CN110842190B - Preparation method of silver-coated copper powder - Google Patents
Preparation method of silver-coated copper powder Download PDFInfo
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- CN110842190B CN110842190B CN201910961023.1A CN201910961023A CN110842190B CN 110842190 B CN110842190 B CN 110842190B CN 201910961023 A CN201910961023 A CN 201910961023A CN 110842190 B CN110842190 B CN 110842190B
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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
- B22F1/17—Metallic particles coated with metal
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1827—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment only one step pretreatment
- C23C18/1834—Use of organic or inorganic compounds other than metals, e.g. activation, sensitisation with polymers
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
- C23C18/44—Coating with noble metals using reducing agents
Abstract
The invention discloses a preparation method of silver-coated copper powder, belonging to the technical field of metal powder. Adding superfine copper powder into an activation-autocatalysis film agent solution, reacting for 5-30 min at normal temperature under stirring, carrying out solid-liquid separation, and washing the solid with deionized water to obtain pretreated copper powder; adding the pretreated copper powder into deionized water, uniformly dispersing to obtain a copper powder dispersion, dropwise adding a silver nitrate solution at the temperature of 30-80 ℃, stirring for 1-10 min to obtain a silver adhesive film coated on the surface of the copper powder, adding a silver nitrate-sodium thiosulfate complex solution, adding a reducing agent, reacting for 10-60 min under a stirring condition, carrying out solid-liquid separation, washing the solid with deionized water, soaking the solid with ethanol, and carrying out vacuum drying to obtain the silver-coated copper powder. According to the invention, the surface of copper powder is activated, autocatalytic silver colloidal nucleus is formed through a displacement reaction, and the halogen-containing anionic surfactant enables the deposition of silver to be oriented to the surface of the copper powder, so that the compact silver-coated copper powder is formed.
Description
Technical Field
The invention relates to a preparation method of silver-coated copper powder, belonging to the technical field of metal powder.
Background
The copper powder is used for preparing paste and used for preparing conductive adhesive or conductive film, so that the surface of the copper powder is easy to oxidize, and therefore, the pure silver powder is mostly adopted as a conductive phase material at home and abroad at present. However, silver is expensive, and the replacement or partial replacement of silver by copper is an effective way to reduce the cost in view of the cost, so that a process technology for plating silver on the surface of copper powder appears.
The existing literature mainly prepares silver-coated copper powder by a chemical plating method, but stannous chloride sensitization, palladium chloride activation and chemical silver plating procedures are often needed, except for more procedures, silver ions can nucleate in a large amount and grow up automatically under certain reduction conditions to form silver particle powder instead of being plated on the copper powder in an all-directional manner. Often results in a silver layer that is thin enough to not adequately block copper from oxygen, and the resulting copper oxidation problem.
Disclosure of Invention
The invention provides a preparation method of silver-coated copper powder, aiming at the problem of preparation of the silver-coated copper powder in the prior art, the invention carries out mild complexing corrosion on the surface of the copper powder through organic ammonium salt and ammonium chloride salt to form a new active surface of copper, halogen ions are riveted on the surface to ensure that silver ions can be directionally deposited on the surface of the copper, a silver nuclear glue layer is deposited on the surface of the copper powder through a displacement reaction to form an autocatalytic silver layer, the deposition rate of the silver ions on the surface of the copper powder is accelerated, and the silver-coated copper powder is formed; for dendritic micron copper powder, the general method for plating silver is not easy to deposit silver into tiny gaps due to geometric effect to form a complete coating silver layer. The invention can easily finish the surface coating of the copper powder with complex configuration due to the action process of the surface chemical agent containing the halogen ions.
The method adopts the activated copper powder surface, and forms the autocatalysis silver colloid nucleus through the replacement reaction and the halogen-containing anionic surfactant to ensure that the deposition of the silver is oriented to the copper powder surface to form the compact silver-coated copper powder.
A preparation method of silver-coated copper powder comprises the following specific steps:
(1) adding superfine copper powder into the activating-autocatalysis film agent solution, reacting for 5-30 min at normal temperature under stirring, carrying out solid-liquid separation, and washing the solid with deionized water to obtain pretreated copper powder;
(2) adding the pretreated copper powder into deionized water, uniformly dispersing to obtain a copper powder dispersion, dropwise adding a silver nitrate solution at the temperature of 30-80 ℃, stirring for 1-10 min to obtain a silver adhesive film coated on the surface of the copper powder, adding a silver nitrate-sodium thiosulfate complex solution, adding a reducing agent, reacting for 10-60 min under a stirring condition, carrying out solid-liquid separation, washing the solid with deionized water, soaking the solid with ethanol, and carrying out vacuum drying to obtain the silver-coated copper powder.
