CN102161104A - Preparation method of copper-silver composite powder - Google Patents
Preparation method of copper-silver composite powder Download PDFInfo
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- CN102161104A CN102161104A CN 201110083797 CN201110083797A CN102161104A CN 102161104 A CN102161104 A CN 102161104A CN 201110083797 CN201110083797 CN 201110083797 CN 201110083797 A CN201110083797 A CN 201110083797A CN 102161104 A CN102161104 A CN 102161104A
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Abstract
The invention relates to a preparation method of copper-silver composite powder. The copper-silver composite powder has a coated nuclear-shell structure; a nuclear layer is made of copper-silver alloy, and the shell layer is made of silver. The preparation method comprises the steps: firstly, adding a mixed aqueous solution of AgNO3 and Cu(NO3)2.3H2O into a mixed aqueous solution consisting of a reducing agent and a dispersing agent to obtain a copper-silver alloy solution containing the reducing agent; then adding an AgNO3 aqueous solution into the copper-silver alloy solution containing the reducing agent, and leading silver to be deposited and coated on the surface of the copper-silver alloy; and then obtaining the 0.3-3mum copper-silver composite powder after filtering, cleaning, drying and surface densified treatment. In the obtained copper-silver composite powder, the coating of the outer-layer silver is uniform, the compact density is high, the conductivity is good, and the high-temperature oxidation resistance is strong.
Description
Technical field
The present invention relates to field of material preparation, specifically, relate to a kind of preparation method of cuprum argentum composite powder.
Background technology
It is the development of the electric slurry of major function phase that the fast development of electronic information industry has driven with the submicron particle, and along with the development of electronic component to aspects such as miniaturization, precise treatment, multifunctions, also more and more higher to the requirement of electric slurry.Common submicron particle has silver powder, bronze, palladium powder, nickel powder, aluminium powder, copper powder etc., and wherein excellent comprehensive performances is widely used in the electronic component silver powder because of having extremely.The low price of copper, and have the specific insulation close with silver, oxidized but copper powder is easy in preparation and use, make the electric conductivity of material reduce.And use the cuprum argentum composite powder physical efficiency to take into account both advantages, and both can reduce cost, can improve the non-oxidizability of powder again, thereby have development prospect widely.
The preparation method of cuprum argentum composite powder has a variety of, and what the most generally adopt is the chemical replacement reducing process, promptly by displacement reaction, replaces the copper of copper particle surface with silver, thereby obtains the silver-plated copper powder of surface cladding type structure.But this method at first needs copper powder carried out preliminary treatment such as cleaning surfaces, activation, sensitization, and copper is easy to oxidized in the preprocessing process, the process that coats in addition is slower, be difficult to form uniform coating, cause coating imprecision, and surface coated silver layer is thinner, during high temperature sintering a little less than the oxidation resistance.Usually also adopt the introducing reducing agent to get the reduction that method promotes silver ion; to obtain to have the silver coating of certain thickness even compact, cause silver-colored homogeneous nucleation easily but add reducing agent, be not easy to control; and the less stable of silver plating liquid has reduced silver-colored service efficiency and covered effect.
Notification number be CN 101244459B patent disclosure a kind of preparation method who adopts rare earth modified chemical silvering copper powder, adopt cleaning, activation, sensitization before this method copper powder plating and adopt ultrasonic wave auxiliary, the technology more complicated, cost is higher.
Notification number be CN 1300381C patent disclosure a kind of preparation method of conducting electricity compound copper powder and compound copper conductor slurry, this method adopts introduces reducing agent being reduced to silver and being deposited on copper powder surface formation cladded type structure silver ion, strong reductants such as the formaldehyde that adopts, hydrazine hydrate make reaction speed fast, be not easy to reduce the spontaneous nucleation growth of silver, reduced silver-colored service efficiency.
Publication number is that the patent of CN 101214547A is by electronation, change the surface topography layout of micron order copper silver particle, make it contain the Nano grade body structure surface, though reduced surperficial sintering or melt temperature, when high temperature sintering, oxygen is easy to pass the top layer and makes the copper oxidation, this system does not use dispersant or ultrasonic dispersion to assist in addition, system dispersed relatively poor, collision is easily reunited between particle in preparation process, and it is wide that the product particle diameter is distributed.
Summary of the invention
Technical problem: the preparation method who the purpose of this invention is to provide the cuprum argentum composite powder of a kind of with low cost, simple to operate, easy control of reaction, good reproducibility, and this cuprum argentum composite powder is spherical, between 0.5 ~ 3 micron of the average grain diameter, and heap real density height, conduct electricity very well, high-temperature oxidation resistance is strong.
