CN111889692B - Monodisperse superfine copper powder and preparation method thereof - Google Patents
Monodisperse superfine copper powder and preparation method thereof Download PDFInfo
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- CN111889692B CN111889692B CN202010656647.5A CN202010656647A CN111889692B CN 111889692 B CN111889692 B CN 111889692B CN 202010656647 A CN202010656647 A CN 202010656647A CN 111889692 B CN111889692 B CN 111889692B
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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
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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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
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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
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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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 monodisperse superfine copper powder and a preparation method thereof. The superfine copper powder prepared by the preparation method provided by the invention has the purity of more than or equal to 99.8 percent, the hydrogen loss value of less than 0.15 percent and the apparent density of 0.7-1.2g/cm 3 D50 particle size is 4.8-5.5um, fsss particle size is 0.6-1.5um, fe is less than 0.001%, pb is less than 0.001%, as is less than 0.001%, cr is less than 0.001%, cd is less than 0.001%, S is less than 0.0015%, acid insoluble is less than 0.015%.
Description
Technical Field
The invention relates to the technical field of metal materials, in particular to monodisperse superfine copper powder and a preparation method thereof.
Background
The superfine copper powder is a nano copper material with good conductivity and high strength, is widely applied to conductive adhesive, conductive coating and electrode materials due to excellent electrical properties, and can be used for preparing catalysts and lubricating oil additives and even treating osteoporosis, fracture and the like in recent research.
At present, the preparation method of the superfine copper powder comprises an electrolytic method, an atomization method, a physical method (including a ball milling method, a gas-phase steam method, a plasma method, a y-ray irradiation-hydrothermal crystallization combination method and a freeze-drying method), a liquid-phase chemical reduction method and a chemical precipitation reduction method, wherein the electrolytic method, the atomization method and the physical method have the problems of high cost, expensive equipment and complex process, the industrial purity and the oxidation resistance of the liquid-phase chemical reduction method are difficult to control, and the conventional chemical precipitation reduction method has the problems of serious agglomeration and poor oxidation resistance of a finished product.
Disclosure of Invention
Aiming at the problems, the monodisperse ultrafine copper powder with good dispersibility, good oxidation resistance and sphere-like shape and the preparation method thereof are provided.
The specific technical scheme is as follows:
the first aspect of the invention provides a method for preparing monodisperse superfine copper powder, which is characterized by comprising the following steps:
1) Separately preparing Cu 2+ Soluble copper salt solution with concentration of 1-2.5mol/L, sodium carbonate solution with concentration of 150-260g/L and tannic acid solution with concentration of 1-10 wt%;
2) Adding the sodium carbonate solution prepared in the step 1) into a reaction kettle, starting stirring, adjusting the concentration of the sodium carbonate solution to 1-5g/L by using pure water, and then heating to 50-55 ℃;
3) Respectively adding the copper salt solution and the sodium carbonate solution prepared in the step 1) into a reaction kettle through a metering pump, controlling the temperature to be 50-55 ℃, the pH to be 7.5-8.5 and the stirring speed to be 200-350r/min, and reacting for 10-60min to nucleate basic copper carbonate precipitate;
4) Adding the tannic acid solution prepared in the step 1) into a reaction kettle by a metering pump according to 0.5-1wt% of the addition of copper ions, controlling the temperature to be 50-55 ℃, and continuously reacting for 10-30min at the stirring speed of 200-250 r/min;
5) Stopping adding the copper salt solution, continuously adding the sodium carbonate solution, controlling the pH value to be 8.5-9.0, then heating the temperature to 80-90 ℃, and continuously reacting for 1-10min by controlling the stirring speed to be 100-200 r/min;
6) Filtering, washing the filtered basic copper carbonate by pure water until the conductivity of the basic copper carbonate in washing water is less than 100, and then drying the washed basic copper carbonate to obtain basic copper carbonate powder;
7) Reducing the basic copper carbonate powder with hydrogen at 350-600 ℃ to obtain copper powder, and cooling and passivating the copper powder in an inert atmosphere to obtain superfine copper powder.