The particle size of the superfine copper powder in the step (1) is 1-50 microns, and the activating-autocatalysis film agent solution is a mixed aqueous solution of one of tetramethylammonium chloride, tetrabutylammonium bromide and tetrabutylammonium iodide and ammonium chloride.
Further, the mass percentage concentration of tetramethylammonium chloride, tetrabutylammonium bromide or tetrabutylammonium iodide in the activation-autocatalysis film agent solution is 0.05-2%, and the mass percentage concentration of ammonium chloride is 2-10%.
The concentration of the silver nitrate solution in the step (2) is 0.05-0.2 mol/L.
The mass of silver in the silver nitrate solution is 0.5-2% of that of copper powder.
In the step (2), the concentration of silver nitrate in the silver nitrate-sodium thiosulfate complex solution is 0.5-3 mol/L, the concentration of sodium thiosulfate is 50-300 g/L, and the mass of silver in the silver nitrate-sodium thiosulfate complex solution is 5-60% of that of copper powder; the reducing agent is one or two of potassium sodium tartrate, sodium formate, formaldehyde, hydrazine hydrate or ethylene diamine tetraacetic acid disodium salt, and the adding amount of the reducing agent is 1.5 times of the total silver molar amount in the silver nitrate solution and the silver nitrate-sodium thiosulfate complex solution.
The invention has the beneficial effects that:
according to the method, stannous chloride and palladium chloride are not needed to be used as a sensitizing and activating step, the surface of copper powder is slightly subjected to complexing corrosion by an amino surface chemical agent solution (organic ammonium salt and ammonium chloride salt solution) for removing an oxidation film to form a new active surface of copper, namely halogen ions (Cl)-，Br-，I-) Riveting the copper powder to the surface, so that silver ions can be directionally deposited on the copper surface to form an autocatalytic silver layer, the deposition rate of silver on the surface of the copper powder is accelerated, and the silver is coated on the surface of the copper powder; the sodium thiosulfate complex silver ions can be gradually dissolved out and reduced on the surface of copper powder according to the principle of equilibrium concentration, the supersaturated self-nucleation growth process of the silver ions under the reduction condition can be inhibited, and particularly, the dendritic micron copper powder wraps the silver layer to prevent the silver layer from being oxidized.
Drawings
FIG. 1 is a scanning electron micrograph of silver-coated dendritic copper powder according to example 1;
FIG. 2 is a scanning electron micrograph of silver-coated copper powder according to example 2;
FIG. 3 is a scanning electron micrograph of a comparative silver-coated copper powder.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Example 1: a preparation method of silver-coated copper powder comprises the following specific steps:
(1) adding 50g of superfine copper powder into 100mL of activating-autocatalysis film agent solution, reacting for 20min at normal temperature under stirring, carrying out solid-liquid separation, and washing the solid with deionized water to obtain pretreated copper powder; wherein the average grain diameter of the superfine copper powder is 25 μm, the shape is dendritic, the activation-autocatalysis film agent solution is a mixed aqueous solution of tetramethylammonium chloride and ammonium chloride, the mass percentage concentration of the tetramethylammonium chloride in the activation-autocatalysis film agent solution is 1.0 percent, and the mass percentage concentration of the ammonium chloride is 8 percent;
(2) adding the pretreated copper powder into 30mL of deionized water, uniformly dispersing to obtain copper powder slurry, dropwise adding 80mL of silver nitrate A solution, stirring for 5min to obtain a silver adhesive film coated on the surface of the copper powder, adjusting the pH to 11 with sodium hydroxide, adding 160mL of silver nitrate-sodium thiosulfate complex solution, adding 80mL of reducing agent solution (hydrazine hydrate solution), reacting for 30min at the temperature of 40 ℃ under the condition of stirring, carrying out solid-liquid separation, washing the solid with deionized water, soaking the solid with ethanol, and carrying out vacuum drying to obtain silver-coated copper powder; wherein the concentration of the silver nitrate A solution is 0.05mol/L, the concentration of silver nitrate in the silver nitrate-sodium thiosulfate complex solution is 0.5mol/L, the concentration of sodium thiosulfate is 220g/L, the mass of silver in the silver nitrate-sodium thiosulfate complex solution is 17.28 percent of the mass of copper powder, the addition amount of a reducing agent solution (80 percent of hydrazine hydrate), and the addition amount of the reducing agent (the hydrazine hydrate solution) is 2 times of the total molar amount of silver in the silver nitrate solution and the silver nitrate-sodium thiosulfate complex solution;
the scanning electron micrograph of the silver-coated copper powder of this example is shown in fig. 1, white is the silver layer, and gray is the copper powder matrix, and it can be seen from fig. 1 that the surface of the dendritic copper powder is coated with the silver layer.
