CN114160804A - Preparation method of submicron monodisperse silver-palladium powder - Google Patents
Preparation method of submicron monodisperse silver-palladium powder Download PDFInfo
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- CN114160804A CN114160804A CN202111361808.9A CN202111361808A CN114160804A CN 114160804 A CN114160804 A CN 114160804A CN 202111361808 A CN202111361808 A CN 202111361808A CN 114160804 A CN114160804 A CN 114160804A
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- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical compound [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000000843 powder Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 56
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 31
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 26
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052709 silver Inorganic materials 0.000 claims abstract description 18
- 239000004332 silver Substances 0.000 claims abstract description 18
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 16
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 14
- 238000001291 vacuum drying Methods 0.000 claims abstract description 9
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 7
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 7
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 5
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000032683 aging Effects 0.000 claims abstract description 3
- 239000012066 reaction slurry Substances 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 229910001252 Pd alloy Inorganic materials 0.000 claims description 16
- 239000007800 oxidant agent Substances 0.000 claims description 14
- 230000001590 oxidative effect Effects 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 48
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 4
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- 239000003223 protective agent Substances 0.000 abstract description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- -1 silver-palladium ions Chemical class 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 11
- 239000002002 slurry Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000003321 amplification Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011267 electrode slurry Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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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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- General Chemical & Material Sciences (AREA)
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Abstract
The invention discloses a preparation method of submicron monodisperse silver-palladium powder, which comprises the steps of taking silver nitrate as a silver source, a palladium nitrate aqueous solution as a palladium source, taking ascorbic acid or hydrazine hydrate as a reducing agent, adjusting the pH value of an excessive reducing agent solution to 9.01-10.0 under the condition of not using any protective agent, quickly adding the reducing agent solution into a mixed solution containing silver-palladium ions, reacting for 40 min-2 h at 20-80 ℃, aging, separating, vacuum drying and the like to obtain the silver-palladium powder with the average particle size of 380-700 nm. The method has the characteristics of simple preparation method, easy separation and cleaning, less equipment investment and contribution to industrial mass production, and the prepared silver-palladium powder has good dispersibility, spherical shape, high yield and high purity.
Description
Technical Field
The invention belongs to the technical field of preparation of noble metal powder materials, and particularly relates to a preparation method of submicron monodisperse silver-palladium powder for conductive paste.
Background
The silver palladium slurry has the advantages of excellent conductivity, silver ion migration resistance, solderability resistance, reliability and the like, and is widely applied to the manufacturing process of low temperature co-fired ceramic (LTCC) and multilayer ceramic capacitor (MLCC) as a conductor electrode slurry and a solderable slurry. The silver palladium powder is a conductive filler of the silver palladium slurry, and can be divided into mixed powder, co-precipitated starch and alloy powder according to a mixing mode of silver and palladium. The silver and palladium in the silver-palladium alloy powder are dispersed at an atomic level, so that the silver-palladium slurry prepared by using the silver-palladium alloy powder as a conductive phase has the best use effect.
The properties of the silver-palladium powder, such as alloying degree, morphology of particles, particle size distribution, tap density and the like, have important influence on the performance of the subsequently prepared silver-palladium slurry.
The chemical liquid phase reduction method is adopted for more domestic researches due to the reasons of mild reaction conditions, simple equipment and the like. The influence factors in the synthesis process are complex, including reaction temperature, reaction time, reaction material concentration, pH value of reaction solution, type of reducing agent, dosage of reducing agent, type and dosage of dispersing agent, stirring speed, drying temperature and the like, and all have important influence on the properties of finally formed silver-palladium alloy powder.
For example, CN201410352615 discloses a preparation method of ultrafine silver-palladium bimetallic alloy powder, and the particle size of the obtained silver-palladium powder is 10-25 nm. The nanometer single particle has poor dispersibility, the filtration and the separation are difficult in the preparation process, and the silver-palladium colloid exists in the filtrate, which affects the product yield and is not beneficial to the amplification production.
Patent CN201210030312.4 discloses a preparation method of submicron monodisperse silver palladium composite microspheres, which performs reduction reaction under alkaline condition, and the dispersibility of the obtained silver palladium microspheres is still poor under the condition of using dispersant.
