CN105268985A - Method for preparing superfine silver-palladium duplex-metal alloy powder - Google Patents
Method for preparing superfine silver-palladium duplex-metal alloy powder Download PDFInfo
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- CN105268985A CN105268985A CN201410352615.0A CN201410352615A CN105268985A CN 105268985 A CN105268985 A CN 105268985A CN 201410352615 A CN201410352615 A CN 201410352615A CN 105268985 A CN105268985 A CN 105268985A
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Abstract
The invention discloses a method for preparing superfine silver-palladium duplex-metal alloy powder. The method comprises the steps that AgNO3, Pd(NO3)2.2H2O, a coordination agent and a dispersing agent are sequentially added into a beaker according to a certain proportion; stirring is conducted till all the components are completely dissolved; and then drying and high-temperature annealing treatment are conducted, so that the superfine silver-palladium duplex-metal alloy powder is obtained. Compared with the prior art, the method for preparing the superfine silver-palladium duplex-metal alloy powder has a series of advantages that the proportion of the chemical components is accurate, operation is easy, the reaction condition at the initial stage is mild, and toxic gas affecting the environment is avoided in the experimental process; it is hopeful to apply the prepared superfine silver-palladium duplex-metal alloy powder to the fields such as electronic paste and fuel cells.
Description
Technical field
The present invention relates to a kind of noble metal composite powder material, be specifically related to a kind of preparation method of ultra-fine silver palladium bimetallic alloy powder.
Background technology
As everyone knows, metal and alloy material thereof have many important application.Silver palladium bimetallic alloy powder is widely used in electronics industry, and such as can make microplate type electronic devices and components, make complicated joint line volume less, capacity is larger.Silver and the alloy of palladium are also widely used in the current-carrying part of hybrid integrated circuit because the cost ratio gold of this alloy is cheap, can with most of electric insulation and resistance system compatible, and go for the connection of hyperacoustic wire.Because metal A g has high conductivity, the features such as anti-oxidant high stability and serviceability are excellent are that consumption is large in the electronics industry, scope is wide for the electric slurry of metallic conduction phase with Ag.But there is a series of shortcomings such as silver ion easily moves in the electric slurry being conductive phase with pure Ag, therefore causes adverse effect to electronic reliability.Metal Pd can form with Ag the body that infinitely dissolves each other, thus improves the resistance to scolding tin erosiveness of Ag.
The method preparing silver palladium bimetallic alloy material reported comprises mechanical mixing, electrochemical deposition method and chemical liquid phase reducing process etc.Mechanical attrition method prepares silver palladium alloy powder length consuming time, and mixes uneven; Silver-colored palladium bimetallic alloy powder prepared by electrodeposition process neither be very even, and cost is higher.Therefore the technical way preparing silver-colored palladium bimetallic alloy powder is chemical liquid phase reducing process, but the influence factor of chemical liquid phase reducing process is more complicated, the type of the such as acid-base value of reaction temperature, solution, the kind of reducing agent and consumption, dispersant and concentration.Therefore chemical liquid phase reducing process still has sizable difficulty in preparation silver-colored palladium bimetallic alloy powder time control powder morphology, Size Distribution and chemical constituent uniformity.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of ultra-fine silver palladium bimetallic alloy powder, prepared silver palladium alloy powder is spherical, and grain size is 10-25nm, is uniformly dispersed.
Technical scheme of the present invention is as follows:
A preparation method for ultra-fine silver palladium bimetallic alloy powder, comprises the following steps:
1. nitrate is joined in solvent, under magnetic agitation, add complexant and dispersant successively, after complexant and dispersant dissolve completely, mixed solution is placed in water-bath ageing;
2. above-mentioned mixed solution is placed in drying box dry, until the complete evaporate to dryness of moisture becomes xerogel;
3. xerogel is placed in the tube furnace being connected with protection gas and carries out the high temperature anneal.