The preparation method also has the characteristic that the soluble copper salt in the copper salt solution in the step 1) is selected from one or more of copper sulfate, copper nitrate or copper chloride.
According to the method, in the step 3), a copper salt and sodium carbonate react to generate basic copper carbonate (at the moment, the basic copper carbonate is mainly nucleated), tannin is added in the subsequent step 4) and then complexed with copper ions, so that the copper ions in the copper salt are gradually released, basic copper carbonate particles grow, after the basic copper carbonate particles grow to a certain degree, the temperature is increased in the step 5) to accelerate tannin self-condensation reaction, so that the basic copper carbonate particles are promoted to agglomerate into quasi-spherical agglomerated particles by increasing the viscosity of a reaction system, and the basic copper carbonate in the agglomerated particles is reduced to form metal copper powder by a reduction system in the step 7), and meanwhile, the tannin can be decomposed by virtue of a high-temperature environment, so that the sintering and hard agglomeration of the basic copper carbonate in the agglomerated particles are avoided, and the dispersibility of the finally cooled and passivated superfine copper powder is ensured.
The complexation of tannin can be divided into two steps of reaction, specifically, the first step is the dissociation of phenolic hydroxyl in tannin: R-OH → R-O - +H + (ii) a The second step is that oxygen anions generated by dissociation are in coordination complexing with copper ions: R-O- + nCu 2+ →[R-O-Cu] n-1 Grown [ R-O-Cu ]] n-1 Attached to the basic copper carbonate to grow basic copper carbonate grains.
The second aspect of the present invention is to provide an ultrafine copper powder prepared according to the above-described preparation method.
The superfine copper powder prepared by the preparation method provided by the invention has the purity of more than or equal to 99.8 percent, the hydrogen loss value of less than 0.15 percent and the apparent density of 0.7-1.2g/cm 3 D50 particle size is 4.8-5.5um, fsss particle size is 0.7-1.5um, fe is less than 0.001%, pb is less than 0.001%, as is less than 0.001%, cr is less than 0.001%, cd is less than 0.001%, S is less than 0.0015%, acid insoluble is less than 0.015%.
Drawings
FIG. 1 is a scanning electron microscope image of agglomerates of basic copper carbonate particles in step 5) of example 1 of the present invention;
FIG. 2 is a scanning electron micrograph of the ultrafine copper powder prepared in example 1 of the present invention;
FIG. 3 is a graph showing the distribution of the particle size of the ultrafine copper powder prepared in example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The invention is further described with reference to the following drawings and specific examples, which are not intended to be limiting.
Example 1
The preparation process of monodisperse superfine copper powder includes the following steps:
1) Separately preparing Cu 2+ A copper sulfate solution with the concentration of 1mol/L, a sodium carbonate solution with the concentration of 150g/L and a tannic acid solution with the concentration of 1 wt%;
2) Adding the sodium carbonate solution prepared in the step 1) into a reaction kettle, starting stirring, adjusting the concentration of the sodium carbonate solution to 1g/L by using pure water, and then heating to 50 ℃;
3) Respectively adding the copper salt solution and the sodium carbonate solution prepared in the step 1) into a reaction kettle through a metering pump, controlling the temperature to be 50-55 ℃, the pH to be 7.5-8.5 and the stirring speed to be 200r/min for reaction for 60min, and enabling the basic copper carbonate to be precipitated and nucleated;
4) Adding the tannic acid solution prepared in the step 1) into a reaction kettle by a metering pump according to 0.5wt% of the addition of copper ions, controlling the temperature to be 50-55 ℃, and continuously reacting for 30min at the stirring speed of 200 r/min;
5) Stopping adding the copper salt solution, continuously adding the sodium carbonate solution, controlling the pH value to be 8.5-9.0, then increasing the temperature to 80-90 ℃, controlling the stirring speed to be 100r/min, and continuously reacting for 10min;
6) Filtering, washing the filtered basic copper carbonate by pure water until the conductivity of the basic copper carbonate in washing water is less than 100%, and then drying the washed basic copper carbonate by a flash evaporation machine to obtain basic copper carbonate powder;
7) Reducing the basic copper carbonate powder with hydrogen at 350-600 ℃ to obtain copper powder, and cooling and passivating the copper powder in an inert atmosphere to obtain superfine copper powder.
