CN111659901A - Preparation method of submicron silver powder - Google Patents
Preparation method of submicron silver powder Download PDFInfo
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- CN111659901A CN111659901A CN202010556033.XA CN202010556033A CN111659901A CN 111659901 A CN111659901 A CN 111659901A CN 202010556033 A CN202010556033 A CN 202010556033A CN 111659901 A CN111659901 A CN 111659901A
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- deionized water
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title abstract description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 128
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 64
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 78
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 72
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 46
- 239000008367 deionised water Substances 0.000 claims description 44
- 229910021641 deionized water Inorganic materials 0.000 claims description 44
- 239000011668 ascorbic acid Substances 0.000 claims description 39
- 229960005070 ascorbic acid Drugs 0.000 claims description 39
- 235000010323 ascorbic acid Nutrition 0.000 claims description 39
- 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 description 30
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 23
- 238000003756 stirring Methods 0.000 claims description 22
- 239000003513 alkali Substances 0.000 claims description 16
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 14
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 11
- 238000010907 mechanical stirring Methods 0.000 claims description 11
- 235000010489 acacia gum Nutrition 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000001785 acacia senegal l. willd gum Substances 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000011085 pressure filtration Methods 0.000 claims description 4
- 230000001276 controlling effect Effects 0.000 claims description 3
- 239000002585 base Substances 0.000 claims description 2
- 241000220479 Acacia Species 0.000 claims 1
- 235000010643 Leucaena leucocephala Nutrition 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 7
- 229910052709 silver Inorganic materials 0.000 abstract description 3
- 239000004332 silver Substances 0.000 abstract description 3
- 239000012670 alkaline solution Substances 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 239000003638 chemical reducing agent Substances 0.000 description 16
- 239000000047 product Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 238000001914 filtration Methods 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 2
- 229920000084 Gum arabic Polymers 0.000 description 1
- 241000978776 Senegalia senegal Species 0.000 description 1
- 239000000205 acacia gum Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Classifications
-
- 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
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a preparation method of submicron silver powder, which takes silver nitrate as a silver source and innovatively adopts an opposite feeding mode to prepare submicron superfine silver powder, and when the opposite feeding mode is adopted for feeding, the silver powder has better dispersibility and higher tap density (more than 4.0 g/cm)3) The alkaline solution is added into the reaction system, so that the regular spherical silver powder can be obtained more favorably, and the reasonable use of the dispersing agent is favorable for improving the dispersibility of the silver powder particles.
Description
Technical Field
The invention belongs to a preparation method of silver powder, and particularly relates to a preparation method of submicron silver powder.
Background
With the development of photovoltaic industry and emerging electronic industry, the electronic conductive paste has wider and wider application. As the most important conductive component, the properties of the metal powder have a crucial influence on the quality of the electronic paste. Because of its good conductivity and relatively low cost, metallic silver is the main raw material for preparing the powder for slurry.
In industrial production, the chemical reduction method becomes a main method for producing silver powder due to the advantages of mild reaction conditions, low production cost, simple process route and the like.
The traditional method for preparing the silver powder mainly comprises two steps of forward feeding and reverse feeding. The forward feeding comprises the steps of dissolving silver nitrate, alkali and a reducing agent in water respectively, dissolving a dispersing agent in a reducing agent solution, slowly pouring an alkali solution into the silver nitrate solution, uniformly stirring, fixing the stirring rate of the reducing agent solution, and finally slowly adding the silver nitrate solution into the reducing agent solution to react for 5 min; and the reverse feeding is to dissolve silver nitrate, alkali and a reducing agent in water respectively, dissolve a dispersing agent in a reducing agent solution, slowly pour an alkali solution into the silver nitrate solution and stir uniformly, fix the stirring rate of the silver nitrate solution, slowly add the reducing agent solution into the silver nitrate solution and react for 5 min.
The preparation method firstly adjusts the pH value of silver nitrate by using alkali liquor, reduces the reaction energy barrier, and has the defect that the appearance of the prepared silver powder is influenced by the alkali liquor.
Disclosure of Invention
The invention aims to provide a method for preparing submicron silver powder with higher sphericity aiming at the defects of the prior art, which is used for converting silver nitrate into the submicron silver powder by a chemical reduction method.
In order to achieve the above purpose, the invention provides the following scheme: a preparation method of submicron silver powder sequentially comprises the following steps:
dissolving silver nitrate in deionized water to obtain a silver nitrate solution, dissolving a reducing agent hydrazine hydrate or ascorbic acid in the deionized water as a reaction bottom solution, and adding a dispersing agent to fully dissolve;
secondly, controlling the stirring speed of the reaction bottom liquid to be 300-600 rpm, keeping the feeding speed consistent, and adding the alkali solution into the reaction bottom liquid simultaneously with the silver nitrate solution instead of the silver nitrate solution; wherein the using amount of hydrazine hydrate or ascorbic acid solution is 1.5 times of the theoretical using amount, the dispersant is 0.3 percent of the mass of silver nitrate, the pH value does not need to be specially adjusted before the reaction starts, and the pH value of the reaction solution is 7 +/-1 after the reaction finishes;
and thirdly, after the reaction is finished, separating out the silver powder by filtering under reduced pressure, washing the silver powder by using deionized water until the conductivity of the filtrate is less than 10 mu S/cm, washing the silver powder by using absolute ethyl alcohol for three times, and drying the silver powder for 24 hours in a blast drying oven at the temperature of 60 ℃ to obtain the submicron-grade silver powder.
