CN106270544A - A kind of preparation method of the silver coprecipitated accumulated powder of palladium - Google Patents
A kind of preparation method of the silver coprecipitated accumulated powder of palladium Download PDFInfo
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- CN106270544A CN106270544A CN201510338347.1A CN201510338347A CN106270544A CN 106270544 A CN106270544 A CN 106270544A CN 201510338347 A CN201510338347 A CN 201510338347A CN 106270544 A CN106270544 A CN 106270544A
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- silver
- palladium
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- mixed solution
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Abstract
The invention discloses the preparation method of a kind of silver coprecipitated accumulated powder of palladium, comprise the following steps: silver nitrate, Palladous nitrate. are dissolved in deionized water by (1) by a certain percentage, be made into silver palladium mixed solution；(2) in silver palladium mixed solution, add a certain amount of macromolecule dispersing agent, and fully dissolve；(3) in silver palladium mixed solution, add pH adjusting agent, solution ph is adjusted between 9-10；(4) being joined by reductant solution in silver palladium mixed solution, the silver coprecipitated accumulated powder of palladium is produced in reduction；(5) washing dried.Reactions steps of the present invention is simple, is suitable for large-scale mass production；By the adjustment of concentration, reaction temperature, powder parameters can be carried out controlled adjustment；Silver-colored palladium codeposition powder body prepared by the present invention takes into account dispersibility, degree of crystallinity and tap density, can meet the application requirement of conductor paste silver palladium codeposition powder body.
Description
Technical field
The present invention relates to the preparation method of a kind of noble metal powder body material, the preparation method of a kind of silver coprecipitated accumulated powder of palladium.
Background technology
Electronic material is the material base of modern electronics industry and scientific technological advance, is primarily referred to as at electronic technology and microelectronics
The material used in technology, including dielectric material, semi-conducting material, piezoelectricity and ferroelectric material, conducting metal and alloy material thereof
Material, magnetic material, photoelectron material and other associated materials.Electronic material covering scope is extensive, and its major function is
The electric property of material itself.Currently, developing rapidly of the cofired materials technique such as MLCC, LTCC, necessarily drive and burn electricity altogether
The development of pole slurry, but more dielectric material, piezoelectric, ferroelectric material cannot simultaneously meet low-temperature sintering and excellent
Different properties of product two aspects, are therefore developed in order to current conductor paste is studied for high temperature co-firing electrode size
Focus.
As the silver-colored palladium slurry of one of conductor paste, obtain in industry because possessing the advantage such as high temperature sintering, price rather moderate
Extensive concern.The key technical index of silver palladium conductor paste is all by the performance of the silver-colored palladium powder body as conducting function phase certainly
Fixed, and the performance of silver palladium powder depends primarily on the forms such as its appearance structure feature, the granularity of powder art, tap density and distribution thereof
Feature.At present, the silver-colored palladium powder of domestic production, due to the defect at aspects such as preparation method, dispensing, technological parameters, causes shape
In the performances such as looks architectural feature, tap density, granularity not ideal enough.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of silver coprecipitated accumulated powder of palladium, to solve proposition in above-mentioned background technology
Problem.
For achieving the above object, the present invention provides following technical scheme:
The preparation method of a kind of silver coprecipitated accumulated powder of palladium, comprises the following steps:
(1) by a certain percentage silver nitrate, Palladous nitrate. are dissolved in deionized water, be made into silver palladium mixed solution；
(2) in silver palladium mixed solution, add a certain amount of macromolecule dispersing agent, and fully dissolve；
(3) in silver palladium mixed solution, add pH adjusting agent, solution ph is adjusted between 9-10；
(4) being joined by reductant solution in silver palladium mixed solution, the silver coprecipitated accumulated powder of palladium is produced in reduction；
(5) washing dried.
As the further scheme of the present invention: in the silver-colored palladium mixed solution prepared in step (1), silver ion is dense with palladium ion
Degree sum is 0.5-1mol/L, and reductant concentration is 0.5-1mol/L, reducing agent molal weight and precious metal salt molal weight ratio
Example is 1: 1.
As the present invention further scheme: in step (2), the quality of macromolecule dispersing agent is precious metal salt quality
10-50%.
As the present invention further scheme: described in step (4), reductant solution adds fashionable, described silver palladium mixing is molten
The temperature of liquid is 20-90 DEG C, and the feed postition of described reductant solution includes dropping mode and topples over mode.