Solvent described in step 1 is absolute ethyl alcohol or water; Described complexant is lactic acid; Dispersant is any one in oleic acid (OA) or polyvinylpyrrolidone (K-30); Nitrate molar concentration is 0.006-0.024mol/L; Nitrate is AgNO
3with Pd (NO
3)
22H
2o.
Above-mentioned Ag
+with Pd
2+mol ratio be 5:1; Ag
+be 1:3-1:6 with the mol ratio of complexant; Ag
+be 1:2-1:4 with the mol ratio of dispersant.
Baking temperature described in step 2 is 70-200 DEG C, and drying time is 24 hours.
High temperature anneal temperature described in step 3 is 300-600 DEG C, and annealing time is 4 hours, and the heating rate of tube furnace is 15-20 DEG C/min.
Compared with prior art, the invention has the advantages that;
1. present invention process is simple, and overcome large, high to equipment requirement, the heavy-polluted shortcoming of existing synthetic technology energy consumption, without the need to adding reducing agent in reaction, initial reaction mild condition, does not occur in experimentation the influential toxic gas of environment.Therefore there is good applicability.
2. the ultra-fine silver palladium bimetallic alloy powder good dispersion in aqueous prepared of the present invention, grain size is 10-25nm, and stability is high.
Accompanying drawing explanation
Fig. 1 is the TEM figure of ultra-fine silver palladium bimetallic alloy powder in the embodiment of the present invention 1.
Fig. 2 is the XRD figure of ultra-fine silver palladium bimetallic alloy powder in the embodiment of the present invention 1.
Fig. 3 is the SAED figure of ultra-fine silver palladium bimetallic alloy powder in the embodiment of the present invention 1.
Fig. 4 is the XRD figure of ultra-fine silver palladium bimetallic alloy powder in the embodiment of the present invention 2.
Fig. 5 is the XRD figure of ultra-fine silver palladium bimetallic alloy powder in the embodiment of the present invention 3.
Detailed description of the invention
Below in conjunction with example and accompanying drawing, the present invention is described in detail.
Embodiment 1: first take 0.3404gAgNO
3with 0.1076gPd (NO
3)
22H
2o is dissolved in 0.1L absolute ethyl alcohol, opens and stirs, make its abundant mixed dissolution, and then in solution, add 0.546g lactic acid and 1.1894g oleic acid (OA), continues to stir 10min.Mixed solution is placed in dry 24 hours of the drying box of 70 DEG C; obtain loose porous xerogel, be then put in by xerogel in the tube furnace being connected with protection gas and carry out the high temperature anneal, the heating rate controlling tube furnace is 15 DEG C/min; annealing temperature is 500 DEG C, and the time is 4 hours.After high annealing terminates, close tube furnace, after the temperature of tube furnace reduces to room temperature, black product is taken out.Fig. 1 is the TEM figure of sample, and as can be seen from the figure obtained ultra-fine silver palladium bimetallic alloy is the spheric granules of 10-25nm, is uniformly dispersed.Fig. 2 is the XRD figure of sample, can find out that four obvious diffraction maximums have appearred in the angle of diffraction in the scope of 30-80 °, analyze (111), (200), (220) and (311) crystal face of these four corresponding silver palladium alloies of diffraction maximums difference known.Fig. 3 is the SAED figure of sample, analyzes and shows that product is the silver palladium alloy superfines of face-centered cubic phase.
Embodiment 2: first take 0.1702gAgNO
3with 0.0538gPd (NO
3)
22H
2o is dissolved in 0.1L deionized water, opens and stirs, make its abundant mixed dissolution, and then in solution, add 0.455g lactic acid and 0.333g polyvinylpyrrolidone (K-30), continues to stir 10min.Mixed solution is placed in dry 24 hours of the drying box of 150 DEG C; obtain loose porous xerogel, be then put in by xerogel in the tube furnace being connected with protection gas and carry out the high temperature anneal, the heating rate controlling tube furnace is 17 DEG C/min; annealing temperature is 300 DEG C, and the time is 4 hours.After high annealing terminates, close tube furnace, after the temperature of tube furnace reduces to room temperature, black product is taken out.Fig. 4 is the XRD figure of sample, and the known product of same analysis is the silver-colored palladium bimetallic alloy powder of face-centered cubic phase.
