CN108080651A - The preparation method of electric slurry nanometer silver-coated copper powder - Google Patents
The preparation method of electric slurry nanometer silver-coated copper powder Download PDFInfo
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- CN108080651A CN108080651A CN201711337617.2A CN201711337617A CN108080651A CN 108080651 A CN108080651 A CN 108080651A CN 201711337617 A CN201711337617 A CN 201711337617A CN 108080651 A CN108080651 A CN 108080651A
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- deionized water
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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
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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Abstract
The invention discloses a kind of electric slurry preparation methods of nanometer silver-coated copper powder, comprise the following steps:Deionized water is added to form mixed solution dispersant and reducing agent, be adjusted to neutrality mixed solution by adding alkaline solution;Mantoquita is taken to form copper salt solution with deionized water, addition complexing agent is complexed to obtain copper ammon solution;Copper ammon solution is added drop-wise in mixed solution obtained by step 1 and obtains reducing solution;Silver nitrate is taken to form silver salt solution with deionized water, addition complexing agent is complexed to obtain silver ammino solution, silver ammino solution is added drop-wise in reducing solution;Acquired solution is filtered and collects filter residue, is dried after deionized water and absolute ethyl alcohol washing are carried out to filter residue, so as to obtain electric slurry nanometer silver-coated copper powder;In the present invention, prepare that raw material components and processing step are simple, are easy to large-scale production and non-hazardous pollution-free, high-efficiency environment friendly;Gained nanometer silver-coated copper powder resistivity is small and with higher oxidation resistance, is meeting electrical property and cost reduction.
Description
Technical field
The present invention relates to metal-powder technical fields, and in particular to a kind of preparation side of electric slurry nanometer silver-coated copper powder
Method.
Background technology
Nanometer wicker copper powder has vast potential for future development at many aspects such as electronics industry.Its emphasis studied is letter
Change preparation section, improve producing efficiency, prepare the cladding copper powder of the thick fine and close high quality of silver coating.
Chelate extraction elite with silver ammino solution is mixed, added by a kind of preparation method of silver-plated copper powder of the prior art
Enter copper powder and electroless copper is carried out under the conditions of 40-90 DEG C;In the method for another chemical silvering and its chemical plating fluid and chemical plating,
Silver nitrate aqueous solution, formaldehyde ethanol solution and rare earth nitrate aqueous solution are sequentially added into carry out chemical plating.
Different according to pattern, wicker copper is generally divided into spherical, and sheet and the spherical wicker coppers of dendroid are usually using chemical method
System.Copper particle surface is after the cleaning treatment of weak acid and weak base, then carries out silver-plated displacement reaction.However, the surface of copper particle
Processing directly affects the conductive capability of wicker copper and silver layer covered effect, and the oxidation resistance for causing wicker copper is poor;Usually only
Have reduces influence of the surface treatment to wicker copper performance by increasing silver content, but raising silver content can increase the consumption of silver.
In summary, now need to provide a kind of electric slurry nano silver that can meet requirement on electric performance but also reduce cost
The preparation method of copper-clad powder.
The content of the invention
For this purpose, the present invention provides a kind of electric slurry preparation methods of nanometer silver-coated copper powder, comprise the following steps:
Step 1: it is 1 by mass ratio:3~1:4 dispersant and reducing agent adds deionized water to form mixed solution, passes through addition
After mixed solution is adjusted to neutrality by alkaline solution, simultaneously electromagnetic agitation 30min is added in reaction vessel;Wherein, deionized water
Volume be 60-70 times of dispersant quality;
Step 2: the mantoquita that quality is 5 times of dispersant quality is taken to form copper salt solution with deionized water, fully network is added after dissolving
Mixture is complexed to obtain copper ammon solution;Under the mixing speed of 2000r/min, with the rate of addition of 0.01L/min by copper ammon solution
It is added drop-wise in mixed solution obtained by step 1, and under conditions of reaction temperature is 70-90 DEG C, is gone back after reacting 30-60min
Stoste;Wherein, the volume of deionized water is 6 times of mantoquita quality, and the volume of complexing agent is 1.5 times of mantoquita quality;
Step 3: the silver nitrate that quality is mantoquita quality 5% is taken to form silver salt solution with deionized water, fully network is added after dissolving
Mixture is complexed to obtain silver ammino solution, under the mixing speed of 3000r/min, with the rate of addition of 0.02L/min by silver ammino solution
It is added drop-wise in reducing solution obtained by step 2, and under the conditions of reaction temperature is 70-90 DEG C, reacts 30-60min;Wherein, deionization
The volume of water is 120-150 times of silver nitrate quality, and the volume of complexing agent is 2 times of silver nitrate quality;
Step 4: step 3 acquired solution is filtered and collects filter residue, deionized water is carried out to filter residue and absolute ethyl alcohol is washed
It after washing, is dried in a vacuum with 50-80 DEG C of temperature, so as to obtain electric slurry nanometer silver-coated copper powder.