Disclosure of Invention
The invention mainly aims to provide a preparation method of submicron monodisperse spherical silver-palladium alloy powder, wherein the mass ratio of silver to palladium can be regulated and controlled according to needs, and the particle size distribution and the average particle size can be controlled within the range of 300-900 nm according to reaction conditions.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of submicron monodisperse silver-palladium powder comprises the following steps
(1) According to the mass ratio of silver to palladium of 7-9: weighing 5.51-6.70 g of analytically pure silver nitrate and 7.10-16.04 g of palladium nitrate aqueous solution containing 9.35% of palladium in 3-1 g, and adding deionized water to prepare 93-232 mL of oxidant solution with the metal ion molar concentration of 0.2-0.6 mol/L;
(2) weighing 24.62-65.50 g of ascorbic acid or hydrazine hydrate as a reducing agent according to the molar weight which is 3-8 times of the sum of silver nitrate and palladium nitrate, dissolving with 63-232 mL of deionized water to ensure that the volume of the reducing agent solution is the same as that of the oxidant solution, and then adding ammonia water or dilute nitric acid solution with the mass concentration of 28% to adjust the pH value of the reducing agent solution to 9.01-10.0;
(3) quickly adding the reducing agent solution prepared in the step (2) into the oxidant solution prepared in the step (1) at the temperature of 20-80 ℃, quickly stirring for 40 min-2 h, and aging for 0.5h at room temperature after the reaction is finished;
(4) and (4) filtering the reaction slurry obtained in the step (3), washing with deionized water and ethanol twice respectively, placing the obtained solid in a vacuum drying oven, and drying for 3-8 hours under the conditions of-0.1 MPa and 30-50 ℃ to obtain 4.93-4.96 g of black silver-palladium alloy powder with the average particle size of 380-700 nm.
In the preparation method of the submicron monodisperse silver-palladium powder, the molar weight ratio of the reducing agent to the silver-palladium nitrate in the step (2) is preferably 4: 1-6: 1.
Compared with the prior art, the invention has the following beneficial effects:
the preparation process of the invention does not need to add any organic protective agent, and can improve the purity of the product while reducing the production cost.
2, the silver palladium powder prepared by the method has good dispersibility and spherical shape, can realize the regulation and control of the particle size between 200 and 900nm by adjusting the conditions of the pH value of the reducing agent, the concentration of the reducing agent, the reaction temperature, the concentration of the oxidizing agent and the like, is easy to carry out suction filtration separation or centrifugal separation, has excessive reducing agent, complete reaction and high product yield.
3, the preparation process has short flow, simple required reaction equipment and easy amplification and mass production.
Drawings
FIG. 1 is a silver palladium powder prepared according to example 1;
FIG. 2 is a silver palladium powder prepared according to example 3;
fig. 3 is a silver palladium powder prepared according to example 4.
Detailed Description
The present invention is further illustrated by the following specific examples, but the scope of the present invention is not limited by these examples.
Example 1
(1) According to the mass ratio of silver to palladium of 7: 3, weighing 5.51g of silver nitrate (analytically pure) and 16.04g of palladium nitrate solution (containing 9.35 percent of palladium) respectively, and adding a proper amount of deionized water to prepare a solution with the total molar concentration of silver and palladium being 0.4mol/L, wherein the volume of the obtained solution is 116 mL.
(2) According to the condition that the molar weight of the reducing agent is 5 times of that of the oxidizing agent (the sum of the molar weights of the silver nitrate and the palladium nitrate in the step (1)), 41.1g of the reducing agent ascorbic acid is weighed and added with 116mL of deionized water, and stirred and dissolved at room temperature. Then, ammonia water with a mass concentration of 28% was added to adjust the pH of the reducing solution to 9.15.
(3) And (3) rapidly adding the reducing solution prepared in the step (2) into the oxidizing solution prepared in the step (1) at 25 ℃, and rapidly stirring for reaction for 1 h. After the reaction, the mixture was aged at room temperature for 0.5 h.
(4) And (3) filtering the reaction slurry obtained in the step (3), washing the reaction slurry twice by using deionized water and ethanol respectively, placing the reaction slurry in a vacuum drying oven, and drying the reaction slurry for 5 hours at the temperature of 40 ℃ under the pressure of-0.1 MPa to obtain 4.95g of black silver-palladium alloy powder, wherein a scanning electron microscope picture is shown in figure 1, and the average particle size is 420 nm.
