CN115722677A - Preparation method of high-dispersity submicron spherical palladium powder - Google Patents
Preparation method of high-dispersity submicron spherical palladium powder Download PDFInfo
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- CN115722677A CN115722677A CN202211567554.0A CN202211567554A CN115722677A CN 115722677 A CN115722677 A CN 115722677A CN 202211567554 A CN202211567554 A CN 202211567554A CN 115722677 A CN115722677 A CN 115722677A
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Abstract
The invention discloses a preparation method of high-dispersibility submicron spherical palladium powder, which comprises the steps of weighing palladium nitrate solid, dissolving the palladium nitrate solid in dilute nitric acid to prepare a palladium nitrate dilute solution, dissolving a reducing agent in deionized water to obtain a reducing solution, weighing a dispersing agent and an additive respectively, dissolving the dispersing agent and the additive in deionized water to obtain a mixed base solution, mixing the three solutions to obtain reaction slurry containing palladium powder, and finally filtering, washing and drying to obtain submicron spherical palladium powder particles. The method adopts a liquid phase reduction method, uses ascorbic acid or hydrazine hydrate as a reducing agent to reduce a palladium nitrate solution to prepare submicron spherical palladium powder, and well controls the particle growth process and the dispersibility by a symmetrical feeding mode and simultaneously adding an organic polymer dispersant and a micromolecular alcohol additive into a base solution on the premise of ensuring the yield of the palladium powder, and the prepared palladium powder particles are spherical and highly dispersed, and have the particle size of 100-600 nm.
Description
Technical Field
The invention belongs to the technical field of precious metal powder material preparation, and particularly relates to a preparation method of high-dispersity submicron spherical palladium powder.
Background
With the vigorous development of the electronic information industry, microelectronic components tend to be integrated, low in cost and high in efficiency, and thick film conductive paste gradually shows unique advantages. The palladium powder is not only a good catalytic material and a hydrogen storage material, but also one of the indispensable important materials in the thick film conductive paste. The palladium powder is used as an additive phase in the thick film conductive paste, can inhibit the migration of silver ions in a high-temperature high-humidity electric field of the conductive film, and can also play a role in improving the anti-corrosion capability of the paste. The properties of palladium powder directly affect the performance of the slurry, which makes the requirements on the quality of palladium powder in industrial production increasingly strict.
However, the electronic paste industry in China is starting late, compared with the research of foreign electronic paste, the technical performance and reliability of the paste in China are lower, core key materials such as silver powder and palladium powder depend on import, and the production technical means of raw materials is laggard. In only a few reports on palladium powder preparation technology, the prepared palladium powder is extremely easy to agglomerate (see CN202210979544.1 a preparation method of high-crystallinity and high-sphericity palladium powder with strong oxidation resistance, CN201710450372.8 high-specific surface area ultrafine palladium powder and a preparation method thereof), and the yield is difficult to guarantee. Therefore, how to improve the powder dispersibility and realize the controllable preparation of the palladium powder particle size on the premise of ensuring the high yield of the palladium powder is a problem which needs to be solved at present.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing high-dispersibility submicron-sized spherical palladium powder, which ensures the correctness and high efficiency of the marine electrical connector in the wiring process.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of high-dispersity submicron spherical palladium powder comprises the following steps:
(1) Weighing palladium nitrate solid, dissolving the palladium nitrate solid in dilute nitric acid, and fully mixing to prepare a palladium nitrate dilute solution;
(2) Dissolving a reducing agent in deionized water, and fully mixing to prepare a reducing solution, wherein the reducing agent is ascorbic acid or hydrazine hydrate;
(3) Respectively weighing 0.05-0.5 g of dispersant and 0.05-0.5 g of additive, and respectively dissolving the dispersant and the additive in a small amount of deionized water to obtain a dispersant solution and an additive solution, wherein the dispersant is one or more of polyvinylpyrrolidone, polyethylene glycol and tween 80, and the additive is one or more of methanol, ethanol and n-propanol; then mixing the dispersant solution and the additive solution, and uniformly stirring to obtain 30-300 g of mixed base solution;
(4) Pumping the mixed base solution obtained in the step (3) into a reaction kettle, rapidly adding a dilute palladium nitrate solution and a reducing solution into the mixed base solution simultaneously under the condition of stirring, continuously reacting for 20-30 min, and obtaining reaction slurry containing palladium powder after the reaction is finished;
(5) Standing and aging the reaction slurry for 30min, filtering, washing with deionized water for multiple times until the conductivity is less than 10us/cm, placing the obtained solid in a vacuum drying oven, and drying at 70 ℃ for 12h to obtain spherical palladium powder particles with the particle size of 100-600 nm, wherein the yield of the palladium powder is 99.3-99.8%, the obtained palladium powder has high yield, and the particles are spherical and highly dispersed.
