of the gas in the nanowire solution by a physical method includes:
generating gas in the nanowire solution by adopting a vacuum gas floating method; or
Performing ultrasonic treatment on the nanowire solution to generate gas; or
Heating the nanowire solution to generate gas; or
And oscillating or stirring the nanowire solution to generate gas.
Preferably, the nanowire includes at least one of a semiconductor nanowire, a metal nanowire, an alloy nanowire, a molecular-based nanowire, or an insulator nanowire.
Preferably, the nanowire includes at least one of a gold nanowire, a silver nanowire, a copper nanowire, an iron nanowire, a cobalt nanowire, a perovskite nanowire, a nickel nanowire, a carbon nanowire, an indium phosphide nanowire, a silicon nanowire, a gallium nitride nanowire, a cadmium selenide nanowire, a silicon dioxide nanowire, a titanium dioxide nanowire, or a DNA-based nanowire.
Preferably, the gas comprises at least one of carbon dioxide, nitrogen or an inert gas.
In another aspect, the present application provides a nanowire obtained by the method for processing a nanowire as described above.
Has the advantages that:
the gas can separate the nanowires from each other by generating the gas in the nanowire solution, and when the knotted and/or doubled nanowires exist in the nanowire solution, the gas can separate the doubled or knotted nanowires from each other. For example, carbonate and weak acid are added into the metal nanowires, the carbonate reacts with the weak acid to generate gas, such as carbon dioxide gas, and the generated gas repels the knotted or doubled metal nanowires, so that the problem that a large amount of knotting and doubling occur in the purification process of the metal nanowires due to operations such as shaking and stirring is solved.
And, further, since a large amount of gas is present in the nanowire solution, it is possible to prevent the nanowires from being doubled or knotted.
Drawings
Fig. 1 is a flow chart of a method for purifying metal nanowires according to an embodiment of the present disclosure;
FIG. 2 is a schematic diagram of a crude product 200 of metal nanowires in an embodiment of the present application;
fig. 3 is a schematic view of a crude product 200 of metal nanowires after adding acetone thereto according to an embodiment of the present disclosure;
FIG. 4 is a schematic diagram of a metal nanowire 201 re-dispersed in a solution according to an embodiment of the present application;
fig. 5 is a schematic diagram of a metal nanowire 201 after a weak acid is added thereto according to an embodiment of the present disclosure;
FIGS. 6 and 7 are schematic views of a metal nanowire with a bubble 203 expanded to release a knot 204 and a doubling 205, respectively, according to an embodiment of the present application;
FIG. 8 is a flow chart of a method for purifying metal nanowires according to another embodiment of the present application;
FIG. 9 is a microscope photograph of the doubling of ultrafine silver nanowires in comparative example 1 of the present application;
fig. 10 is a microscope image of knotting of the ultra fine silver nanowires in comparative example 1 of the present application;
fig. 11 is a microscopic view of the ultra fine silver nanowires after purification in example 1 of the present application;
FIG. 12 is a TEM image of the ultra-fine silver nanowires after purification in example 1 of the present application;
FIG. 13 is a flow chart of a method for processing nanowires in an embodiment of the present application;
FIG. 14 shows CsPbBr treated in example 2 of the present application3Microscopic images of perovskite nanowires;
FIG. 15 shows the CsPbBr untreated in comparative example 2 of the present application3Microscopic images of perovskite nanowires.
Detailed Description
The technical solutions in the examples of the present application will be described in detail below with reference to the embodiments of the present application. It should be noted that the described embodiments are only some embodiments of the present application, and not all embodiments.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting. Unless otherwise defined, all terms (including technical and scientific terms) in the specification may be defined as commonly understood by one of ordinary skill in the art. Terms defined in commonly used dictionaries should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and the present disclosure, and may not be interpreted in an idealized or overly formal sense unless expressly so defined.
Furthermore, unless expressly stated to the contrary, the terms "comprises" and "comprising," when used in this specification, specify the presence of stated features, regions, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, regions, integers, steps, operations, elements, components, and/or groups thereof. Thus, the above wording will be understood to mean that the stated elements are included, but not to exclude any other elements.