Example 2
(1) According to the mass ratio of silver to palladium of 7: 3, weighing 5.51g of silver nitrate (analytically pure) and 16.04g of palladium nitrate solution (containing 9.35 percent of palladium) respectively, and adding a proper amount of deionized water to prepare a solution with the total molar concentration of silver and palladium being 0.2mol/L, wherein the volume of the obtained solution is 232 mL.
(2) According to the condition that the molar weight of the reducing agent is 4 times of that of the oxidizing agent (the sum of the molar weights of the silver nitrate and the palladium nitrate in the step (1)), 32.82g of the reducing agent ascorbic acid is weighed, 232mL of deionized water is added, and the mixture is stirred and dissolved at room temperature. Then, ammonia water with a mass concentration of 28% was added to adjust the pH of the reducing solution to 9.01.
(3) And (3) rapidly adding the reducing solution prepared in the step (2) into the oxidizing solution prepared in the step (1) at the temperature of 55 ℃, and rapidly stirring for reacting for 80 min. After the reaction, the mixture was aged at room temperature for 0.5 h.
(4) And (4) filtering the reaction slurry obtained in the step (3), washing the reaction slurry twice by using deionized water and ethanol respectively, placing the reaction slurry in a vacuum drying oven, and drying the reaction slurry for 8 hours at the temperature of 30 ℃ under the pressure of-0.1 MPa to obtain black silver-palladium alloy powder with the average particle size of 700nm, wherein the black silver-palladium alloy powder is 4.96 g.
Example 3
(1) According to the mass ratio of silver to palladium of 7.5: 2.5, weighing 5.91g of silver nitrate (analytically pure) and 13.38g of palladium nitrate solution (containing 9.35 percent of palladium), adding a proper amount of deionized water to prepare a solution with the total molar concentration of silver and palladium being 0.5mol/L, wherein the volume of the obtained solution is 93 mL.
(2) According to the condition that the molar weight of the reducing agent is 3 times of that of the oxidizing agent (the sum of the molar weights of the silver nitrate and the palladium nitrate in the step (1)), 24.62g of the reducing agent ascorbic acid is weighed, 93mL of deionized water is added, and the mixture is stirred and dissolved at room temperature. Then, ammonia water with a mass concentration of 28% was added to adjust the pH of the reducing solution to 9.50.
(3) And (3) rapidly adding the reducing solution prepared in the step (2) into the oxidizing solution prepared in the step (1) at 35 ℃, and rapidly stirring for reaction for 1.5 h. After the reaction, the mixture was aged at room temperature for 0.5 h.
(4) And (4) filtering the reaction slurry obtained in the step (3), washing the reaction slurry twice by using deionized water and ethanol respectively, placing the reaction slurry in a vacuum drying oven, and drying the reaction slurry for 4 hours at the temperature of 45 ℃ under the pressure of-0.1 MPa to obtain black silver-palladium alloy powder with the average particle size of 380nm, wherein the black silver-palladium alloy powder is 4.96 g.
Example 4
(1) According to the mass ratio of silver to palladium of 8: 2, weighing 6.32g of silver nitrate (analytically pure) and 10.70g of palladium nitrate solution (containing 9.35 percent of palladium) respectively, and adding a proper amount of deionized water to prepare a solution with the total molar concentration of silver and palladium being 0.3mol/L, wherein the volume of the obtained solution is 155 mL.
(2) 65.50g of ascorbic acid serving as a reducing agent is weighed according to the condition that the molar weight of the reducing agent is 8 times of that of the oxidizing agent (the sum of the molar weights of the silver nitrate and the palladium nitrate in the step (1)), 155mL of deionized water is added, and the mixture is stirred and dissolved at room temperature. Then, ammonia water with a mass concentration of 28% was added to adjust the pH of the reducing solution to 9.3.
(3) And (3) rapidly adding the reducing solution prepared in the step (2) into the oxidizing solution prepared in the step (1) at the temperature of 80 ℃, and rapidly stirring for reaction for 2 hours. After the reaction, the mixture was aged at room temperature for 0.5 h.