Technical scheme
A kind of preparation method of cuprum argentum composite powder is characterized in that, this method may further comprise the steps:
(1) mixed aqueous solution of preparation reducing agent and dispersant, preparation AgNO
3With Cu (NO
3)
23H
2The mixed aqueous solution of O, wherein, AgNO
3Mass volume ratio concentration be 5 ~ 100 grams per liters, Cu (NO
3)
23H
2The mass volume ratio concentration of O is 50 ~ 400 grams per liters, and in the mixed nitrate solution silver and the mol ratio of copper between 1:3 ~ 20, under stirring with AgNO
3With Cu (NO
3)
23H
2The mixed aqueous solution of O is added in the mixed aqueous solution of being made up of reducing agent and dispersant, and with the pH value of ammonia spirit or sodium hydroxide solution conditioned reaction solution between 3 ~ 13, temperature is controlled at 15 ~ 90 ℃, under stirring, reacted 0.5 ~ 4 hour, obtain containing the solution of the Kufil of reducing agent, the consumption of described reducing agent requires to react excessive 0.2 ~ 2 times than equivalent, and the mass volume ratio concentration of dispersant is 2 ~ 100 grams per liters
(2) preparation mass volume ratio concentration is the AgNO of 20 ~ 300 grams per liters
3The aqueous solution, under stirring with AgNO
3The aqueous solution be added in the solution of the Kufil that contains reducing agent, and with the pH value of ammonia spirit or sodium hydroxide solution conditioned reaction solution between 3 ~ 13, temperature is controlled at 15 ~ 80 ℃, question response fully after, the cuprum argentum composite powder that leave standstill, filter, wash, dry, surperficial densification obtains 0.5 ~ 3 micron granularity after handling.
Used reducing agent is any one in ascorbic acid, formaldehyde, sodium hypophosphite, hydrazine hydrate, sodium borohydride, the potassium borohydride.Used dispersant is any one or any several any ratio in polyvinylpyrrolidone, gelatin, softex kw, polyethylene glycol, polyvinyl alcohol, Arabic gum, the soluble starch.
Used surperficial densification is treated to ball milling or coating machine coats.
The cuprum argentum composite powder of preparation is the cladded type nucleocapsid structure, and stratum nucleare is a Kufil, and shell is a silver.Cuprum argentum composite powder is spherical, silver content in wt% between 10 ~ 70%.
The cuprum argentum composite powder of the present invention's preparation, adopt its pattern of sem observation and covered effect,, survey particle size and distribution with the laser particle size analysis tester with the heap real density of heap real density instrument survey powder, survey silver content with atomic spectrophotometer, survey the powder resistance rate with the four point probe instrument.Adopt thermogravimetric analyzer to survey the non-oxidizability of powder.
Beneficial effect:
1. the method for preparing cuprum argentum composite powder of the present invention, in a reactor, carry out in two steps, i.e. preparation earlier contains the solution system of the Kufil of reducing agent, adding liquor argenti nitratis ophthalmicus again makes silver coat growth on the Kufil surface, wherein silver atoms is contained on the Kufil surface, help in the coated with silver on surface process absorption to silver to form uniform cladded type structure, both save the pretreating process on copper powder surface in the general technology, suppress silver-colored spontaneous nucleation growth again, improved silver-colored service efficiency and covered effect.
2. the cuprum argentum composite powder of the present invention's preparation is spherical, average grain diameter is between 0.5 ~ 3 micron, and by making the silver layer of coating fine and close more after the surperficial densification processing, improved the obstruction ability of under the high temperature oxygen being passed the top layer, make high-temperature oxidation resistance strong, conductance is good, and in the cuprum argentum composite powder silver content in wt% between 10 ~ 70%, save a large amount of noble metal silver, reduced cost.
3. the method for preparing cuprum argentum composite powder provided by the invention, stable process conditions is reliable, and is simple to operation, is fit to industrial mass production.
Description of drawings
Fig. 1 prepares the schematic diagram at cuprum argentum composite powder end for the present invention.
Fig. 2 is the sem photograph of the cuprum argentum composite powder of embodiment 1 gained.
Fig. 3 is the sem photograph of the cuprum argentum composite powder of Comparative Examples 1 gained.
Fig. 4 is the sem photograph of the cuprum argentum composite powder of Comparative Examples 2 gained.