In the preparation method of the high-dispersity submicron spherical palladium powder, the mass concentration of the dilute palladium nitrate solution in the step (1) is 1-10% calculated by simple substance palladium.
Further, the dilute palladium nitrate solution in the step (1) is obtained by adding 10g of palladium nitrate to 40 to 460g of dilute nitric acid having a concentration of 1% by weight and mixing them thoroughly.
The preparation method of the high-dispersibility submicron spherical palladium powder comprises the following steps that in the step (2), the molar weight ratio of the reducing agent to the palladium nitrate is 2.5.
Further, the reducing solution in the step (2) is obtained by dissolving 10.8-30 g of ascorbic acid or hydrazine hydrate in 40-400 g of deionized water.
The preparation method of the high-dispersity submicron spherical palladium powder comprises the following steps that in the step (3), the using amount of a dispersing agent accounts for 1-10% of the mass of palladium; the dosage of the additive is 1 to 10 percent of the mass of the palladium.
The preparation method of the high-dispersibility submicron spherical palladium powder comprises the step (4) of controlling the reaction temperature to be 20-70 ℃, controlling the feeding time of the palladium nitrate dilute solution and the reducing solution to be 30-60 s, and controlling the stirring speed to be 400-600 r/min in the reaction process.
The beneficial effects of the invention are:
1, the invention carries out dispersion treatment on the palladium powder generated in the reaction process by adding organic polymer and micromolecular alcohol, so that the prepared palladium powder has higher dispersibility.
2, in the preparation process, the palladium nitrate is fully reduced into palladium powder by controlling the reaction temperature, the concentration of the reducing agent and ensuring the reaction time, so that the yield of the palladium powder is not less than 99 percent, the loss is reduced and the cost is reduced.
3, the invention adopts a feeding mode that an oxidant and a reducing agent are simultaneously added into the base solution, and on the basis, the internal processes of nucleation and growth of the palladium powder are effectively regulated and controlled by controlling the reaction temperature, the reactant concentration, the dispersant and the additive concentration, so that the prepared palladium powder has high particle sphericity and submicron particle size.
Drawings
FIG. 1 is a scanning electron micrograph of submicron spherical palladium powder according to example 1 of the present invention;
FIG. 2 is a scanning electron micrograph of submicron spherical palladium powder in accordance with example 2 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, but the protection scope of the present invention is not limited by these embodiments.
Example 1
The method for preparing the high-dispersity submicron spherical palladium powder comprises the following steps:
(1) 10g of palladium nitrate solid is weighed, 460g of dilute nitric acid with the concentration of 1 percent by weight is added for dissolution, and the palladium nitrate dilute solution is prepared for standby after full mixing, wherein the mass concentration of palladium in the solution is 1 percent.
(2) Weighing 20g of ascorbic acid according to the molar weight ratio of the reducing agent to the palladium nitrate of 2.5.
(3) Weighing 0.25g of polyvinylpyrrolidone, dissolving in a small amount of deionized water to obtain a dispersant solution, weighing 0.25g of methanol, dissolving in a small amount of deionized water to obtain an additive solution, mixing the dispersant solution and the additive solution, stirring uniformly, and supplementing deionized water to obtain 300g of mixed base solution. In this example, the dispersant used was polyvinylpyrrolidone, the additive was methanol, and the amounts of dispersant and additive were all 5% by mass of palladium.