It will be understood that, although the terms first, second, third, etc. may be used herein to describe various elements, components, regions, layers and/or sections, these elements, components, regions, layers and/or sections should not be limited by these terms. These terms are only used to distinguish one element, component, region, layer or section from another element, component, region, layer or section. Thus, a first element, component, region, layer or section discussed below could be termed a second element, component, region, layer or section without departing from the teachings of the present embodiments.
Definition of
The following definitions apply to aspects described in relation to some embodiments of the invention, and these definitions may be extended herein as well.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting. As used herein, the singular forms "a," "an," and "the" include plural referents unless the context clearly dictates otherwise. Unless the context clearly dictates otherwise, reference to an object may include multiple objects.
As used herein, "combination" includes all types of combinations, including blends, alloys, solutions, and the like.
As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items. The term "or" means "and/or". The expression "at least one of" when preceding or following a list of elements modifies the entire list of elements without modifying individual elements of the list.
As used herein, "about" or "approximately" includes the stated value and is meant to be within an acceptable range of deviation for the particular value as determined by one of ordinary skill in the art in view of the measurement in question and the error associated with measurement of the particular quantity (i.e., limitations of the measurement system). For example, "about" may mean a deviation from the stated value within one or more standard deviation ranges, or within ± 10%, 5%.
As used herein, the term "nano-range" or "nm range" refers to a size range of about 1nm to about 1 μm.
As used herein, the term "aspect ratio" refers to the ratio of the largest dimension or range of an object to the average of the remaining dimensions or ranges of the object, wherein the remaining dimensions are orthogonal relative to each other and relative to the largest dimension. In some cases, the remaining dimensions of the object may be substantially the same, and an average of the remaining dimensions may substantially correspond to any of the remaining dimensions. For example, the aspect ratio of a cylinder refers to the ratio of the length of the cylinder to the diameter of the cross-section of the cylinder.
As used herein, the term "nanoscale" object refers to an object having at least one dimension in the nanometer range. The nanoscale objects can have any of a wide variety of shapes, and can be formed from a wide variety of materials. Examples of nanoscale objects include nanowires, nanotubes, nanoplatelets, nanoparticles, and other nanostructures.
As used herein, the term "quantum dot" is a nanoparticle having a three-dimensional size of less than 100 nanometers.
As used herein, the term "nanowire" refers to an elongated nanoscale object that is substantially solid. Typically, nanowires have lateral dimensions in the nanometer range (e.g., cross-sectional dimensions in terms of diameter, width, or width or diameter representing an average across orthogonal directions).
As used herein, the term "weak acid" is used in relation to a strong acid, which is fully ionized and the weak acid is partially ionized. The pH of the weak acid is generally 4 to 6.
In one embodiment of the present application, a method for processing a nanowire includes the steps of:
providing a nanowire solution;
a gas is generated in the nanowire solution, which separates the nanowires from each other, or which prevents the nanowires from being doubled or knotted.
This embodiment is through producing gas in the nanowire solution, and gas can make the nanowire alternate segregation, when having the nanowire of knoing and/or doubling in the nanowire solution, gas can make the nanowire alternate segregation of doubling or knoing to the problem of a large amount of knots and doubling appears in the operation such as vibration and stirring in the purification process of nanowire has been solved. And, since a large amount of gas is present in the nanowire solution, it is possible to prevent the nanowires from being doubled or knotted.
In another embodiment of the present application, knotted and/or merged nanowires are present in the nanowire solution, and the gas is capable of separating the merged or knotted nanowires from each other.
The gas generated in the nanowire solution can be generated by a physical method, a chemical method or a combination of physical and chemical methods.
In one embodiment of the present application, a chemical method for generating a gas in a nanowire solution includes:
and adding a first reactant and a second reactant into the nanowire solution, wherein the first reactant and the second reactant react to generate gas.
In another embodiment herein, the first reactant is a carbonate and the second reactant is a weak acid.
Preferably, the carbonate salt comprises at least one of a normal carbonate salt, a basic carbonate salt or a bicarbonate salt.
Preferably, the carbonate salt includes at least one of sodium carbonate, sodium bicarbonate, lithium carbonate, lithium bicarbonate, magnesium carbonate, calcium carbonate, potassium carbonate, or potassium bicarbonate.
Preferably, the weak acid comprises a carboxylic acid, preferably, the carboxylic acid further comprises acetic acid.
In another embodiment of the present application, a chemical method of generating a gas in a nanowire solution includes:
the nanowire solution is subjected to electrolytic treatment to generate gas.
