CN113263186A - Nano copper wire and preparation method thereof - Google Patents
Nano copper wire and preparation method thereof Download PDFInfo
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- CN113263186A CN113263186A CN202110565267.5A CN202110565267A CN113263186A CN 113263186 A CN113263186 A CN 113263186A CN 202110565267 A CN202110565267 A CN 202110565267A CN 113263186 A CN113263186 A CN 113263186A
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
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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
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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
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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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 invention relates to a nano copper wire and a preparation method thereof. During preparation, dropwise adding the alkali solution into the mixed solution of the copper salt added with the protective agent and the guiding agent and the reducing agent, and adjusting the pH value to 7-9, so that the diameter of the prepared nano copper wire completely meets the requirement of the nano level and the appearance is easy to control. The invention uses thiourea dioxide as a reducing agent, has the characteristics of strong reducibility, obvious effect, low cost, good thermal stability, convenient storage and transportation and the like, is environment-friendly and pollution-free in the using process, solves the problems of strict supervision or high toxicity and high cost of the common reducing agent, and realizes double guarantee of social benefit and economic benefit.
Description
Technical Field
The invention belongs to the technical field of nano material property, and particularly relates to a nano copper wire and a preparation method thereof.
Background
The nano copper wire has the properties of nano size effect, surface effect, good heat and electric conduction and the like, and is widely applied to the fields of catalysis, magnetofluid, lubrication, microelectronics, coating, medicine and the like. The nano copper wire has the advantages of small resistivity, low electromigration speed, low price and the like, and is gradually one of ideal substitutes for the conductive paste taking silver as the inner electrode in the multilayer ceramic capacitor. The nano copper wire is favored by the advantages of high conductivity, relatively low price, large reserve, easily available materials, no influence on coating performance caused by silver migration of silver powder in the coating, and the like, and can be widely applied in the technical field of nano and micro electronics in the future. The method has abundant copper resources in China, so that the resources are fully utilized, the economic benefit is improved, the progress of the research and development of the nano copper wire technology in China is promoted, and the method has very important significance in the research of the preparation of the nano copper wire with controllable appearance, size and structure.
At present, the method for preparing the nano copper wire is mostly a liquid phase reduction method, generally hydrazine hydrate, sodium borohydride and other explosive chemicals or formaldehyde and other highly toxic medicines are used, so that the supervision is strict, the cost is high, and pollution is easily caused in the using process; the liquid phase reduction of the nano copper wire by using the reducing agent has the defects of high cost, difficult raw material obtaining, complex experimental device, relatively long process flow, difficult realization of industrial production and the like.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a nano copper wire prepared by taking thiourea dioxide as a reducing agent and a preparation method thereof, which solve the problems of high toxicity, easy explosion, strict supervision, high cost and the like of the common reducing agent.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention relates to a nano copper wire which is prepared from copper salt, a protective agent, a dispersing agent, a guiding agent, a reducing agent, a solvent and alkali liquor; the copper salt is at least one of copper chloride, cuprous chloride, copper sulfate and copper nitrate, the protective agent and the dispersing agent are at least one of polyethylene glycol, polyvinyl alcohol, gelatin, sodium carboxymethylcellulose, hydroxyethyl cellulose and hydroxypropyl methyl cellulose, the guiding agent is 1, 2-propane diamine, the reducing agent is thiourea dioxide, the solvent is deionized water, and the alkali liquor is at least one of sodium hydroxide solution, potassium hydroxide solution and ethylenediamine.