The specific embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
Get 30 gram AgNO
3Be dissolved in 300 ml distilled waters and be mixed with AgNO
3Solution; Get 10 gram AgNO
3With 57 gram Cu (NO
3)
23H
2O is dissolved in altogether in 200 ml distilled waters and is mixed with AgNO
3With Cu (NO
3)
23H
2The mixed aqueous solution of O, silver is 1:4 with the mol ratio of copper in the mixed solution; Get 80 the gram ascorbic acid and 8 the gram polyvinylpyrrolidones be dissolved in the mixed aqueous solution that is mixed with reducing agent and dispersant in 1 liter of distilled water altogether.Under stirring with AgNO
3With Cu (NO
3)
23H
2The mixed aqueous solution of O be added to by mixing of forming of reducing agent and dispersant water-soluble in, the dropping time is 20 minutes, and be that the pH value of 4% ammonia spirit conditioned reaction solution is 4.5 with mass fraction, temperature is controlled at 70 ℃, reaction is after 2 hours under stirring, obtain containing the solution of the Kufil of reducing agent, with AgNO
3The aqueous solution be added in the solution of the Kufil that contains reducing agent, and be that the pH value of 4% ammonia spirit conditioned reaction solution is 3.5 with mass fraction, temperature is controlled at 35 ℃, treat to stop after 1 hour reaction, leaving standstill, filter, spend deionised water is 10 ~ 20 little Siemens/cm to washing electrical conductivity of water, with the ethanol washing, oven dry adopts coating machine to coat at last again.The gained cuprum argentum composite powder is carried out performance test, and test result sees Table 1.
Embodiment 2
Get 20 gram AgNO
3Be dissolved in 800 ml distilled waters and be mixed with AgNO
3Solution; Get 10 gram AgNO
3With 114 gram Cu (NO
3)
23H
2O is dissolved in altogether in 400 ml distilled waters and is mixed with AgNO
3With Cu (NO
3)
23H
2The mixed aqueous solution of O, silver is 1:8 with the mol ratio of copper in the mixed solution; Get 120 the gram ascorbic acid and 10 the gram gelatin be dissolved in the mixed aqueous solution that is mixed with reducing agent and dispersant in 2000 ml distilled waters altogether.Under stirring with AgNO
3With Cu (NO
3)
23H
2The mixed aqueous solution of O be added to by mixing of forming of reducing agent and dispersant water-soluble in, the dropping time is 30 minutes, and be that the pH value of 4% ammonia spirit conditioned reaction solution is 5 with mass fraction, temperature is controlled at 80 ℃, reaction is after 3 hours under stirring, obtain containing the solution of the Kufil of reducing agent, with AgNO
3The aqueous solution be added in the solution of the Kufil that contains reducing agent, and be that the pH value of 4% ammonia spirit conditioned reaction solution is 6 with mass fraction, temperature remains on 50 ℃, treat to stop after 0.5 hour reaction, leaving standstill, filter, spend deionised water is 10 ~ 20 little Siemens/cm to washing electrical conductivity of water, with the ethanol washing, dry last ball-milling treatment again.The gained cuprum argentum composite powder is carried out performance test, and test result sees Table 1.
Embodiment 3
Get 20 gram AgNO
3Be dissolved in 100 ml distilled waters and be mixed with AgNO
3Solution; Get 10 gram AgNO
3With 142 gram Cu (NO
3)
23H
2O is dissolved in altogether in 800 ml distilled waters and is mixed with AgNO
3With Cu (NO
3)
23H
2The mixed aqueous solution of O, silver is 1:10 with the mol ratio of copper in the mixed solution; Get 150 gram mass marks and be 37% formalin and 20 gram polyvinylpyrrolidones and be dissolved in the mixed aqueous solution that is mixed with reducing agent and dispersant in 600 ml distilled waters altogether.Under stirring with AgNO
3With Cu (NO
3)
23H
2The mixed aqueous solution of O be added to by mixing of forming of reducing agent and dispersant water-soluble in, the dropping time is 40 minutes and is that the pH value of 4% sodium hydroxide solution conditioned reaction solution is 12 with mass fraction, temperature is controlled at 80 ℃, reaction is after 3 hours under stirring, obtain containing the solution of the Kufil of reducing agent, with AgNO
3The aqueous solution be added in the solution of the Kufil that contains reducing agent, and be that the pH value of 4% sodium hydroxide solution conditioned reaction solution is 10 with mass fraction, temperature remains on 30 ℃, treat to stop after 1 hour reaction, leaving standstill, filter, spend deionised water is 10 ~ 20 little Siemens/cm to washing electrical conductivity of water, with the ethanol washing, oven dry adopts coating machine to coat at last again.The gained cuprum argentum composite powder is carried out performance test, and test result sees Table 1.