Preferably, a direct current is applied to the nanowire solution to generate a gas in the nanowire solution.
In another embodiment of the present application, a chemical method of generating a gas in a nanowire solution includes:
the nanowire solution is photolyzed to generate a gas.
In another embodiment of the present application, the physical method of generating gas in the nanowire solution includes, but is not limited to:
generating gas in the nanowire solution by adopting a vacuum gas floating method; or, carrying out ultrasonic treatment on the nanowire solution to generate gas; or heating the nanowire solution to generate gas; or shaking or stirring the nanowire solution to generate gas.
In an embodiment of the present application, the nanowire includes, but is not limited to, at least one of a semiconductor nanowire, a metal nanowire, an alloy nanowire, a molecular-based nanowire, or an insulator nanowire. For example, the nanowire includes, but is not limited to, at least one of a gold nanowire, a silver nanowire, a copper nanowire, an iron nanowire, a cobalt nanowire, a perovskite nanowire, a nickel nanowire, a carbon nanowire, an indium phosphide nanowire, a silicon nanowire, a gallium nitride nanowire, a cadmium selenide nanowire, a silicon dioxide nanowire, a titanium dioxide nanowire, or a DNA-based nanowire.
In an embodiment of the present application, the gas generated in the nanowire solution includes, but is not limited to, at least one of carbon dioxide, nitrogen, or an inert gas.
In another embodiment of the present application, a nanowire is obtained by a method for processing a nanowire, the method for processing a nanowire comprising the steps of: providing a nanowire solution; a gas is generated in the nanowire solution, and the gas separates the nanowires from each other, or the gas prevents the nanowires from being merged or knotted. After the nanowire solution is treated by adding gas, nanowires are mutually separated by the gas, and when knotted and/or doubled nanowires exist in the nanowire solution, the doubled or knotted nanowires can be repelled by the gas to be mutually separated, so that the problem of massive knotting and doubling of the nanowires in the purification process due to operations such as vibration and stirring is solved. And, since a large amount of gas is present in the nanowire solution, it is also possible to prevent the nanowires from being re-combined or knotted. In one embodiment of the present application, a method for purifying metal nanowires includes:
step one, preparing unpurified metal nanowires;
secondly, adding carbonate into the metal nanowires;
step three, separating and purifying the metal nanowires;
adding a weak acid into the metal nanowires, wherein the weak acid reacts with the carbonate to generate gas;
and step five, obtaining the purified metal nanowire.
In the embodiment, in the purification process of the metal nanowires, for example, the metal nanowires are silver nanowires, carbonate and weak acid are added into the metal nanowires, the carbonate reacts with the weak acid to generate gas, for example, carbon dioxide gas, and the generated gas repels the knotted or doubled metal nanowires, so that the problem that a large number of knotted and doubled metal nanowires are generated due to operations such as vibration and stirring in the purification process of the metal nanowires is solved.
At present, after a crude product of the metal nanowire is prepared, the crude product needs to be repeatedly washed to separate and purify the metal nanowire. The common washing solvent is acetone, and the acetone is added into the crude product of the metal nanowires, so that the acetone can dissolve metal nanoparticles, polymers, unreacted ions and the like in the crude product, and after the metal nanowires are precipitated, turbid liquid on the upper part is removed. Then, the metal nanowire precipitate is redispersed in water through operations such as oscillation, stirring and the like, and acetone is added again for separation and purification.
And finally obtaining the purified metal nanowire after acetone is separated and purified for multiple times. However, the metal nanowires are largely knotted and doubled by the operation such as agitation.
Therefore, in this embodiment, before the acetone is added to the crude metal nanowire product for separation and purification, carbonate is added to the crude metal nanowire product in advance. In a preferred embodiment of the present application, the carbonate is a carbonate aqueous solution previously dissolved in water.
And adding acetone to precipitate the metal nanowires, and removing upper turbid liquid to obtain the metal nanowire precipitate containing carbonate aqueous solution. After the weak acid is added into the aqueous solution of the metal nanowire precipitate, the weak acid reacts with carbonate in the metal nanowire precipitate to generate carbon dioxide gas, so that bubbles are generated in the metal nanowire precipitate, the bubbles are increased along with the reaction, the metal nanowires are repelled and separated by the bubbles, and the knotted or doubled metal nanowires are separated and untied.