In step 1, reducing agent is set to ascorbic acid or glucose or hydrazine hydrate.
In step 1, dispersant is set to polyvinylpyrrolidone.
In step 1, alkaline solution is set to sodium hydroxide or potassium hydroxide.
In step 2, mantoquita is set to cupric sulfate pentahydrate or copper chloride or copper nitrate.
In step 2 and step 3, complexing agent is the ammonium hydroxide that mass fraction is 25% or ethylenediamine tetra-acetic acid or dodecane
Base benzene sulfonic acid sodium salt.
The present invention has the following advantages that part compared with the prior art:
In the present invention, on the one hand, prepare that raw material components and processing step are simple, are easy to mass produce, and tune can be passed through
Reagent and PH are saved to adjust nanometer wicker copper powder particles size and a pattern, all non-hazardous no dirt of the reagent added in W-response
Dye, high-efficiency environment friendly;On the other hand, the nanometer silver-coated copper powder resistivity that the preparation method is obtained after testing is less than 4.86 μ Ω
Cm has higher oxidation resistance;To sum up, the preparation-obtained electric slurry nano silver of method of the present invention is utilized
Copper-clad powder can reduce its cost under conditions of electrical property is met the requirements.
Description of the drawings
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution of the prior art
Embodiment or attached drawing needed to be used in the description of the prior art are briefly described, it should be apparent that, in describing below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, can also be obtained according to these attached drawings other attached drawings.
Fig. 1 is the TEM figures of present invention gained electric slurry nanometer silver-coated copper powder;
Fig. 2 is the resistivity curve figure of the electric slurry nanometer silver-coated copper powder of the different silver contents of present invention gained.
Specific embodiment
Technical scheme is clearly and completely described below in conjunction with attached drawing, it is clear that described implementation
Example is part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill
Personnel's all other embodiments obtained without making creative work, belong to the scope of protection of the invention.
As long as in addition, technical characteristic involved in invention described below different embodiments non-structure each other
It can be combined with each other into conflict.
Embodiment 1
A kind of preparation method of electric slurry nanometer silver-coated copper powder is present embodiments provided, is comprised the following steps:
Step 1: it is 1 by mass ratio:3~1:4 dispersant and reducing agent adds deionized water to form mixed solution, passes through addition
After mixed solution is adjusted to neutrality by alkaline solution, simultaneously electromagnetic agitation 30min is added in reaction vessel;Wherein, deionized water
Volume be 60-70 times of dispersant quality;
Step 2: the mantoquita that quality is 5 times of dispersant quality is taken to form copper salt solution with deionized water, fully network is added after dissolving
Mixture is complexed to obtain copper ammon solution;Under the mixing speed of 2000r/min, with the rate of addition of 0.01L/min by copper ammon solution
It is added drop-wise in mixed solution obtained by step 1, and under conditions of reaction temperature is 70-90 DEG C, is gone back after reacting 30-60min
Stoste;Wherein, the volume of deionized water is 6 times of mantoquita quality, and the volume of complexing agent is 1.5 times of mantoquita quality;
Step 3: the silver nitrate that quality is mantoquita quality 5% is taken to form silver salt solution with deionized water, fully network is added after dissolving
Mixture is complexed to obtain silver ammino solution, under the mixing speed of 3000r/min, with the rate of addition of 0.02L/min by silver ammino solution
It is added drop-wise in reducing solution obtained by step 2, and under the conditions of reaction temperature is 70-90 DEG C, reacts 30-60min;Wherein, deionization
The volume of water is 120-150 times of silver nitrate quality, and the volume of complexing agent is 2 times of silver nitrate quality;
Step 4: step 3 acquired solution is filtered and collects filter residue, deionized water is carried out to filter residue and absolute ethyl alcohol is washed
It after washing, is dried in a vacuum with 50-80 DEG C of temperature, so as to obtain electric slurry nanometer silver-coated copper powder.