Embodiment 4
Get 30 gram AgNO
3Be dissolved in 600 ml distilled waters and be mixed with AgNO
3Solution; Get 10 gram AgNO
3With 284 gram Cu (NO
3)
23H
2O is dissolved in altogether in 2000 ml distilled waters and is mixed with AgNO
3With Cu (NO
3)
23H
2The mixed aqueous solution of O, silver is 1:20 with the mol ratio of copper in the mixed solution; Get 300 gram ascorbic acid and 10 Arabic gums and be dissolved in the mixed aqueous solution that is mixed with reducing agent and dispersant in 900 ml distilled waters.Under stirring with AgNO
3With Cu (NO
3)
23H
2The mixed aqueous solution of O be added to by mixing of forming of reducing agent and dispersant water-soluble in, the dropping time is 20 minutes and is that the pH value of 4% ammonia spirit conditioned reaction solution is 3.5 with mass fraction, temperature is controlled at 70 ℃, reaction is after 2 hours under stirring, obtain containing the solution of the Kufil of reducing agent, with AgNO
3The aqueous solution be added in the solution of the Kufil that contains reducing agent, and be that the pH value of 4% ammonia spirit conditioned reaction solution is 5 with mass fraction, temperature is controlled at 30 ℃, treat to stop after 2 hours reaction, leaving standstill, filter, spend deionised water is 10 ~ 20 little Siemens/cm to washing electrical conductivity of water, with the ethanol washing, dry last ball-milling treatment again.The gained cuprum argentum composite powder is carried out performance test, and test result sees Table 1.
Comparative Examples 1
Get 40 gram AgNO
3Be dissolved in 400 ml distilled waters and be mixed with AgNO
3Solution; Get 57 gram Cu (NO
3)
23H
2O is dissolved in and is mixed with Cu (NO in 200 ml distilled waters
3)
23H
2O solution is got 80 gram ascorbic acid and 8 gram polyvinylpyrrolidones are dissolved in the mixed aqueous solution that is mixed with reducing agent and dispersant in 1 liter of distilled water altogether.Under stirring with Cu (NO
3)
23H
2The aqueous solution of O be added to by mixing of forming of reducing agent and dispersant water-soluble in, the dropping time is 20 minutes, and be that the pH value of 4% ammonia spirit conditioned reaction solution is 4.5 with mass fraction, temperature is controlled at 70 ℃, reaction is after 2 hours under stirring, obtain containing the solution of the copper microballoon of reducing agent, with AgNO
3The aqueous solution be added in the solution of the copper microballoon that contains reducing agent, and be that the pH value of 4% ammonia spirit conditioned reaction solution is 3.5 with mass fraction, temperature is controlled at 35 ℃, treat to stop after 1 hour reaction, leaving standstill, filter, spend deionised water is 10 ~ 20 little Siemens/cm to washing electrical conductivity of water, again with ethanol washing, oven dry at last.The gained cuprum argentum composite powder is carried out performance test, and test result sees Table 1.
Comparative Examples 2
Get 30 gram AgNO
3Be dissolved in 300 ml distilled waters and be mixed with AgNO
3Solution; Get 10 gram AgNO
3With 57 gram Cu (NO
3)
23H
2O is dissolved in altogether in 200 ml distilled waters and is mixed with AgNO
3With Cu (NO
3)
23H
2The mixed aqueous solution of O, silver is 1:4 with the mol ratio of copper in the mixed solution; Get 80 the gram ascorbic acid and 8 the gram polyvinylpyrrolidones be dissolved in the mixed aqueous solution that is mixed with reducing agent and dispersant in 1 liter of distilled water altogether.Under stirring with AgNO
3With Cu (NO
3)
23H
2The mixed aqueous solution of O be added to by mixing of forming of reducing agent and dispersant water-soluble in, the dropping time is 20 minutes, and be that the pH value of 4% ammonia spirit conditioned reaction solution is 4.5 with mass fraction, temperature is controlled at 70 ℃, reaction is after 2 hours under stirring, obtain containing the solution of the Kufil of reducing agent, with AgNO
3The aqueous solution be added in the solution of the Kufil that contains reducing agent, and be that the pH value of 4% ammonia spirit conditioned reaction solution is 3.5 with mass fraction, temperature is controlled at 35 ℃, treat to stop after 1 hour reaction, leaving standstill, filter, spend deionised water is 10 ~ 20 little Siemens/cm to washing electrical conductivity of water, with the ethanol washing, oven dry does not adopt surface densification to handle at last again.The gained cuprum argentum composite powder is carried out performance test, and test result sees Table 1.