Meanwhile, as the metal nanowires are cleaned by acetone for multiple times, the carbonate and the weak acid can be synchronously added for multiple times, so that the problems of knotting and doubling of the metal nanowires can be solved when the metal nanowires are vibrated, stirred and redispersed in water each time.
Fig. 1 is a flow chart of a method for purifying metal nanowires according to an embodiment of the present disclosure. The purification method comprises the following steps:
step S101, preparing unpurified metal nanowires;
in step S101, the unpurified metal nanowires are crude metal nanowires, and as shown in fig. 2, the crude metal nanowires 200 in this embodiment are schematic diagrams, and the crude metal nanowires 200 may include impurities such as a polymer (not shown), various unreacted ions (not shown), and metal nanoparticles 202, in addition to the metal nanowires 201. These impurities seriously affect the quality of the metal nanowire, especially the metal nanoparticle 202, and when the metal nanowire is applied as a transparent conductive material, the metal nanoparticle 202 scatters light, which seriously affects the photoelectric performance of the metal nanowire. Therefore, it is necessary to separate and purify the metal nanowire 201 to remove the metal nanoparticle 202 and impurities such as unreacted ions and polymers.
Step S102, adding carbonate into the metal nanowire;
before the metal nanowire 201 is separated and purified, carbonate is added to the dispersion system of the metal nanowire 201, and the metal nanowire 201 is generally dispersed in an aqueous solution, and preferably, when the carbonate is added to the dispersion system of the metal nanowire 201, the carbonate is dissolved in water and then added to the dispersion system of the metal nanowire 201.
In one embodiment of the present application, the carbonate salt comprises a normal carbonate salt or a bicarbonate salt. For example, the positive carbonate includes at least one of sodium carbonate, lithium carbonate, and potassium carbonate; the bicarbonate comprises at least one of sodium bicarbonate, lithium bicarbonate and potassium bicarbonate. However, the present application is not limited thereto, as long as the carbonate does not damage or corrode the metal nanowire and reacts with the subsequently added weak acid to generate gas.
Step S103, separating and purifying the metal nanowires;
separating and purifying the metal nanowire 201, generally adding acetone into a crude product of the metal nanowire 201 to precipitate the metal nanowire 201; in addition, the metal nanowires 201 may also be separated from the solution by centrifugation, the metal nanowires 201 tend to agglomerate and precipitate out of the solution, and the metal nanoparticles 202 tend to be suspended in the solution. Thereby removing the upper solution, i.e., removing the polymer, unreacted ions, and metal nanoparticles 202 together.
As shown in fig. 3, which is a schematic diagram of the crude product 200 of the metal nanowire 201 after acetone is added in the present embodiment, since the metal nanowire 201 is coated with a polymer, for example, polyvinylpyrrolidone (PVP), and the polymer makes the metal nanowire 201 insoluble in acetone, the metal nanowire 201 is collected and precipitated, and the metal nanoparticle 202 and impurities such as ions not participating in the reaction are dissolved in the solution. By removing the upper layer solution, the metal nanoparticles 202 and impurities such as unreacted ions in the upper layer solution are removed. The separation and purification of the metal nanowire 201 are realized. Next, the precipitate of the metal nanowires 201 is redispersed in a solution, such as an aqueous solution, by shaking and stirring. So as to facilitate the separation and purification of the metal nanowire 201 again.
However, as shown in fig. 4, the metal nanowires 201 may have a problem of knotting 204 and doubling 205 in a schematic view in which the metal nanowires 201 are re-dispersed in a solution in this embodiment.
Step S104, adding a weak acid into the metal nanowires, wherein the weak acid reacts with the carbonate to generate gas;
after the metal nanowires 201 are separated and purified, the metal nanowires 201 are re-dispersed in the solution, for example, the precipitate of the metal nanowires 201 is re-dispersed in water by shaking and stirring, at this time, the solution of the metal nanowires 201 contains carbonate, in this step, a weak acid is added to the solution re-dispersed by the metal nanowires 201, the weak acid reacts with the carbonate to generate gas, a large amount of bubbles exist in the solution of the metal nanowires 201 along with the reaction, the bubbles repel and separate the metal nanowires 201 knotted 204 or doubled 205, and the metal nanowires 201 knotted 204 or doubled 205 are untied.