Embodiment 3: first take 0.0851gAgNO
3with 0.0269gPd (NO
3)
22H
2o is dissolved in 0.1L deionized water, opens and stirs, make its abundant mixed dissolution, and then in solution, add 0.273g lactic acid and 0.222g polyvinylpyrrolidone (K-30), continues to stir 10min.Mixed solution is placed in dry 24 hours of the drying box of 200 DEG C; obtain loose porous xerogel, be then put in by xerogel in the tube furnace being connected with protection gas and carry out the high temperature anneal, the heating rate controlling tube furnace is 20 DEG C/min; annealing temperature is 600 DEG C, and the time is 4 hours.After high annealing terminates, close tube furnace, after the temperature of tube furnace reduces to room temperature, black product is taken out.Fig. 5 is the XRD figure of sample, and the known product of same analysis is the silver-colored palladium bimetallic alloy powder of face-centered cubic phase.
Claims (5)
1. a preparation method for ultra-fine silver palladium bimetallic alloy powder, is characterized in that, comprise the following steps:
Nitrate joins in solvent by step 1., adds complexant and dispersant successively under magnetic agitation, after complexant and dispersant dissolve completely, mixed solution is placed in water-bath ageing;
It is dry that above-mentioned mixed solution is placed in drying box by step 2., until the complete evaporate to dryness of moisture becomes xerogel;
Xerogel is placed in the tube furnace being connected with protection gas by step 3. carries out the high temperature anneal.
2. the preparation method of ultra-fine silver palladium bimetallic alloy powder according to claim 1, it is characterized in that, the solvent described in step 1 is absolute ethyl alcohol or water; Described complexant is lactic acid; Dispersant is any one in oleic acid or polyvinylpyrrolidone; Nitrate molar concentration is 0.006-0.024mol/L; Nitrate is AgNO
3with Pd (NO
3)
22H
2o.
3. the preparation method of ultra-fine silver palladium bimetallic alloy powder according to claim 2, is characterized in that, the Ag in nitrate
+with Pd
2+mol ratio be 5:1; Ag
+be 1:3-1:6 with the mol ratio of complexant; Ag
+be 1:2-1:4 with the mol ratio of dispersant.
4. the preparation method of ultra-fine silver palladium bimetallic alloy powder according to claim 1, it is characterized in that, the baking temperature described in step 2 is 70-200 DEG C, and drying time is 24 hours.
5. the preparation method of ultra-fine silver palladium bimetallic alloy powder according to claim 1, it is characterized in that, the high temperature anneal temperature described in step 3 is 300-600 DEG C, and annealing time is 4 hours, and the heating rate of tube furnace is 15-20 DEG C/min.
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|---|---|---|---|
| CN201410352615.0A CN105268985A (en) | 2014-07-23 | 2014-07-23 | Method for preparing superfine silver-palladium duplex-metal alloy powder |
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|---|---|---|---|
| CN201410352615.0A CN105268985A (en) | 2014-07-23 | 2014-07-23 | Method for preparing superfine silver-palladium duplex-metal alloy powder |
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|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111893526A (en) * | 2020-08-06 | 2020-11-06 | 中国科学技术大学 | Nano-silver alloy modified substrate and preparation method and application thereof |
-
2014
- 2014-07-23 CN CN201410352615.0A patent/CN105268985A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111893526A (en) * | 2020-08-06 | 2020-11-06 | 中国科学技术大学 | Nano-silver alloy modified substrate and preparation method and application thereof |
| CN111893526B (en) * | 2020-08-06 | 2022-05-13 | 中国科学技术大学 | Nano-silver alloy modified substrate and preparation method and application thereof |
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Application publication date: 20160127 |
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