As shown in fig. 1, basic copper carbonate particle agglomerates are obtained in step 5) of example 1 of the present invention.
As shown in fig. 2 and 3, the ultrafine copper powder provided in the examples of the present invention has a uniform dispersion, specifically, a D50 particle size of 5.1um and an fsss particle size of 0.69um.
Further examination showed that the purity of the ultrafine copper powder provided in this example was 99.81%, the hydrogen loss value was 0.15%, and the apparent density was 0.79g/cm 3 The contents of Fe, pb, and As were 0.0006%, 0.0003%, 0.0005%, 0.0003%, 0.0001%, 0.0012%, and 0.012%, respectively, for acid-insoluble matters, respectively.
Example 2
A monodisperse superfine copper powder is prepared by the following steps:
1) Separately preparing Cu 2+ A copper nitrate solution with the concentration of 1mol/L, a sodium carbonate solution with the concentration of 150g/L and a tannic acid solution with the concentration of 5 wt%;
2) Adding the sodium carbonate solution prepared in the step 1) into a reaction kettle, starting stirring, adjusting the concentration of the sodium carbonate solution to 1g/L by using pure water, and then heating the sodium carbonate solution to 52 ℃;
3) Respectively adding the copper salt solution prepared in the step 1) and the sodium carbonate solution into a reaction kettle through a metering pump, controlling the temperature to be 50-55 ℃, the pH to be 7.5-8.5 and the stirring speed to be 270r/min, and reacting for 35min to nucleate basic copper carbonate precipitate;
4) Adding the tannic acid solution prepared in the step 1) into a reaction kettle by a metering pump according to 1wt% of the addition of copper ions, controlling the temperature to be 50-55 ℃, and continuously reacting for 20min at the stirring speed of 250 r/min;
5) Stopping adding the copper salt solution, continuously adding the sodium carbonate solution, controlling the pH value to be 8.5-9.0, then increasing the temperature to 80-90 ℃, controlling the stirring speed to be 150r/min, and continuously reacting for 5min;
6) Filtering, washing the filtered basic copper carbonate by pure water until the conductivity of the basic copper carbonate in washing water is less than 100%, and then drying the washed basic copper carbonate by a flash evaporation machine to obtain basic copper carbonate powder;
7) Reducing the basic copper carbonate powder with hydrogen at 350-600 ℃ to obtain copper powder, and cooling and passivating the copper powder in an inert atmosphere to obtain superfine copper powder.
Further detection shows that the D50 particle size of the superfine copper powder provided by the embodiment is 4.8um, the Fsss particle size is 1.19um, the purity is 99.88%, the hydrogen loss value is 0.13%, and the apparent density is 0.99g/cm 3 The alloy contained Fe (0.0008%), pb (0.0005%), as (0.0006%), cr (0.0005%), cd (0.0002%), S (0.0011%) and acid-insoluble substances (0.011%).