As shown in fig. 5, which is a schematic diagram of the metal nanowires 201 after a weak acid is added thereto in this embodiment, since a carbonate reacts with the weak acid to generate a gas, a large number of bubbles 203 may exist around the metal nanowires 201, and the bubbles 203 may repel and separate the metal nanowires 201 from each other, thereby avoiding a problem that the metal nanowires 201 are knotted 204 or doubled 205.
More specifically, as shown in fig. 6 and 7, there is shown a schematic view of the expansion of the bubble 203 to release the knot 204 and the doubling 205 in the embodiment of the present application. As the reaction proceeds, bubbles 203 grow larger and larger, thereby repelling and separating the metal nanowires 201 of the knot 204 or the parallel 205.
In the embodiment, the weak acid includes a carboxylic acid, and further, preferably, the carboxylic acid is acetic acid, which does not corrode or damage the metal nanowire 201 and can react with the carbonate to generate gas.
And step S105, obtaining the purified metal nanowire.
In the embodiment, in the purification process of the metal nanowire 201, the carbonate and the weak acid are added into the metal nanowire 201, the carbonate reacts with the weak acid to generate gas, the gas is gathered into the bubble 203, and the metal nanowire 201 knotted 204 or doubled 205 is repelled by the bubble 203, so that the problem that a large number of knots 204 and doubled 205 are formed in the purification process of the metal nanowire 201 due to operations such as vibration and stirring is solved.
Fig. 8 is a flow chart of a method for purifying metal nanowires according to another embodiment of the present application. The difference from the previous embodiment is that a weak acid is added to the metal nanowires, and then the metal nanowires are separated and purified, and then carbonate is added to the metal nanowires.
The purification method comprises the following steps:
step S201, preparing unpurified metal nanowires;
in step S201, the unpurified metal nanowires are a crude product of the metal nanowires, and the crude product may contain impurities such as a polymer, various ions that do not participate in the reaction, and metal nanoparticles, in addition to the metal nanowires.
Step S202, adding weak acid into the metal nanowire;
in the present embodiment, the weak acid includes a carboxylic acid, and preferably, the carboxylic acid is acetic acid, which does not corrode or damage the metal nanowire 201 and can react with a carbonate added later to generate a gas.
Step S203, separating and purifying the metal nanowires;
separating and purifying the metal nanowires, generally adding acetone into a crude product of the metal nanowires to precipitate the metal nanowires; in addition, the nanowires may also be separated from the solution by centrifugation, with the metal nanowires tending to agglomerate and precipitate out of solution, while the metal nanoparticles tend to be suspended in solution. Thereby removing the upper solution, namely removing the polymer, the unreacted ions and the nano particles in the solution together.
Step S204, adding carbonate into the metal nanowires, wherein the carbonate reacts with the weak acid to generate gas;
after the metal nanowires are separated and purified, carbonate is added to the dispersion solution of the metal nanowires, and the metal nanowires are generally dispersed in an aqueous solution.
In this embodiment, the carbonate salt includes a normal carbonate salt or a bicarbonate salt. For example, the positive carbonate includes at least one of sodium carbonate, lithium carbonate, and potassium carbonate; the bicarbonate comprises at least one of sodium bicarbonate, lithium bicarbonate and potassium bicarbonate. However, the present application is not limited thereto, as long as the carbonate does not damage or corrode the metal nanowire and reacts with the weak acid to generate gas.
After the metal nanowires are separated and purified, the metal nanowires are re-dispersed in the solution, for example, the metal nanowire precipitate is re-dispersed in water through operations such as shaking and stirring, at this time, the metal nanowire solution contains a weak acid, in this step, carbonate is added to the solution in which the metal nanowires are re-dispersed, the carbonate reacts with the weak acid to generate gas, and as the reaction proceeds, a large amount of bubbles exist in the metal nanowire solution, and the bubbles repel and separate the metal nanowires which are knotted or doubled, so that the knotted or doubled metal nanowires are untied.
And step S205, obtaining the purified metal nanowire.
According to the method, the carbonate and the weak acid are added into the metal nanowires in the purification process of the metal nanowires, the carbonate reacts with the weak acid to generate gas, for example, carbon dioxide gas, and the generated gas can repel the knotted or doubled metal nanowires, so that the problems of massive knotting and doubling of the metal nanowires due to operations such as vibration and stirring in the purification process are solved.