Further, the dispersing agent is Arabic gum or PVP; the alkali solution is ammonia water or sodium hydroxide solution.
Wherein, the first step is to weigh 80 g of silver nitrate, 25 g of hydrazine hydrate and 45 ml of ammonia water and respectively dissolve the silver nitrate, the hydrazine hydrate and the ammonia water in 250ml of deionized water, 250ml of deionized water and 300 ml of deionized water; weighing 0.25 g of Arabic gum, dissolving in a hydrazine hydrate solution, and putting into a mechanical stirring paddle for stirring; and secondly, placing two separating funnels with well-adjusted liquid flow rates on two sides of the hydrazine hydrate solution, respectively pouring the silver nitrate solution and the dilute ammonia water, slowly adding the silver nitrate solution and the dilute ammonia water into the hydrazine hydrate solution, and reacting for 5min after all the materials are added.
Wherein, the first step is to weigh 80 g of silver nitrate, 50 g of ascorbic acid and 45 ml of sodium hydroxide and respectively dissolve the silver nitrate, the ascorbic acid and the 45 ml of sodium hydroxide in 250ml of deionized water, 250ml of deionized water and 300 ml of deionized water; weighing 0.25 g of Arabic gum, dissolving in ascorbic acid solution, and stirring with a mechanical stirring paddle; the second step is to place two separating funnels with well regulated liquid flow rate on two sides of ascorbic acid solution, pour silver nitrate solution and sodium hydroxide solution separately, add the two into ascorbic acid solution slowly, after the materials are added completely, react for 5min
Wherein, the first step is to weigh 80 g of silver nitrate, 50 g of ascorbic acid and 45 ml of sodium hydroxide and respectively dissolve the silver nitrate, the ascorbic acid and the 45 ml of sodium hydroxide in 250ml of deionized water, 250ml of deionized water and 300 ml of deionized water; weighing 0.25 g of PVP, dissolving in ascorbic acid solution, and stirring in a mechanical stirring paddle; and the second step is that two separating funnels with well regulated liquid flow rate are placed on two sides of the ascorbic acid solution, the silver nitrate solution and the sodium hydroxide solution are poured into the ascorbic acid solution and the silver nitrate solution and the sodium hydroxide solution respectively, the silver nitrate solution and the sodium hydroxide solution are slowly added into the ascorbic acid solution, and after all the materials are added, the reaction is carried out for 5 min.
The invention has the beneficial effects that: on the basis of the prior art, the invention takes ascorbic acid, hydrazine hydrate and the like as reducing agents, adopts a novel opposite charging mode, and adopts alkaliThe solution is not added into the silver nitrate solution, but is added into the reaction base solution simultaneously with the silver nitrate solution, so that the influence of the alkali liquor on the system is reduced, compared with a preparation method of forward feeding and reverse feeding, the interference of the formation of silver oxide on the appearance of the silver powder is reduced, the sphericity of the silver powder is increased, and the silver powder has better dispersibility and higher tap density (more than 4.0 g/cm)3)。
Drawings
FIG. 1 is a silver powder prepared by forward charging in the prior art;
FIG. 2 is a silver powder prepared by reverse charging in the prior art;
FIG. 3 is a diagram of a product of silver powder prepared by the method of the present invention at 10 μm;
FIG. 4 is a product diagram of silver powder prepared by the method of the present invention at 1 μm.
Detailed Description
The invention is further described with reference to the accompanying drawings and specific embodiments.
The reducing agents commonly used for producing the silver powder by adopting the chemical reduction method comprise glycerol, hydrazine hydrate, sodium borohydride, hydrogen peroxide, ascorbic acid and the like, and the silver powder obtained by adopting different reducing agents has different properties due to different chemical properties. In the reaction process, in order to overcome the agglomeration problem among silver powder particles, one or more dispersants are often added into the reaction system. The action mechanism of the dispersing agent is that the silver particles are coated on the outer layer of the particles after being formed, so that agglomeration among the particles is prevented. In addition, the charging mode also has great influence on the performance of the silver powder.
The invention adopts a basic method as a chemical reduction method, and mainly comprises the following steps:
dissolving silver nitrate in deionized water to obtain a silver nitrate solution, dissolving a reducing agent hydrazine hydrate or ascorbic acid in the deionized water as a reaction bottom solution, and adding a dispersing agent to fully dissolve.