Further, the mass ratio of the copper salt to the sum of the protective agent and the dispersing agent is 2-6: 1, the molar ratio of the copper salt to the 1, 2-propane diamine is 1-4: 1.
the invention also provides a preparation method of the nano copper wire, which comprises the following steps:
a1. dissolving a copper salt in a solvent to form a copper salt solution;
a2. adding a protective agent and a dispersing agent into a copper salt solution to obtain a mixed solution A;
a3. adding 1, 2-propane diamine into the mixed solution A to obtain a mixed solution B;
a4. dissolving thiourea dioxide in the mixed solution B, and stirring and mixing to obtain a mixed solution C;
a5. dropwise adding alkali liquor into the mixed solution C under the condition of magnetic stirring, and adjusting the pH value to obtain a mixed solution D;
a6. placing the mixed solution D in a constant-temperature water bath kettle, stirring and heating in a water bath;
a7. and cooling the heated mixed solution D to room temperature, and then sequentially carrying out centrifugal treatment, filtration, washing, filtration and drying to obtain the nano copper wire.
Further, the concentration of the copper salt solution in the step a1 is 0.02 mol/L-0.5 mol/L, and the concentration of the alkali liquor in the step a5 is 0.1 mol/L-5.0 mol/L.
Further, the molar ratio of the copper salt to the thiourea dioxide in the mixed solution C in the step a4 is 1: (0.5-2).
Further, in the step a5, the pH value is adjusted to be 7-9.
Further, the reaction temperature of the water bath stirring and heating in the step a6 is 60-75 ℃, and the stirring time is 30-40 min.
Further, the "centrifugal treatment" in the step a7 is specifically: and placing the mixture in a table type low-speed centrifuge for centrifugal treatment, wherein the rotating speed during the centrifugal treatment is 3000 rad/min-5000 rad/min, and the time for the centrifugal treatment is 10-30 min.
Further, the "washing" in the step a7 is specifically: and (3) putting the nano copper wire filtered from the mixed solution D after the centrifugal treatment into distilled water and absolute ethyl alcohol for washing.
By adopting the technical scheme, the invention mainly has the following beneficial effects:
(1) according to the invention, copper salt is used as a raw material, thiourea dioxide with extremely strong reducibility is used as a reducing agent, and alkali liquor is added dropwise, so that the diameter of the prepared nano copper wire is ensured to completely meet the requirement of nano level, the appearance is easy to control, and the used reducing agent thiourea dioxide has the advantages of good thermal stability, convenience in storage and transportation, low requirement on reaction conditions, no pollution, safety, environmental friendliness and no toxic or side effect in the use process, and the problems of severe toxicity, easiness in explosion, strict supervision, high cost and the like of common reducing agents such as hydrazine hydrate, sodium borohydride, formaldehyde and the like are effectively solved without supervision and restriction;
(2) the preparation method disclosed by the invention has the advantages of short reaction period, low cost, easiness in obtaining raw materials, high safety, high dispersity, good shape controllability, low heating temperature, low energy consumption, easiness in realizing industrial production and capability of realizing macro-preparation.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing a nano copper wire according to the present invention;
FIG. 2 is an XRD spectrum of a nano-copper wire prepared in example 1 of the present invention;
FIG. 3 is a scanning electron microscope photograph of a nano-copper wire obtained in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The nano copper wire is prepared from copper salt, a protective agent, a dispersing agent, a guiding agent, a reducing agent, a solvent and alkali liquor; wherein the copper salt is at least one of copper chloride, cuprous chloride, copper sulfate and copper nitrate, the protective agent and the dispersing agent are at least one of polyethylene glycol, polyvinyl alcohol, gelatin, sodium carboxymethylcellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose and the like, the guiding agent is 1, 2-propane diamine, the reducing agent is thiourea dioxide, the solvent is deionized water, and the alkali liquor is at least one of sodium hydroxide solution, potassium hydroxide solution and ethylenediamine; moreover, the preferable scheme is as follows: the mass ratio of the copper salt to the protective agent to the dispersant is 2-6: 1 (preferred mass ratio 2: 1, 3: 1, 4: 1), wherein the molar ratio of the copper salt to the 1, 2-propanediamine is 1-4: 1.
as shown in fig. 1, the method for preparing a nano copper wire according to the present invention comprises the following steps:
s100, dissolving copper salt in a solvent to form a copper salt solution; the concentration of the copper salt solution is preferably 0.02mol/L to 0.5 mol/L.