In addition, in another embodiment of the present application, the preparing of unpurified metal nanowires step comprises:
heating a mixture of a polyol, a metal compound, a polymer and a halide.
Wherein the polyol serves as a liquid medium for the reaction and as a reducing agent for reducing the metal compound to the metal. Suitable polyols are organic compounds having a core moiety comprising at least 2 carbon atoms, wherein the core moiety is substituted with at least 2 hydroxyl groups per molecule, and each hydroxyl group is attached to a different carbon atom of the core moiety. Suitable polyols are known and include, but are not limited to, at least one of ethylene glycol, propylene glycol, glycerol, butylene glycol, pentylene glycol, hexylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, dipropylene glycol, or glycerol. In one embodiment herein, the polyol is ethylene glycol.
Among them, suitable metal compounds capable of producing a metal upon reduction are known, including but not limited to metal oxides, metal inorganic salts or metal organic salts, for example, metal inorganic salts including at least one of nitrate, nitrite, sulfate, halide, carbonate, phosphate, fluoroborate or sulfonate; the metal organic salt comprises at least one of formate, acetate, propionate, butyrate, trifluoroacetate, acetoacetate, lactate, citrate, glycolate, tosylate, or tris (dimethylpyrazole) borate. In a specific embodiment of the present application, the metal compound is nitrate, the metal nanowire is silver nanowire, and the metal compound is silver nitrate.
Wherein the polymer comprises at least one of poly (N-vinylformamide), poly (N-vinylacetamide), poly (N-vinylpropionamide), or polyvinylpyrrolidone (PVP); the polymer is preferably polyvinylpyrrolidone having a molecular weight of between 5 and 130 million. The polymer functions as a capping agent in the synthesis stage of the metal nanowire, the capping agent is a substance that adsorbs to a specific surface of the generated core, and the capping agent suppresses the growth rate of the surface to control the shape of the generated particle. In the synthesis of the metal nanowire, a substance to be adsorbed to a side surface of the metal nanowire is selected, whereby a thin and long metal nanowire can be obtained. In a specific embodiment of the present application, the polymer is polyvinylpyrrolidone (PVP).
Wherein the halide comprises at least one of sodium chloride, potassium chloride, sodium bromide, potassium bromide, sodium iodide, potassium iodide, cetyltrimethylammonium bromide or cetyltrimethylammonium chloride. The copolymer contains halide which is used as counter ion and mainly plays a role in balancing polymer charges on the surface of the metal nanowire. In one embodiment of the present application, the halide is sodium bromide.
In the purified metal nanowire according to one embodiment of the present application, the purified metal nanowire is obtained by the following purification method. The purification method comprises the following steps:
step one, preparing unpurified metal nanowires;
secondly, adding carbonate into the metal nanowires;
step three, separating and purifying the metal nanowires;
adding a weak acid into the metal nanowires, wherein the weak acid reacts with the carbonate to generate gas;
and step five, obtaining the purified metal nanowire.
In the embodiment, in the purification process of the metal nanowires, for example, the metal nanowires are silver nanowires, carbonate and weak acid are added into the metal nanowires, the carbonate reacts with the weak acid to generate gas, for example, carbon dioxide gas, and the generated gas repels the knotted or doubled metal nanowires, so that the problem that a large number of knotted and doubled metal nanowires are generated due to operations such as vibration and stirring in the purification process of the metal nanowires is solved.
In this embodiment, before the acetone is added to the crude metal nanowire product for separation and purification, carbonate is added to the crude metal nanowire product in advance. In a preferred embodiment of the present application, the carbonate is a carbonate aqueous solution previously dissolved in water.
And adding acetone to precipitate the metal nanowires, and removing upper turbid liquid to obtain the metal nanowire precipitate containing carbonate aqueous solution. After the weak acid is added into the aqueous solution of the metal nanowire precipitate, the weak acid reacts with carbonate in the metal nanowire precipitate to generate carbon dioxide gas, so that bubbles are generated in the metal nanowire precipitate, the bubbles are increased along with the reaction, the metal nanowires are repelled and separated by the bubbles, and the knotted or doubled metal nanowires are separated and untied.
Meanwhile, as the metal nanowires are cleaned by acetone for multiple times, the carbonate and the weak acid can be synchronously added for multiple times, so that the problems of knotting and doubling of the metal nanowires can be solved when the metal nanowires are vibrated, stirred and redispersed in water each time.