(4) And (4) filtering the reaction slurry obtained in the step (3), washing the reaction slurry twice by using deionized water and ethanol respectively, placing the reaction slurry in a vacuum drying oven, and drying the reaction slurry for 3 hours at 50 ℃ under the pressure of-0.1 MPa to obtain black silver-palladium alloy powder with the average particle size of 650nm, wherein the black silver-palladium alloy powder is 4.93 g.
Example 5
(1) According to the mass ratio of silver to palladium of 8.5: 1.5, 6.70g of silver nitrate (analytically pure) and 8.02g of palladium nitrate solution (containing 9.35 percent of palladium) are respectively weighed, and a proper amount of deionized water is added to prepare a solution with the total molar concentration of silver and palladium being 0.6mol/L, wherein the volume of the obtained solution is 77 mL.
(2) 34.90g of hydrazine hydrate serving as a reducing agent is weighed according to the condition that the molar weight of the reducing agent is 6 times of that of the oxidizing agent (the sum of the molar weights of the silver nitrate and the palladium nitrate in the step (1)), 63mL of deionized water is added, and the mixture is stirred and dissolved at room temperature. The pH of the reducing solution was then adjusted to 9.8 with dilute nitric acid solution.
(3) And (3) rapidly adding the reducing solution prepared in the step (2) into the oxidizing solution prepared in the step (1) at the temperature of 30 ℃, and rapidly stirring for reacting for 50 min. After the reaction, the mixture was aged at room temperature for 0.5 h.
(4) And (4) filtering the reaction slurry obtained in the step (3), washing the reaction slurry twice by using deionized water and ethanol respectively, placing the reaction slurry in a vacuum drying oven, and drying the reaction slurry for 5 hours at the temperature of 40 ℃ under the pressure of-0.1 MPa to obtain black silver-palladium alloy powder with the average particle size of 330nm, wherein the black silver-palladium alloy powder is 4.93 g.
Example 6
(1) According to the mass ratio of silver to palladium of 9: 1, weighing 6.70g of silver nitrate (analytically pure) and 7.10g of palladium nitrate solution (containing 9.35 percent of palladium) respectively, and adding a proper amount of deionized water to prepare a solution with the total molar concentration of silver and palladium being 0.4mol/L, wherein the volume of the obtained solution is 116 mL.
(2) According to the condition that the molar weight of the reducing agent is 7 times of that of the oxidizing agent (the sum of the molar weights of the silver nitrate and the palladium nitrate in the step (1)), 40.66g of hydrazine hydrate serving as a reducing agent is weighed, 100mL of deionized water is added, and the mixture is stirred and dissolved at room temperature. The pH of the reducing solution was then adjusted to 10.0 with dilute nitric acid solution.
(3) And (3) rapidly adding the reducing solution prepared in the step (2) into the oxidizing solution prepared in the step (1) at the temperature of 20 ℃, and rapidly stirring for reacting for 40 min. After the reaction, the mixture was aged at room temperature for 0.5 h.
(4) And (4) filtering the reaction slurry obtained in the step (3), washing the reaction slurry twice by using deionized water and ethanol respectively, placing the reaction slurry in a vacuum drying oven, and drying the reaction slurry for 6 hours at the temperature of 45 ℃ under the pressure of-0.1 MPa to obtain black silver-palladium alloy powder with the average particle size of 510nm and 4.93 g.
Finally, the above embodiments are merely illustrative and not restrictive, and it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the present invention, which is to be covered by the claims.
Claims (4)
1. A preparation method of submicron monodisperse silver-palladium powder is characterized by comprising the following steps: comprises the following steps
(1) According to the mass ratio of silver to palladium of 7-9: 3-1, weighing silver nitrate solid and palladium nitrate water solution containing 9.35% of palladium, and adding deionized water to prepare oxidant solution with metal ion molar concentration of 0.2-0.6 mol/L;
(2) weighing ascorbic acid or hydrazine hydrate as a reducing agent according to the molar weight which is 3-8 times of the sum of silver nitrate and palladium nitrate, dissolving with 63-232 mL of deionized water to ensure that the volume of the reducing agent solution is the same as that of the oxidant solution, and then adding ammonia water or dilute nitric acid solution with the mass concentration of 28% to adjust the pH value of the reducing agent solution to 9.01-10.0;
(3) adding a reducing agent solution into an oxidant solution at the temperature of 20-80 ℃, quickly stirring for 40 min-2 h, and aging for 0.5h at room temperature after the reaction is finished;
(4) and filtering the reaction slurry, washing twice with deionized water and ethanol respectively, placing the obtained solid in a vacuum drying oven, and drying for 3-8 h under the conditions of-0.1 MPa and 30-50 ℃ to obtain black silver-palladium alloy powder with the average particle size of 380-700 nm.