In the present embodiment, on the one hand, prepare that raw material components and processing step are simple, are easy to mass produce, and can be with
Nanometer wicker copper powder particles size and a pattern are adjusted by adjusting reagent and PH, the reagent added in W-response is all non-hazardous
Pollution-free, high-efficiency environment friendly;On the other hand, the nanometer silver-coated copper powder resistivity that the preparation method is obtained after testing is less than 4.86 μ
Ω cm have higher oxidation resistance;To sum up, the above method preparation-obtained electric slurry nanometer wicker copper is utilized
Powder can reduce its cost under conditions of electrical property is met the requirements.
Specifically, in step 1, reducing agent is set to ascorbic acid or glucose or hydrazine hydrate, and dispersant is set to polyethylene
Pyrrolidones, alkaline solution are set to sodium hydroxide or potassium hydroxide.In the present embodiment, preferably described reducing agent is Vitamin C
Acid.
In step 2, mantoquita is set to cupric sulfate pentahydrate or copper chloride or copper nitrate;In the present embodiment, preferably described copper
Salt is cupric sulfate pentahydrate.
In step 2 and step 3, complexing agent is the ammonium hydroxide that mass fraction is 25% or ethylenediamine tetra-acetic acid or dodecane
Base benzene sulfonic acid sodium salt;In the present embodiment, preferably described complexing agent is the ammonium hydroxide that mass fraction is 25%.
Embodiment 2
On the basis of embodiment 1, the present embodiment further provides for a kind of specific embodiment:
Step 1: by 5.79g VC(Ascorbic acid)With 1.5g PVP(Polyvinylpyrrolidone)Add in the deionized water of 200ml
Middle formation mixed solution, and add alkaline solution and the acid-base value of the mixed solution is adjusted to neutral, it is then that neutrality mixing is molten
Liquid is added in three-necked bottle, and electromagnetic agitation 30min;
Step 2: the deionized water of 7.47g cupric sulfate pentahydrates solution and 50ml is taken to be mixed to form copper salt solution, fully add after dissolving
The ammonium hydroxide that 30ml mass fractions is added to be 25%, obtains copper ammon solution;Low whipping speed is under the stirring of 2000r/min, with 0.01L/
Copper ammon solution is added drop-wise in the three-necked bottle after step 1 by the rate of addition of min, and is 70-90 DEG C of condition in reaction temperature
Under, obtain reducing solution after reacting 30-60min;
Step 3: the deionized water of 0.566g silver nitrates and 50ml is taken to be mixed to form silver salt solution, addition 1.5ml mass fractions are
25% ammonium hydroxide complexing is silver ammino solution, and low whipping speed is under the stirring of 3000r/min, is incited somebody to action with the rate of addition of 0.02L/min
Silver ammino solution is added drop-wise in the three-necked bottle after step 2 and reacts 30 min;
Step 4: the solution after step 3 is reacted is filtered and collects filter residue, using deionized water and alcohol to filter residue
After being cleaned multiple times, filter residue is placed in thermostatic drying chamber with 70 DEG C of drying, electric slurry nanometer silver-coated copper powder is obtained, such as schemes
Shown in 1.
Embodiment 3
On the basis of embodiment 1, the present embodiment further provides for a kind of specific embodiment:
Step 1: by 46.32g VC(Ascorbic acid)With 12g PVP(Polyvinylpyrrolidone)Add in the deionized water of 800ml
Middle formation mixed solution, and add alkaline solution and the acid-base value of the mixed solution is adjusted to neutral, it is then that neutrality mixing is molten
Liquid is added in three-necked bottle, and electromagnetic agitation 30min;
Step 2: the deionized water of 59.76g cupric sulfate pentahydrates solution and 350ml is taken to be mixed to form copper salt solution, fully after dissolving
The ammonium hydroxide that 90ml mass fractions are 25% is added, obtains copper ammon solution;Low whipping speed be 2000r/min stirring under, with
Copper ammon solution is added drop-wise in the three-necked bottle after step 1 by the rate of addition of 0.01L/min, and is 70-90 DEG C in reaction temperature
Under the conditions of, obtain reducing solution after reacting 30-60min;
Step 3: the deionized water of 2.866g silver nitrates and 400ml is taken to be mixed to form silver salt solution, addition 5ml mass fractions are
25% ammonium hydroxide complexing is silver ammino solution, and low whipping speed is under the stirring of 3000r/min, is incited somebody to action with the rate of addition of 0.02L/min
Silver ammino solution is added drop-wise in the three-necked bottle after step 2 and reacts 30 min;
Step 4: the solution after step 3 is reacted is filtered and collects filter residue, using deionized water and alcohol to filter residue
After being cleaned multiple times, filter residue is placed in thermostatic drying chamber with 70 DEG C of drying, electric slurry nanometer silver-coated copper powder is obtained, and is somebody's turn to do
Powder particle is spherical shape.