S200, adding a protective agent and a dispersing agent into a copper salt solution to obtain a mixed solution A;
s300, adding 1, 2-propane diamine into the mixed solution A to obtain a mixed solution B;
s400, dissolving thiourea dioxide in the mixed solution B, and stirring and mixing to obtain a mixed solution C; wherein the molar ratio of the copper salt to the thiourea dioxide in the mixed solution C is 1: (0.5-2) and stirring for 20 min.
S500, dropwise adding alkali liquor into the mixed solution C, and stirring and adjusting the pH value (the pH value is adjusted to 7-9) by using a magnetic stirrer to obtain a mixed solution D; wherein the concentration of the alkali liquor is 0.1-5.0 mol/L.
S600, placing the mixed solution D in a constant-temperature water bath kettle, stirring and heating in a water bath manner; wherein the reaction temperature of the water bath stirring and heating is 60-75 ℃, and the stirring time is 30-40 min.
S700, cooling the heated mixed solution D to room temperature, and then sequentially performing centrifugal treatment, filtration, washing, filtration and drying to obtain a nano copper wire; wherein the centrifugal treatment is specifically as follows: placing the mixture in a table type low-speed centrifuge for centrifugal treatment, wherein the rotating speed during the centrifugal treatment is 3000 rad/min-5000 rad/min, and the time for the centrifugal treatment is 10-30 min; the washing is specifically as follows: and (3) putting the nano copper wire filtered from the mixed solution D after the centrifugal treatment into distilled water and absolute ethyl alcohol for washing.
According to the nano copper wire, copper salt is used as a raw material, thiourea dioxide with strong reducibility is used as a reducing agent, alkali liquor is added dropwise (the alkali liquor is required to be added dropwise into a mixed solution of the copper salt and the thiourea dioxide added with a protective agent and a guiding agent, the pH value of the solution is adjusted to 7-9, otherwise, the nano copper wire cannot be obtained, the thiourea dioxide is easy to decompose under an alkaline condition to generate sulfinic acid with strong reducibility, so that the reduction effect can be controlled, if the alkali liquor is not added dropwise, the amount of the generated sulfinic acid is uncontrollable, so that the local reducibility is easily caused to be too strong, the nano copper wire cannot be prepared, and the prepared nano copper wire is ensured to completely meet the requirement of a nano level and the shape is controllable (see figure 3). The thiourea dioxide has good thermal stability, convenient storage and transportation, low requirement on reaction conditions, no pollution in the using process, safety and environmental protection, and effectively solves the problems of high toxicity, easy explosion, strict supervision, high cost and the like of common reducing agents such as hydrazine hydrate, sodium borohydride, formaldehyde and the like; the preparation method has the advantages of short reaction period (about 1-2 hours), low cost, easily available raw materials, high safety, good appearance controllability, low heating temperature, low energy consumption, easy realization of industrial production and capability of realizing macro-preparation.
The following examples further illustrate the copper nanowires and the preparation method of the present invention, but the following examples should not be construed as limiting the scope of the claims.