Example 3
A monodisperse superfine copper powder is prepared by the following steps:
1) Separately preparing Cu 2+ A copper chloride solution with the concentration of 2.5mol/L, a sodium carbonate solution with the concentration of 260g/L and a tannic acid solution with the concentration of 10 wt%;
2) Adding the sodium carbonate solution prepared in the step 1) into a reaction kettle, starting stirring, adjusting the concentration of the sodium carbonate solution to 5g/L by using pure water, and then heating the sodium carbonate solution to 55 ℃;
3) Respectively adding the copper salt solution and the sodium carbonate solution prepared in the step 1) into a reaction kettle by a metering pump, controlling the temperature to be 50-55 ℃, the pH to be 7.5-8.5 and the stirring speed to be 350r/min, and reacting for 10min to nucleate the basic copper carbonate precipitate;
4) Adding the tannic acid solution prepared in the step 1) into a reaction kettle by a metering pump according to 0.75wt% of the addition of copper, controlling the temperature to be 50-55 ℃, and continuously reacting for 10min at the stirring speed of 200 r/min;
5) Stopping adding the copper salt solution, continuously adding the sodium carbonate solution, controlling the pH value to be 8.5-9.0, then increasing the temperature to 80-90 ℃, controlling the stirring speed to be 200r/min, and continuously reacting for 1min;
6) Filtering, washing the filtered basic copper carbonate by pure water until the conductivity of the basic copper carbonate in washing water is less than 100%, and then drying the washed basic copper carbonate by a flash evaporation machine to obtain basic copper carbonate powder;
7) Reducing the basic copper carbonate powder with hydrogen at 350-600 ℃ to obtain copper powder, and cooling and passivating the copper powder in an inert atmosphere to obtain superfine copper powder.
Further examination shows that the D50 particle size of the superfine copper powder provided in the embodiment is 5.5um, the Fsss particle size is 1.5um, the purity is 99.81%, the hydrogen loss value is 0.10%, and the apparent density is 1.19g/cm 3 The contents of Fe, pb, as, cr, cd, S and acid-insoluble substances were 0.0005%, 0.0003%, 0.0002%, 0.0001%, 0.0010% and 0.012%, respectively.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made without departing from the spirit and scope of the invention.
Claims (3)
1. A preparation method of monodisperse superfine copper powder is characterized by comprising the following steps:
1) Separately preparing Cu 2+ Soluble copper salt solution with concentration of 1-2.5mol/L, sodium carbonate solution with concentration of 150-260g/L and tannic acid solution with concentration of 1-10 wt%;
2) Adding the sodium carbonate solution prepared in the step 1) into a reaction kettle, starting stirring, adjusting the concentration of the sodium carbonate solution to 1-5g/L by using pure water, and then heating to 50-55 ℃;
3) Respectively adding the copper salt solution and the sodium carbonate solution prepared in the step 1) into a reaction kettle through a metering pump, controlling the temperature to be 50-55 ℃, the pH value to be 7.5-8.5 and the stirring speed to be 200-350r/min, and reacting for 10-60min to nucleate the basic copper carbonate precipitate;
4) Adding the tannic acid solution prepared in the step 1) into a reaction kettle by a metering pump according to 0.5-1wt% of the addition of copper ions, controlling the temperature to be 50-55 ℃, and continuously reacting for 10-30min at the stirring speed of 200-250 r/min;
5) Stopping adding the copper salt solution, continuously adding the sodium carbonate solution, controlling the pH value to be 8.5-9.0, then heating the temperature to 80-90 ℃, and continuously reacting for 1-10min by controlling the stirring speed to be 100-200 r/min;
6) Filtering, washing the filtered basic copper carbonate by pure water until the conductivity of the basic copper carbonate in washing water is less than 100%, and then drying the washed basic copper carbonate to obtain basic copper carbonate powder;
7) Reducing the basic copper carbonate powder with hydrogen at 350-600 ℃ to obtain copper powder, and cooling and passivating the copper powder in an inert atmosphere to obtain superfine copper powder.
2. The method of claim 1, wherein the soluble copper salt in step 1) is selected from one or more of copper sulfate, copper nitrate and copper chloride.
3. Monodisperse ultrafine copper powder prepared by the preparation method according to claim 1 or 2.
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