As the present invention further scheme: the temperature of described silver palladium mixed solution is 20-70 DEG C.
As the present invention further scheme: step (5) guarantees by the way of detection supernatant water conductivity
Fully clean, the water conductivity≤50 μ S of the supernatant.
Compared with prior art, the invention has the beneficial effects as follows: reactions steps of the present invention is simple, be suitable for extensive batch
Produce；Additionally by the adjustment of concentration, reaction temperature, powder parameters can be carried out controlled adjustment；Silver-colored palladium prepared by the present invention
Codeposition powder body takes into account dispersibility, degree of crystallinity and tap density, and the application that can meet conductor paste silver palladium codeposition powder body is wanted
Ask.
Accompanying drawing explanation
Fig. 1 is the grain size distribution of the preparation method gained coprecipitated accumulated powder of silver palladium of the silver coprecipitated accumulated powder of palladium.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clearly and completely
Describe, it is clear that described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based on this
Embodiment in invention, the every other reality that those of ordinary skill in the art are obtained under not making creative work premise
Execute example, broadly fall into the scope of protection of the invention.
The preparation method of a kind of silver coprecipitated accumulated powder of palladium, comprises the following steps:
(1) by a certain percentage silver nitrate, Palladous nitrate. are dissolved in deionized water, be made into silver palladium mixed solution, described silver
In palladium mixed solution, silver ion and palladium ion concentration sum are 0.5-1mol/L, and reductant concentration is 0.5-1mol/L, reducing agent
Molal weight and precious metal salt molal weight ratio are 1: 1；
(2) adding a certain amount of macromolecule dispersing agent in silver palladium mixed solution, and fully dissolve, described macromolecule disperses
The quality of agent is the 10-50% of precious metal salt quality；
(3) in silver palladium mixed solution, add pH adjusting agent, solution ph is adjusted between 9-10；
(4) being joined by reductant solution in silver palladium mixed solution, the silver coprecipitated accumulated powder of palladium is produced in reduction, and described reducing agent is molten
Liquid adds fashionable, and the temperature of silver palladium mixed solution is 20-90 DEG C, and described reductant solution feed postition includes dropping mode and inclines
Mode.
(5) washing dried, guarantees fully to clean, the supernatant by the way of detection supernatant water conductivity
Water power lead and need to meet≤50 μ S.
Said method prepares the silver-colored palladium codeposition powder body of gained, and diameter of particle: D50 is 1-3 μm, tap density 2-4g/mL,
Specific surface area 1.5-4.0m2/g。
Embodiment 1:
Preparation containing 0.5mol silver nitrate, the precious metal solution 1L of 0.5mol Palladous nitrate. and contains 1mol vitamin C respectively
Reducing solution 1L, and in precious metal solution, add the gelatin of 50g, and fully dissolve, in precious metal solution, add hydrogen-oxygen
Change sodium, in the range of solution ph regulation to 9-10, afterwards precious metal solution be placed in water-bath and be heated to 50 DEG C, it
After reducing solution is added dropwise in preheated precious metal solution reaction, obtain the silver coprecipitated accumulated powder of palladium；Clean with deionized water
After precipitating 3-5 time, 60 DEG C of dry powder body, the particle diameter of the coprecipitated accumulated powder of gained silver palladium is distributed as it is shown in figure 1, D50 is 1.4 μm,
Good dispersion, narrow diameter distribution, specific surface area 2.5m2/ g, tap density 2g/mL.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, and do not carrying on the back
In the case of the spirit or essential attributes of the present invention, it is possible to realize the present invention in other specific forms.Therefore, no matter from
From the point of view of which point, all should regard embodiment as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all by fall in the implication of equivalency and scope of claim
Change is included in the present invention.Should not be considered as limiting involved claim by any reference in claim.
Although moreover, it will be appreciated that this specification is been described by according to embodiment, but the most each embodiment only comprises
One independent technical scheme, this narrating mode of description is only the most for clarity sake, and those skilled in the art should be by
Description is as an entirety, and the technical scheme in each embodiment can also be through appropriately combined, and forming those skilled in the art can
With other embodiments understood.