[ example 1 ]
The preparation steps of the nano copper wire of the embodiment 1 of the invention are as follows:
1) dissolving 0.6 g of copper nitrate trihydrate into 50 ml of deionized water, and stirring to form a copper nitrate aqueous solution with the solution concentration of 0.05 mol/L;
2) adding 0.2 g of polyethylene glycol into the copper nitrate aqueous solution obtained in the step 1) to obtain a mixed solution A;
3) adding 2.0ml of 1, 2-propane diamine into the mixed solution A obtained in the step 2) to obtain a mixed solution B;
4) dissolving 4.0 g of thiourea dioxide reducing agent in the mixed solution B obtained in the step 3), stirring for 20 minutes, and obtaining a mixed solution (mixed solution C) of copper nitrate and thiourea dioxide after the solution is dissolved;
5) dropwise adding an ethylenediamine solution with the solution concentration of 0.1mol/L into the mixed solution C prepared in the step 4), adjusting the pH to 8.0, and stirring the mixed solution by using a magnetic stirrer to obtain a mixed solution D;
6) placing the mixed solution D obtained in the step 5) in a constant-temperature water bath kettle at 70 ℃ for heating and stirring in a water bath for 30 min;
7) and (3) cooling the mixed solution D subjected to the water bath treatment in the step 6) to room temperature, placing the mixed solution D in a table type high-speed centrifuge, centrifuging for 20 minutes at the rotating speed of 3000rad/min, filtering, washing with distilled water and absolute ethyl alcohol respectively, filtering, and drying to obtain the nano copper wire.
Comparing the XRD spectrum (see fig. 2) of the nano-copper wire obtained in example 1 with the standard XRD spectrum of copper, it can be known that the nano-copper wire obtained in example 1 is elemental copper, and the diameter of the nano-copper wire obtained in example 1 completely meets the requirement of nano-scale and the morphology is controlled (see fig. 3).
[ example 2 ]
1) Dissolving 0.8 g of copper sulfate in 50 ml of deionized water, and stirring to form a copper sulfate aqueous solution with the solution concentration of 0.10 mol/L;
2) adding 0.2 g of polyvinyl alcohol into the copper sulfate aqueous solution obtained in the step 1) to obtain a mixed solution A;
3) adding 3.0ml of 1, 2-propane diamine into the mixed solution A obtained in the step 2) to obtain a mixed solution B;
4) dissolving 6.5 g of thiourea dioxide reducing agent in the mixed solution B obtained in the step 3), stirring for 20 minutes, and obtaining a mixed solution (mixed solution C) of copper sulfate and thiourea dioxide after dissolving;
5) dropwise adding a sodium hydroxide solution with the concentration of 0.2mol/L into the mixed solution C prepared in the step 4), adjusting the pH to 8.5, and stirring the mixed solution by using a magnetic stirrer to obtain a mixed solution D;
6) placing the mixed solution D obtained in the step 5) in a constant-temperature water bath kettle at 65 ℃ for water bath heating and stirring for 40 min;
7) and (3) cooling the mixed solution D subjected to the water bath treatment in the step 6) to room temperature, placing the mixed solution D in a table type high-speed centrifuge, centrifuging the mixed solution D for 20 minutes at the rotating speed of 4000rad/min, filtering the mixed solution D, washing the filtered mixed solution D with distilled water and absolute ethyl alcohol respectively, and filtering and drying the washed solution D to obtain the nano copper wire.
[ example 3 ]
1) Dissolving 1.0 g of copper chloride in 50 ml of deionized water, and stirring to form a copper chloride aqueous solution with the solution concentration of 0.15 mol/L;
2) adding 0.3 g of hydroxyethyl cellulose into the copper chloride aqueous solution obtained in the step 1) to obtain a mixed solution A;
3) adding 4.0ml of 1, 2-propane diamine into the mixed solution A obtained in the step 2) to obtain a mixed solution B;
4) dissolving 12.0 g of thiourea dioxide reducing agent in the mixed solution B obtained in the step 3), stirring for 20 minutes, and obtaining a mixed solution (mixed solution C) of copper chloride and thiourea dioxide after the solution is dissolved;
5) dropwise adding a potassium hydroxide solution with the solution concentration of 0.3mol/L into the mixed solution C prepared in the step 4), adjusting the pH to 9.0, and stirring the mixed solution by using a magnetic stirrer to obtain a mixed solution D;
6) placing the mixed solution D obtained in the step 5) in a constant-temperature water bath kettle at 70 ℃ for heating in a water bath for 30 min;
7) and (3) cooling the mixed solution D subjected to the water bath treatment in the step 6) to room temperature, placing the mixed solution D in a table-type high-speed centrifuge, centrifuging the mixed solution D for 20 minutes at the rotating speed of 5000rad/min, filtering the mixed solution D, washing the filtered mixed solution D with distilled water and absolute ethyl alcohol respectively, and filtering and drying the washed solution D to obtain the nano copper wire.