Example 2: a preparation method of silver-coated copper powder comprises the following specific steps:
(1) adding 50g of superfine copper powder into 100mL of activating-autocatalysis film agent solution, reacting for 15min at normal temperature under stirring, carrying out solid-liquid separation, and washing the solid with deionized water to obtain pretreated copper powder; wherein the average grain diameter of the superfine copper powder is 5 mu m, the shape of the superfine copper powder is similar to a sphere, the activating-autocatalysis film agent solution is a mixed aqueous solution of tetrabutylammonium bromide and ammonium chloride, the mass percentage concentration of the tetrabutylammonium bromide in the activating-autocatalysis film agent solution is 1.5 percent, and the mass percentage concentration of the ammonium chloride is 8 percent;
(2) adding the pretreated copper powder into 30mL of deionized water, uniformly dispersing to obtain copper powder slurry, dropwise adding 30mL of silver nitrate solution, stirring for 8min to obtain a silver colloid film coated on the surface of the copper powder, adjusting the pH to 11 by using 5% sodium hydroxide solution, adding 100mL of silver nitrate-sodium thiosulfate complex solution, adding 180mL of reducing agent solution (sodium formate solution), reacting for 30min at the temperature of 50 ℃ under stirring, carrying out solid-liquid separation, washing the solid by using deionized water, soaking the solid in ethanol, and carrying out vacuum drying to obtain silver-coated copper powder; wherein the concentration of the silver nitrate solution is 0.05mol/L, the concentration of the silver nitrate in the silver nitrate-sodium thiosulfate complex solution is 1mol/L, the concentration of the sodium thiosulfate is 150g/L, the mass of the silver in the silver nitrate-sodium thiosulfate complex solution is 21.6 percent of the mass of the copper powder, and the addition amount of the reducing agent (sodium formate) is 1.8 times of the total molar mass of the silver in the silver nitrate solution and the silver nitrate-sodium thiosulfate complex solution;
the scanning electron micrograph of the silver-coated copper powder of this example is shown in fig. 2, white is the silver layer, and gray is the copper powder matrix, and it can be seen from fig. 2 that the copper powder surfaces are all coated with a thicker silver layer.
Comparative example: the preparation method of the silver-coated copper powder comprises the following specific steps:
weighing 50g of commercially available superfine copper powder, wherein the average particle size of the superfine copper powder is 5 mu m, and the shape of the superfine copper powder is similar to a sphere; adding untreated superfine copper powder into deionized water, uniformly mixing to obtain copper powder dispersion, dropwise adding 100mL of silver nitrate solution, adding 160mL of silver nitrate-sodium thiosulfate complex solution, adding 100mL of reducing agent solution (sodium formate solution), reacting for 60min at 60 ℃ under stirring, carrying out solid-liquid separation, washing solids by using deionized water, soaking by using ethanol solution, and carrying out vacuum drying at 40 ℃ to obtain the silver-coated copper powder, wherein the concentration of the silver nitrate solution is 0.05mol/L, the concentration of silver nitrate in the silver nitrate-sodium thiosulfate complex solution is 1mol/L, the concentration of sodium thiosulfate is 220g/L, the mass of silver in the silver nitrate-sodium thiosulfate complex solution is 21.6 percent of the mass of the copper powder, the concentration of the reducing agent solution (sodium formate solution) is 160g/L, and the addition amount of the reducing agent (sodium formate) is the total mass of silver in the silver nitrate solution and the silver-sodium thiosulfate complex solution 1.8 times of the mass;
the scanning electron microscope of the silver-coated copper powder of the comparative example is shown in FIG. 3, white is a silver layer, gray is a copper powder matrix, and as can be seen from FIG. 3, only part of the surface of the copper powder is coated with silver.