On the basis of embodiment 2 and 3, Resistivity testing is carried out with nanometer silver-coated copper powder to the electric slurry each obtained,
As shown in Fig. 2, silver content is higher, then resistivity is lower.
Obviously, the above embodiments are merely examples for clarifying the description, and is not intended to limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And the obvious variation thus extended out or
Among changing still in the protection domain of the invention.
Claims (6)
1. the electric slurry preparation method of nanometer silver-coated copper powder, it is characterised in that:It comprises the following steps:
Step 1: it is 1 by mass ratio:3~1:4 dispersant and reducing agent adds deionized water to form mixed solution, passes through addition
After mixed solution is adjusted to neutrality by alkaline solution, simultaneously electromagnetic agitation 30min is added in reaction vessel;Wherein, deionized water
Volume be 60-70 times of dispersant quality;
Step 2: the mantoquita that quality is 5 times of dispersant quality is taken to form copper salt solution with deionized water, fully network is added after dissolving
Mixture is complexed to obtain copper ammon solution;Under the mixing speed of 2000r/min, with the rate of addition of 0.01L/min by copper ammon solution
It is added drop-wise in mixed solution obtained by step 1, and under conditions of reaction temperature is 70-90 DEG C, is gone back after reacting 30-60min
Stoste;Wherein, the volume of deionized water is 6 times of mantoquita quality, and the volume of complexing agent is 1.5 times of mantoquita quality;
Step 3: the silver nitrate that quality is mantoquita quality 5% is taken to form silver salt solution with deionized water, fully network is added after dissolving
Mixture is complexed to obtain silver ammino solution, under the mixing speed of 3000r/min, with the rate of addition of 0.02L/min by silver ammino solution
It is added drop-wise in reducing solution obtained by step 2, and under the conditions of reaction temperature is 70-90 DEG C, reacts 30-60min;Wherein, deionization
The volume of water is 120-150 times of silver nitrate quality, and the volume of complexing agent is 2 times of silver nitrate quality;
Step 4: step 3 acquired solution is filtered and collects filter residue, deionized water is carried out to filter residue and absolute ethyl alcohol is washed
It after washing, is dried in a vacuum with 50-80 DEG C of temperature, so as to obtain electric slurry nanometer silver-coated copper powder.
2. the electric slurry according to claim 1 preparation method of nanometer silver-coated copper powder, it is characterised in that:In step 1
In, reducing agent is set to ascorbic acid or glucose or hydrazine hydrate.
3. the electric slurry according to claim 1 or 2 preparation method of nanometer silver-coated copper powder, it is characterised in that:In step
In rapid one, dispersant is set to polyvinylpyrrolidone.
4. the electric slurry according to any one of claim 1-3 preparation method of nanometer silver-coated copper powder, feature exist
In:In step 1, alkaline solution is set to sodium hydroxide or potassium hydroxide.
5. the preparation method of the electric slurry nanometer silver-coated copper powder according to any one of claim 1-4, feature exist
In:In step 2, mantoquita is set to cupric sulfate pentahydrate or copper chloride or copper nitrate.
6. the preparation method of the electric slurry nanometer silver-coated copper powder according to any one of claim 1-5, feature exist
In:In step 2 and step 3, complexing agent is the ammonium hydroxide that mass fraction is 25% or ethylenediamine tetra-acetic acid or detergent alkylate sulphur
Sour sodium.
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Cited By (3)
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CN109355034A (en) * | 2018-10-24 | 2019-02-19 | 焦作市高森建电子科技有限公司 | A kind of conducting resinl silver-coated copper powder and preparation method thereof |
CN111304640A (en) * | 2020-03-10 | 2020-06-19 | 哈尔滨工业大学(深圳)(哈尔滨工业大学深圳科技创新研究院) | Silver-coated copper powder, preparation method thereof and electronic paste |
WO2024113797A1 (en) * | 2022-12-01 | 2024-06-06 | 湖南维胜科技电路板有限公司 | Method for preparing fine copper powder by recovering pcb alkaline etching waste solution |
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