In a specific embodiment of the present application, the metal nanowire is preferably a silver nanowire, but the present application is not limited thereto, and the metal nanowire may also be a copper nanowire (Cu), a gold nanowire (Au), a nickel nanowire (Ni) platinum nanowire (Pt), or the like. The present application is not limited to the kind of metal.
In another embodiment of the present disclosure, during the purification process of the metal nanowire, the weak acid may be added to the metal nanowire, and then the carbonate may be added to the metal nanowire after the metal nanowire is separated and purified. The purification method of the metal nanowires has been explained in the above embodiments, and is not repeated herein.
A method of purifying silver nanowires according to some exemplary embodiments of the present application will be described in more detail below with reference to various examples; however, the exemplary embodiments of the present application are not limited thereto.
Preparation example
Preparing a coarse product of the superfine silver nanowires:
a three-necked flask of 1000ml Ethylene Glycol (EG), 8ml potassium bromide (KBr:200mM), 3g silver nitrate (AgNO3), and 5g PVP (K85) was heated to 180 ℃ under nitrogen with moderate stirring (100 to 200 rpm). The reaction was stopped 10 minutes after the temperature of 180 ℃ was reached, and a crude product of ultra-fine silver nanowires was obtained.
Example 1
Purifying the superfine silver nanowires:
1. adding sodium bicarbonate water (NaHCO)3) Diluting with water (1g/100ml), pouring into 500ml of the coarse product of the superfine silver nanowires in the preparation example, and uniformly stirring;
2. adding 2L of acetone into the uniformly mixed product, standing for 1h, and finding layering, pouring out turbid liquid at the upper part of the layering at the moment, and leaving a dough-like dark gray precipitate;
3. adding 10% glacial acetic acid 1L into the beaker in step 2, covering the precipitate, dispersing by shaking table, wherein a large amount of bubbles gush out,
chemical reaction:
NaHCO3+CH3COOH＝CH3COONa+H2O+CO2↑
the bubbles repel the densely arranged silver nanowires, thereby achieving the purpose of dispersing, knotting and doubling the silver nanowires. And can prevent the silver nanowires from being further knotted and doubled.
As shown in fig. 11, is a microscope image of the ultra-fine silver nanowires in this example;
as shown in fig. 12, which is a TEM image of a transmission electron microscope of the ultrafine silver nanowires in this embodiment, it is obvious that the knotted and doubled silver nanowires are greatly reduced, and the whole silver nanowires are uniformly dispersed.
Comparative example 1:
purifying the superfine silver nanowires:
unlike example 1, sodium bicarbonate and glacial acetic acid were not added during the purification of the silver nanowires.
1. Adding 2L of acetone into 500ml of the coarse product of the superfine silver nanowires in the preparation example, standing for 1h to find layering, and pouring out turbid liquid at the upper part of the layering at the moment to leave a dough-like dark gray precipitate;
2. the doughy dark grey precipitate was redispersed in water by shaking and stirring.
As shown in fig. 9, which is a microscope image of the doubling of the ultra-fine silver nanowires in comparative example 1;
as shown in fig. 10, which is a microscope image of the knotted ultrafine silver nanowires of comparative example 1, it is apparent that the knotting and doubling of the silver nanowires are very severe.
As can be seen from comparison between fig. 11 and 12 of example 1 and fig. 9 and 10 of comparative example 1, the knotting and doubling of the ultra-fine silver nanowires in example 1 is greatly reduced, and it can be seen that the knotting and doubling of the ultra-fine silver nanowires can be well solved after carbonate and weak acid are added in the purification process of the ultra-fine silver nanowires.
Example 2
CsPbBr3The perovskite nanowire treatment steps are as follows:
1. for CsPbBr filled therein3The gas tank of the perovskite nanowire crude product solution is cooled, so that CsPbBr is obtained3Reducing the temperature of the perovskite nanowire crude product solution to 5 ℃ and adding CsPbBr3Argon gas is blown into the perovskite nanowire crude product solution, so that CsPbBr is generated3Excessive argon is dissolved in the perovskite nanowire crude product solution, and the argon is in a supersaturated state;
2. for CsPbBr filled therein3Vacuumizing the gas tank of the perovskite nanowire crude product solution, and CsPbBr3Argon dissolved in the perovskite nanowire crude product solution is separated out to generate a large amount of micro bubbles, and the bubbles repel the CsPbBr which is tightly arranged3Perovskite nanowires, CsPbBr for dispersed knotting and doubling3Perovskite nano-wire.