Similarly, comparing the XRD patterns of the nano-copper wires obtained in examples 2 and 3 with the standard XRD patterns of copper, it can be seen that the nano-copper wires obtained in examples 2 and 3 are elemental copper, and the nano-copper wires obtained in examples 2 and 3 are observed and imaged by using a scanning electron microscope, and the diameters of the nano-copper wires obtained in examples 2 and 3 completely meet the requirements of nano-scale and have controlled morphology.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (9)
1. The nano copper wire is characterized by being prepared from copper salt, a protective agent, a dispersing agent, a guiding agent, a reducing agent, a solvent and alkali liquor; the copper salt is at least one of copper chloride, cuprous chloride, copper sulfate and copper nitrate, the protective agent and the dispersing agent are at least one of polyethylene glycol, polyvinyl alcohol, gelatin, sodium carboxymethylcellulose, hydroxyethyl cellulose and hydroxypropyl methyl cellulose, the guiding agent is 1, 2-propane diamine, the reducing agent is thiourea dioxide, the solvent is deionized water, and the alkali liquor is at least one of sodium hydroxide solution, potassium hydroxide solution and ethylenediamine.
2. The copper nanophase wire according to claim 1, wherein the ratio of the copper salt to the sum of the mass of the protective agent and the mass of the dispersing agent is 2 to 6: 1, the molar ratio of the copper salt to the 1, 2-propane diamine is 1-4: 1.
3. a method for preparing a nano copper wire according to claim 1 or 2, comprising the steps of:
a1. dissolving a copper salt in a solvent to form a copper salt solution;
a2. adding a protective agent and a dispersing agent into a copper salt solution to obtain a mixed solution A;
a3. adding 1, 2-propane diamine into the mixed solution A to obtain a mixed solution B;
a4. dissolving thiourea dioxide in the mixed solution B, and stirring and mixing to obtain a mixed solution C;
a5. dropwise adding alkali liquor into the mixed solution C under the condition of magnetic stirring, and adjusting the pH value to obtain a mixed solution D;
a6. placing the mixed solution D in a constant-temperature water bath kettle, stirring and heating in a water bath;
a7. and cooling the heated mixed solution D to room temperature, and then sequentially carrying out centrifugal treatment, filtration, washing, filtration and drying to obtain the nano copper wire.
4. The method according to claim 3, wherein the concentration of the copper salt solution in step a1 is 0.02 mol/L-0.5 mol/L, and the concentration of the alkali solution in step a5 is 0.1 mol/L-5.0 mol/L.
5. The preparation method according to claim 3, wherein the molar ratio of the copper salt to thiourea dioxide in the mixed solution C in the step a4 is 1: (0.5-2).
6. The method as claimed in claim 3, wherein the pH value is adjusted to 7-9 in step a5.
7. The preparation method according to claim 3, wherein the reaction temperature of the water bath stirring and heating in the step a6 is 60-75 ℃, and the stirring time is 30-40 min.
8. The preparation method according to claim 3, wherein the "centrifugation treatment" in step a7 is specifically: and placing the mixture in a table type low-speed centrifuge for centrifugal treatment, wherein the rotating speed during the centrifugal treatment is 3000 rad/min-5000 rad/min, and the time for the centrifugal treatment is 10-30 min.
9. The preparation method according to claim 3, wherein the "washing" in the step a7 is specifically: and (3) putting the nano copper wire filtered from the mixed solution D after the centrifugal treatment into distilled water and absolute ethyl alcohol for washing.
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