2. The method for preparing submicron monodisperse Ag-Pd powder according to claim 1, wherein 5.51-6.70 g of analytically pure silver nitrate and 7.10-16.04 g of palladium nitrate solution are weighed in step (1) to prepare 93-232 mL of oxidant solution.
3. The method for preparing submicron monodisperse Ag-Pd powder according to claim 1, wherein the molar weight ratio of the reducing agent to Ag-Pd nitrate in step (2) is 4: 1-6: 1.
4. The method for preparing submicron monodisperse Ag-Pd powder according to claim 1, 2 or 3, wherein 24.62-65.50 g of reducing agent is weighed in step (2).
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| 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 |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4776883A (en) * | 1986-05-30 | 1988-10-11 | Mitsui Mining & Smelting Co., Ltd. | Process for the production of silver-palladium alloy fine powder |
| JPH06256810A (en) * | 1993-03-08 | 1994-09-13 | Noritake Co Ltd | Silver-palladium composite powder and production thereof |
| JPH07109505A (en) * | 1993-10-08 | 1995-04-25 | Noritake Co Ltd | Production of silver-palladium composite powder and silver-palladium composite powder |
| JPH07118868A (en) * | 1993-10-20 | 1995-05-09 | Sumitomo Metal Mining Co Ltd | Production of palladium-coated spherical silver powder |
| JPH07150206A (en) * | 1993-12-01 | 1995-06-13 | Daido Steel Co Ltd | Production of ag-pd powder |
| CN104399972A (en) * | 2014-12-11 | 2015-03-11 | 成都明日星辰科技有限公司 | Preparation method of liquid phase single dispersing silver palladium composite powder |
| CN106270544A (en) * | 2015-06-12 | 2017-01-04 | 中国振华集团云科电子有限公司 | A kind of preparation method of the silver coprecipitated accumulated powder of palladium |
| CN108746659A (en) * | 2018-06-01 | 2018-11-06 | 西北工业大学 | A kind of flower-shaped AgPd Nanoalloys and preparation and application |
-
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Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4776883A (en) * | 1986-05-30 | 1988-10-11 | Mitsui Mining & Smelting Co., Ltd. | Process for the production of silver-palladium alloy fine powder |
| JPH06256810A (en) * | 1993-03-08 | 1994-09-13 | Noritake Co Ltd | Silver-palladium composite powder and production thereof |
| JPH07109505A (en) * | 1993-10-08 | 1995-04-25 | Noritake Co Ltd | Production of silver-palladium composite powder and silver-palladium composite powder |
| JPH07118868A (en) * | 1993-10-20 | 1995-05-09 | Sumitomo Metal Mining Co Ltd | Production of palladium-coated spherical silver powder |
| JPH07150206A (en) * | 1993-12-01 | 1995-06-13 | Daido Steel Co Ltd | Production of ag-pd powder |
| CN104399972A (en) * | 2014-12-11 | 2015-03-11 | 成都明日星辰科技有限公司 | Preparation method of liquid phase single dispersing silver palladium composite powder |
| CN106270544A (en) * | 2015-06-12 | 2017-01-04 | 中国振华集团云科电子有限公司 | A kind of preparation method of the silver coprecipitated accumulated powder of palladium |
| CN108746659A (en) * | 2018-06-01 | 2018-11-06 | 西北工业大学 | A kind of flower-shaped AgPd Nanoalloys and preparation and application |
Non-Patent Citations (1)
| Title |
|---|
| 熊庆丰;林智杰;姬爱青;刘绍宏;霍地;孙旭东;: "亚微米级球形银钯合金粉末的制备", 材料与冶金学报 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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