Comparative example 2:
untreated CsPbBr3Perovskite nanowire:
unlike example 2, CsPbBr was not treated3And carrying out cooling and air dissolving and vacuum air floating treatment on the perovskite nanowire.
FIG. 14 shows CsPbBr treated in example 23The microscopic picture of the perovskite nanowire shows that the perovskite nanowire has good dispersibility after spin coating and film forming.
As shown in FIG. 15, CsPbBr was untreated in comparative example 23The perovskite nanowire is shown in a microscopic picture, and the perovskite nanowire is agglomerated and knotted, and the perovskite nanowire is poor in dispersibility after being subjected to spin coating film forming.
As can be seen from comparison between fig. 14 of example 2 and fig. 15 of comparative example 2, the perovskite nanowires in example 2 are greatly reduced in agglomeration and knotting, and thus, the dispersibility of the perovskite nanowires can be improved after the perovskite nanowires are treated.
Although the present disclosure has been described and illustrated in greater detail by the inventors, it should be understood that modifications and/or alterations to the above-described embodiments, or equivalent substitutions, will be apparent to those skilled in the art without departing from the spirit of the disclosure, and that no limitations to the present disclosure are intended or should be inferred therefrom.

Claims (10)

1. A method of processing nanowires, comprising the steps of:
providing a nanowire solution;
a gas is generated in the nanowire solution, which separates the nanowires from each other, or which prevents the nanowires from being doubled or knotted.
2. The processing method according to claim 1, characterized in that it further comprises the steps of:
knotted and/or doubled nanowires exist in the nanowire solution;
the gas separates the doubled or knotted nanowires from each other.
3. The processing method of claim 1, wherein the step of generating a gas in the nanowire solution comprises:
physical and/or chemical methods generate the gas.
4. The processing method of claim 3, wherein chemically generating a gas in the nanowire solution comprises:
and adding a first reactant and a second reactant into the nanowire solution, wherein the first reactant and the second reactant react to generate gas.
5. The processing method according to claim 4,
the first reactant is a carbonate and the second reactant is a weak acid;
preferably, the carbonate comprises at least one of a normal carbonate, a basic carbonate or a bicarbonate;
preferably, the carbonate includes at least one of sodium carbonate, sodium bicarbonate, lithium carbonate, lithium bicarbonate, magnesium carbonate, calcium carbonate, potassium carbonate, or potassium bicarbonate;
preferably, the weak acid comprises a carboxylic acid;
preferably, the carboxylic acid comprises acetic acid.
6. The processing method of claim 1, wherein chemically generating a gas in the nanowire solution comprises:
performing electrolytic treatment on the nanowire solution to generate gas; or
Performing photolysis treatment on the nanowire solution to generate gas;
preferably, a direct current is passed to the nanowire solution.
7. The processing method of claim 1, wherein generating a gas in the nanowire solution by a physical method comprises:
generating gas in the nanowire solution by adopting a vacuum gas floating method; or
Performing ultrasonic treatment on the nanowire solution to generate gas; or
Heating the nanowire solution to generate gas; or
And oscillating or stirring the nanowire solution to generate gas.
8. The process of claim 1, wherein the nanowires comprise at least one of semiconductor nanowires, metal nanowires, alloy nanowires, molecular-based nanowires, or insulator nanowires;
preferably, the nanowire includes at least one of a gold nanowire, a silver nanowire, a copper nanowire, an iron nanowire, a cobalt nanowire, a perovskite nanowire, a nickel nanowire, a carbon nanowire, an indium phosphide nanowire, a silicon nanowire, a gallium nitride nanowire, a cadmium selenide nanowire, a silicon dioxide nanowire, a titanium dioxide nanowire, or a DNA-based nanowire.
9. The process of claim 1, wherein the gas comprises at least one of carbon dioxide, nitrogen, or an inert gas.
10. A nanowire obtained by the method for treating a nanowire according to any one of claims 1 to 9.
CN202010016795.0A 2020-01-08 2020-01-08 Nanowire processing method and nanowire Pending CN111217389A (en)

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