(4) Pumping the mixed base solution into a reaction kettle, heating and stirring, rapidly adding a palladium nitrate dilute solution and a reducing solution into the mixed base solution at the rotation speed of 500r/min and at the temperature of 70 ℃, and continuously reacting for 20min after the addition is finished. And obtaining reaction slurry containing palladium powder after the reaction is finished. In this example, the feeding time of the dilute palladium nitrate solution and the reducing solution was 60 seconds.
(5) Standing and aging the reaction slurry for 30min, filtering, repeatedly washing with deionized water for multiple times until the conductivity is 8us/cm, placing the obtained solid in a vacuum drying oven, and vacuum drying at 70 ℃ for 12h to obtain palladium powder particles.
The yield of the palladium powder prepared by the preparation method of the embodiment is 99.5%, the obtained palladium powder has good dispersibility, the particles are spherical, and the particle size is 200-400 nm. The scanning electron micrograph of the prepared palladium powder is shown in figure 1.
Example 2
The method for preparing the high-dispersity submicron spherical palladium powder comprises the following steps:
(1) Weighing 10g of palladium nitrate solid, adding 160g of dilute nitric acid with the concentration of 1 percent by weight for dissolving, and fully mixing to prepare a dilute palladium nitrate solution for later use, wherein the mass concentration of palladium in the solution is 3 percent.
(2) Weighing 30g of ascorbic acid to dissolve in 140g of deionized water according to the molar weight ratio of the reducing agent to the palladium nitrate of 4:1, and fully mixing to prepare a reducing solution for later use.
(3) Weighing 0.5g of tween 80, dissolving in a small amount of deionized water to obtain a dispersant solution, weighing 0.5g of n-propanol, dissolving in a small amount of deionized water to obtain an additive solution, mixing the dispersant solution and the additive solution, stirring uniformly, and supplementing deionized water to obtain 200g of mixed base solution. In this example, tween 80 was used as the dispersant, n-propanol was used as the additive, and the amounts of the dispersant and the additive were 10% by mass of palladium.
(4) Pumping the mixed base solution into a reaction kettle, heating and stirring, quickly adding a palladium nitrate dilute solution and a reducing solution into the mixed base solution at the rotation speed of 600r/min and the temperature of 50 ℃, and continuously reacting for 30min after the addition is finished. And obtaining reaction slurry containing palladium powder after the reaction is finished. In this example, the feeding time of the dilute palladium nitrate solution and the reducing solution was 30 seconds.
(5) And standing and aging the reaction slurry for 30min, filtering, repeatedly washing with deionized water for many times until the conductivity is 9us/cm, placing the obtained solid in a vacuum drying oven, and performing vacuum drying at 70 ℃ for 12h to obtain palladium powder particles.
The yield of the palladium powder prepared by the preparation method of the embodiment is 99.3%, the obtained palladium powder has good dispersibility, the particles are spherical, and the particle size is 300-600 nm. The scanning electron micrograph of the prepared palladium powder is shown in figure 2.
Example 3
The method for preparing the high-dispersity submicron spherical palladium powder comprises the following steps:
(1) Weighing 10g of palladium nitrate solid, adding 40g of dilute nitric acid with the concentration of 1 percent by weight, dissolving, and fully mixing to prepare a palladium nitrate dilute solution for later use, wherein the mass concentration of palladium in the solution is 10 percent.
(2) According to the molar weight ratio of the reducing agent to the palladium nitrate of 5:1, 10.8g of hydrazine hydrate is weighed and dissolved in 40g of deionized water, and the hydrazine hydrate and the deionized water are fully mixed to prepare reducing liquid for later use.
(3) Weighing 0.05g of polyethylene glycol, dissolving in a small amount of deionized water to obtain a dispersant solution, weighing 0.05g of ethanol, dissolving in a small amount of deionized water to obtain an additive solution, mixing the dispersant solution and the additive solution, stirring uniformly, and supplementing deionized water to obtain 30g of mixed base solution. In this example, the dispersant used was polyethylene glycol, the additive was ethanol, and the amounts of dispersant and additive were all 1% of the mass of palladium.