Example 3: a preparation method of silver-coated copper powder comprises the following specific steps:
(1) adding 50g of superfine copper powder into the activating-autocatalysis film agent solution, reacting for 10min at normal temperature under stirring, carrying out solid-liquid separation, and washing the solid by using deionized water to obtain pretreated copper powder; wherein the average particle size of the superfine copper powder is 1 mu m, the shape of the superfine copper powder is similar to a sphere, the activating-autocatalysis film agent solution is a mixed aqueous solution of tetrabutylammonium iodide and ammonium chloride, the mass percentage concentration of the tetrabutylammonium iodide in the activating-autocatalysis film agent solution is 1.5%, and the mass percentage concentration of the ammonium chloride is 10%;
(2) adding the pretreated copper powder into deionized water, uniformly dispersing to obtain a copper powder dispersion, dropwise adding a silver nitrate solution, stirring for 15min to obtain a silver adhesive film coated on the surface of the copper powder, adding 120ml of a silver nitrate-sodium thiosulfate complexing solution, adding a reducing agent solution (a potassium sodium tartrate alkali solution) under stirring, reacting for 40min at the temperature of 60 ℃ under stirring, carrying out solid-liquid separation, washing the solid with deionized water, soaking the solid with ethanol, and carrying out vacuum drying to obtain silver-coated copper powder; wherein the concentration of the silver nitrate A solution is 0.05mol/L, the concentration of silver nitrate in the silver nitrate-sodium thiosulfate complex solution is 2mol/L, the concentration of sodium thiosulfate is 220g/L, the mass of silver in the silver nitrate-sodium thiosulfate complex solution is 51.8 percent of the mass of copper powder, the concentration of a reducing agent solution (potassium sodium tartrate solution) is 150g/L, and the adding amount of a reducing agent (potassium sodium tartrate) is 2.0 times of the total molar amount of silver in the silver nitrate solution and the silver nitrate-sodium thiosulfate complex solution;
the surface of the copper powder of the silver-coated copper powder is uniformly coated with a thick silver layer.
Claims (7)
1. The preparation method of the silver-coated copper powder is characterized by comprising the following specific steps of:
(1) adding superfine copper powder into the activating-autocatalysis film agent solution, reacting for 5-30 min at normal temperature under stirring, carrying out solid-liquid separation, and washing the solid with deionized water to obtain activated copper powder; wherein the activating-autocatalysis film agent solution is a mixed aqueous solution of ammonium chloride and one of tetramethylammonium chloride, tetrabutylammonium bromide and tetrabutylammonium iodide;
(2) adding activated copper powder into deionized water, uniformly dispersing to obtain a copper powder dispersion liquid, dropwise adding a silver nitrate solution, stirring for 1-10 min to obtain a silver adhesive film coated on the surface of the copper powder, adding a silver nitrate-sodium thiosulfate complexing solution, adding a reducing agent, reacting for 10-60 min at the temperature of 30-80 ℃ under stirring, carrying out solid-liquid separation, washing the solid with deionized water, soaking the solid with ethanol, and carrying out vacuum drying to obtain the silver-coated copper powder.
2. The method for producing silver-coated copper powder according to claim 1, wherein: the particle size of the superfine copper powder in the step (1) is 1-50 mu m.
3. The method for producing silver-coated copper powder according to claim 2, wherein: the mass percentage concentration of tetramethylammonium chloride, tetrabutylammonium bromide or tetrabutylammonium iodide in the activation-autocatalysis film agent solution is 0.05-2%, and the mass percentage concentration of ammonium chloride is 2-10%.
4. The method for producing silver-coated copper powder according to claim 1, wherein: the concentration of the silver nitrate solution in the step (2) is 0.05-0.2 mol/L.
5. The method for producing silver-coated copper powder according to claim 4, wherein: the mass of silver in the silver nitrate solution is 0.5-2% of that of the copper powder.
6. The method for producing silver-coated copper powder according to claim 1, wherein: in the step (2), the concentration of silver nitrate in the silver nitrate-sodium thiosulfate complex solution is 0.5-3 mol/L, the concentration of sodium thiosulfate is 50-300 g/L, and the mass of silver in the silver nitrate-sodium thiosulfate complex solution is 5-60% of that of copper powder.
7. The method for producing silver-coated copper powder according to claim 1, wherein: the reducing agent is potassium sodium tartrate, sodium formate, formaldehyde, hydrazine hydrate or ethylene diamine tetraacetic acid disodium salt, and the adding amount of the reducing agent is 1.5-2.0 times of the total silver molar mass in the silver nitrate solution and the silver nitrate-sodium thiosulfate complex solution.
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| CN113877606A (en) * | 2021-09-30 | 2022-01-04 | 合肥工业大学 | Non-complete coated core-shell nanoparticle self-driven catalyst and application thereof |
| CN114535595A (en) * | 2022-03-11 | 2022-05-27 | 南京理工大学 | Method for preparing ultrafine silver-copper nanoparticles by reactive liquid-phase laser ablation method |
| CN115106523A (en) * | 2022-05-24 | 2022-09-27 | 中科铜都粉体新材料股份有限公司 | Preparation method of high-stability coated copper powder |
| CN116060610B (en) * | 2023-03-07 | 2023-10-20 | 东方电气集团科学技术研究院有限公司 | Silver-coated copper powder and preparation method and application thereof |
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