By Fig. 2, Fig. 3 and Fig. 4 as can be known, when copper microsphere surface coated with silver, silver is on the copper surface intersperses the type structure, and covered effect is poor, and can see a large amount of tiny silver-colored particles by Fig. 3, and the spontaneous nucleation phenomenon of silver is more serious, and the coating efficiency of silver is reduced; Show that at Kufil the method that coats silver powder can suppress silver-colored spontaneous nucleation growth effectively and adopt, as shown in Figure 4, silver is more even at the cladding ratio on Kufil surface, and handles back (Fig. 2) particle surface even compact more through surperficial densification.
As shown in Table 1, the volume conductance of the cuprum argentum composite powder of the present invention's preparation is lower than the specific insulation of the powder of the method preparation of adopting copper surface contracted payment, and expose half a year in air after, resistivity also has no change basically.When the cuprum argentum composite powder of the present invention's preparation adopts the thermogravimetric analyzer test to be warmed up to 600 ℃, actual weightening finish is more much smaller than the weightening finish under the copper complete oxidation situation (theoretical weightening finish), high-temperature oxidation resistance is better, and powder copper when being warmed up to 600 ℃ of the method preparation of employing copper surface contracted payment is oxidized substantially fully.Increased the heap real density of powder after adopting surperficial densification to handle, and made that the silver layer that coats is fine and close more, improved and under the high temperature oxygen has been passed the obstruction ability on top layer, and then strengthened its high-temperature oxidation resistance.
Table 1
Claims (6)
1. the preparation method with cuprum argentum composite powder is characterized in that, this method may further comprise the steps:
(1) mixed aqueous solution of preparation reducing agent and dispersant, preparation AgNO
3With Cu (NO
3)
23H
2The mixed aqueous solution of O, wherein, AgNO
3Mass volume ratio concentration be 5 ~ 100 grams per liters, Cu (NO
3)
23H
2The mass volume ratio concentration of O is 50 ~ 400 grams per liters, and in the mixed nitrate solution silver and the mol ratio of copper between 1:3 ~ 20, under stirring with AgNO
3With Cu (NO
3)
23H
2The mixed aqueous solution of O is added in the mixed aqueous solution of being made up of reducing agent and dispersant, and with the pH value of ammonia spirit or sodium hydroxide solution conditioned reaction solution between 3 ~ 13, temperature is controlled at 15 ~ 90 ℃, under stirring, reacted 0.5 ~ 4 hour, obtain containing the solution of the Kufil of reducing agent, the consumption of described reducing agent requires to react excessive 0.2 ~ 2 times than equivalent, and the mass volume ratio concentration of dispersant is 2 ~ 100 grams per liters
(2) preparation mass volume ratio concentration is the AgNO of 20 ~ 300 grams per liters
3The aqueous solution, under stirring with AgNO
3The aqueous solution be added in the solution of the Kufil that contains reducing agent, and with the pH value of ammonia spirit or sodium hydroxide solution conditioned reaction solution between 3 ~ 13, temperature is controlled at 15 ~ 80 ℃, question response fully after, the cuprum argentum composite powder that leave standstill, filter, wash, dry, surperficial densification obtains 0.5 ~ 3 micron granularity after handling.
2. the preparation method of a kind of cuprum argentum composite powder according to claim 1 is characterized in that, described reducing agent is any one in ascorbic acid, formaldehyde, sodium hypophosphite, hydrazine hydrate, sodium borohydride, the potassium borohydride.
3. the preparation method of a kind of cuprum argentum composite powder according to claim 1, it is characterized in that, described dispersant be in polyvinylpyrrolidone, gelatin, softex kw, polyethylene glycol, polyvinyl alcohol, Arabic gum, the soluble starch any one or more than one.
4. the preparation method of a kind of cuprum argentum composite powder according to claim 1 is characterized in that, described surperficial densification is treated to ball milling or coating machine coats.
5. the preparation method of a kind of cuprum argentum composite powder according to claim 1 is characterized in that, described cuprum argentum composite powder is the cladded type nucleocapsid structure, and stratum nucleare is a Kufil, and shell is a silver.
6. the preparation method of a kind of cuprum argentum composite powder according to claim 1 is characterized in that, described cuprum argentum composite powder is spherical, silver content in wt% between 10 ~ 70%.
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| CN102560451A (en) * | 2012-02-22 | 2012-07-11 | 江苏大学 | Chemical nano-silver plating solution and preparation method thereof, and silver plating method for copper part |
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Application publication date: 20110824 |