(4) Pumping the mixed base solution into a reaction kettle, heating and stirring, quickly adding a palladium nitrate dilute solution and a reducing solution into the mixed base solution at the rotation speed of 400r/min and the temperature of 20 ℃, and continuously reacting for 30min after the addition is finished. And obtaining reaction slurry containing palladium powder after the reaction is finished. In this example, the time for feeding the dilute palladium nitrate solution and the reducing solution was 30 seconds.
(5) Standing and aging the reaction slurry for 30min, filtering, repeatedly washing with deionized water for multiple times until the conductivity is 8us/cm, placing the obtained solid in a vacuum drying oven, and vacuum drying at 70 ℃ for 12h to obtain palladium powder particles.
The yield of the palladium powder prepared by the preparation method of the embodiment is 99.8%, the obtained palladium powder has good dispersibility, the particles are spherical, and the particle size is 100-200 nm.
Other advantages and effects of the present invention will be apparent to those skilled in the art from the description of the present specification. Various details of the present description may also be modified or changed in various respects, all without departing from the spirit of the present invention.
Claims (7)
1. A preparation method of high-dispersity submicron spherical palladium powder is characterized by comprising the following steps: comprises the following steps
(1) Weighing palladium nitrate solid, dissolving the palladium nitrate solid in dilute nitric acid, and fully mixing to prepare a dilute palladium nitrate solution;
(2) Dissolving a reducing agent in deionized water, and fully mixing to prepare a reducing solution, wherein the reducing agent is ascorbic acid or hydrazine hydrate;
(3) Respectively weighing a dispersing agent and an additive, respectively dissolving the dispersing agent and the additive in deionized water to obtain a dispersing agent solution and an additive solution, wherein the dispersing agent is one of polyvinylpyrrolidone, polyethylene glycol and tween 80, and the additive is one of methanol, ethanol and n-propanol; mixing the dispersant solution and the additive solution, and uniformly stirring to obtain a mixed base solution;
(4) Pumping the mixed base solution into a reaction kettle, rapidly adding a dilute palladium nitrate solution and a reducing solution into the mixed base solution simultaneously under the stirring condition, continuously reacting for 20-30 min, and obtaining reaction slurry containing palladium powder after the reaction is finished;
(5) And standing and aging the reaction slurry for 30min, filtering, washing with deionized water for multiple times until the conductivity is less than 10us/cm, placing the obtained solid in a vacuum drying oven, and drying at 70 ℃ for 12h to obtain spherical palladium powder particles with the particle size of 100-600 nm.
2. The method for preparing highly dispersible submicron spherical palladium powder according to claim 1, wherein the mass concentration of the dilute palladium nitrate solution in step (1) is 1-10% calculated by the elemental palladium.
3. The method for preparing a highly dispersible submicron-sized spherical palladium powder according to claim 2, characterized in that the dilute solution of palladium nitrate in step (1) is obtained by adding 10g of palladium nitrate to 40-460 g of dilute nitric acid having a concentration of 1% by weight and thoroughly mixing.
4. The method for preparing highly dispersible submicron spherical palladium powder according to claim 1, wherein the molar ratio of the reducing agent to the palladium nitrate in step (2) is 2.5.
5. The method for preparing high-dispersibility submicron-sized spherical palladium powder according to claim 4, wherein the reducing solution obtained in step (2) is prepared by dissolving 10.8-30 g of ascorbic acid or hydrazine hydrate in 40-400 g of deionized water.
6. The method for preparing high-dispersibility submicron-sized spherical palladium powder according to claim 1, wherein the amount of the dispersant in the step (3) is 1-10% of the mass of palladium; the dosage of the additive is 1-10% of the mass of the palladium.
7. The method for preparing high-dispersibility submicron-sized spherical palladium powder according to claim 1, wherein the reaction temperature in the step (4) is 20-70 ℃, the feeding time of the dilute palladium nitrate solution and the reducing solution is 30-60 s, and the stirring speed in the reaction process is 400-600 r/min.
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