Claims (6)
1. the preparation method of the coprecipitated accumulated powder of silver-colored palladium, it is characterised in that comprise the following steps:
(1) by a certain percentage silver nitrate, Palladous nitrate. are dissolved in deionized water, be made into silver palladium mixed solution；
(2) in silver palladium mixed solution, add a certain amount of macromolecule dispersing agent, and fully dissolve；
(3) in silver palladium mixed solution, add pH adjusting agent, solution ph is adjusted between 9-10；
(4) being joined by reductant solution in silver palladium mixed solution, the silver coprecipitated accumulated powder of palladium is produced in reduction；
(5) washing dried.
The preparation method of the silver coprecipitated accumulated powder of palladium the most according to claim 1, it is characterised in that joined in step (1)
In the silver-colored palladium mixed solution of system, silver ion and palladium ion concentration sum are 0.5-1mol/L, and reductant concentration is 0.5-1mol/L,
Reducing agent molal weight and precious metal salt molal weight ratio are 1: 1.
The preparation method of the silver coprecipitated accumulated powder of palladium the most according to claim 1, it is characterised in that high score in step (2)
The quality of sub-dispersant is the 10-50% of precious metal salt quality.
The preparation method of the silver coprecipitated accumulated powder of palladium the most according to claim 1, it is characterised in that described in step (4)
Reductant solution adds fashionable, and the temperature of described silver palladium mixed solution is 20-90 DEG C, the feed postition bag of described reductant solution
Include dropping mode and topple over mode.
The preparation method of the silver coprecipitated accumulated powder of palladium the most according to claim 4, it is characterised in that described silver palladium mixing is molten
The temperature of liquid is 20-70 DEG C.
The preparation method of the silver coprecipitated accumulated powder of palladium the most according to claim 1, it is characterised in that step is passed through in (5)
The mode of detection supernatant water conductivity guarantees fully to clean, the water conductivity≤50 μ S of the supernatant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510338347.1A CN106270544A (en) | 2015-06-12 | 2015-06-12 | A kind of preparation method of the silver coprecipitated accumulated powder of palladium |
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| CN201510338347.1A CN106270544A (en) | 2015-06-12 | 2015-06-12 | A kind of preparation method of the silver coprecipitated accumulated powder of palladium |
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Cited By (3)
| 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 |
| CN114160804A (en) * | 2021-11-17 | 2022-03-11 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Preparation method of submicron monodisperse silver-palladium powder |
| CN115041698A (en) * | 2022-07-01 | 2022-09-13 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Preparation method of silver-palladium alloy powder |
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| US3788833A (en) * | 1972-02-18 | 1974-01-29 | Du Pont | Production of palladium-silver alloy powder |
| CN1104137A (en) * | 1994-08-31 | 1995-06-28 | 华东理工大学 | Super-fine globular silver-palladium alloy powder production method |
| CN102554264A (en) * | 2012-02-28 | 2012-07-11 | 东北大学 | Preparation method of palladium-silver alloy powder for conductive paste |
| CN103203458A (en) * | 2013-01-27 | 2013-07-17 | 贵研铂业股份有限公司 | Method for preparing monodisperse silver-palladium composite microsphere |
| CN104384526A (en) * | 2014-12-11 | 2015-03-04 | 成都明日星辰科技有限公司 | Preparation method for submicron monodisperse silver-palladium composite powder |
-
2015
- 2015-06-12 CN CN201510338347.1A patent/CN106270544A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3788833A (en) * | 1972-02-18 | 1974-01-29 | Du Pont | Production of palladium-silver alloy powder |
| CN1104137A (en) * | 1994-08-31 | 1995-06-28 | 华东理工大学 | Super-fine globular silver-palladium alloy powder production method |
| CN102554264A (en) * | 2012-02-28 | 2012-07-11 | 东北大学 | Preparation method of palladium-silver alloy powder for conductive paste |
| CN103203458A (en) * | 2013-01-27 | 2013-07-17 | 贵研铂业股份有限公司 | Method for preparing monodisperse silver-palladium composite microsphere |
| CN104384526A (en) * | 2014-12-11 | 2015-03-04 | 成都明日星辰科技有限公司 | Preparation method for submicron monodisperse silver-palladium composite powder |
Cited By (5)
| 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 |
| CN114160804A (en) * | 2021-11-17 | 2022-03-11 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Preparation method of submicron monodisperse silver-palladium powder |
| CN115041698A (en) * | 2022-07-01 | 2022-09-13 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Preparation method of silver-palladium alloy powder |
| CN115041698B (en) * | 2022-07-01 | 2023-10-13 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Preparation method of silver-palladium alloy powder |
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