Secondly, controlling the stirring speed of the reaction bottom liquid to be 300-600 rpm, keeping the feeding speed consistent, and adding the alkali solution into the reaction bottom liquid simultaneously with the silver nitrate solution instead of the silver nitrate solution; the using amount of hydrazine hydrate or ascorbic acid solution is 1.5 times of the theoretical using amount, the dispersing agent is 0.3 percent of the mass of silver nitrate, the pH value does not need to be specially adjusted before the reaction starts, and the pH value of the reaction solution is 7 +/-1 after the reaction finishes.
And thirdly, after the reaction is finished, separating out the silver powder by filtering under reduced pressure, washing the silver powder by using deionized water until the conductivity of the filtrate is less than 10 mu S/cm, washing the silver powder by using absolute ethyl alcohol for three times, and drying the silver powder for 24 hours in a blast drying oven at the temperature of 60 ℃ to prepare the submicron silver powder.
The innovation of the present disclosure is mainly focused on the second reaction step.
Compared with the traditional method, the difference of the opposite feeding is as follows: the traditional method firstly adjusts the pH value of silver nitrate by using alkali liquor and reduces the reaction energy barrier, and the method has the defects that the morphology of the prepared silver powder is influenced by the alkali liquor; when the silver powder is prepared by adopting the opposite adding mode, the alkali solution and the silver nitrate solution are simultaneously added into the reducing solution, so that the interference of the alkali solution can be effectively eliminated, and the silver powder with higher sphericity can be obtained.
Example 1
80 g of silver nitrate, 25 g of hydrazine hydrate and 45 ml of ammonia water are weighed out and dissolved in 250ml of deionized water, 250ml of deionized water and 300 ml of deionized water respectively, and 0.25 g of Arabic gum is weighed out and dissolved in the hydrazine hydrate solution. And (3) putting a mechanical stirring paddle into the hydrazine hydrate solution, and adjusting a proper stirring speed. Two separating funnels with well regulated liquid flow rate are set on two sides of hydrazine hydrate solution, silver nitrate solution and dilute ammonia water are poured separately and added slowly into hydrazine hydrate solution. After all the materials are added, the reaction is carried out for 5min, the product is subjected to reduced pressure filtration and separation, then is washed by deionized water until the conductivity of the filtrate is less than 10 mu S/cm, and then is washed by absolute ethyl alcohol for three times and is dried for 24 h in a blast drying oven at 60 ℃. Thus, silver powder prepared by a double addition method was obtained.
Example 2
80 g of silver nitrate, 50 g of ascorbic acid and 45 ml of sodium hydroxide are weighed out and dissolved in 250ml, 250ml and 300 ml of deionized water, respectively, and 0.25 g of gum arabic is weighed out and dissolved in the ascorbic acid solution. A mechanical stirring paddle is placed in the ascorbic acid solution, and the stirring speed is adjusted properly. Two separating funnels with well-adjusted liquid flow rates are placed on two sides of the ascorbic acid solution, and the silver nitrate solution and the sodium hydroxide solution are poured into the ascorbic acid solution and the silver nitrate solution and the sodium hydroxide solution respectively, so that the silver nitrate solution and the sodium hydroxide solution are slowly added into the ascorbic acid solution. After all the materials are added, the reaction is carried out for 5min, the product is subjected to reduced pressure filtration and separation, then is washed by deionized water until the conductivity of the filtrate is less than 10 mu S/cm, and then is washed by absolute ethyl alcohol for three times and is dried for 24 h in a blast drying oven at 60 ℃. Thus, silver powder prepared by a double addition method was obtained.
Example 3
80 g of silver nitrate, 50 g of ascorbic acid and 45 ml of sodium hydroxide are weighed out and dissolved in 250ml of deionized water, 250ml of deionized water and 300 ml of deionized water, and 0.25 g of PVP is weighed out and dissolved in the ascorbic acid solution. A mechanical stirring paddle is placed in the ascorbic acid solution, and the stirring speed is adjusted properly. Two separating funnels with well-adjusted liquid flow rates are placed on two sides of the ascorbic acid solution, and the silver nitrate solution and the sodium hydroxide solution are poured into the ascorbic acid solution and the silver nitrate solution and the sodium hydroxide solution respectively, so that the silver nitrate solution and the sodium hydroxide solution are slowly added into the ascorbic acid solution. After all the materials are added, the reaction is carried out for 5min, the product is subjected to reduced pressure filtration and separation, then is washed by deionized water until the conductivity of the filtrate is less than 10 mu S/cm, and then is washed by absolute ethyl alcohol for three times and is dried for 24 h in a blast drying oven at 60 ℃. Thus, silver powder prepared by a double addition method was obtained.
COMPARATIVE EXAMPLE 1 (Forward Charge)
80 g of silver nitrate, 25 g of hydrazine hydrate and 45 ml of ammonia water are weighed out and dissolved in 250ml of deionized water, 250ml of deionized water and 300 ml of deionized water respectively, and 0.25 g of Arabic gum is weighed out and dissolved in the hydrazine hydrate solution. And stirring the silver nitrate solution at a constant speed by using a glass rod, and slowly pouring the diluted ammonia water into the silver nitrate solution while stirring to finally obtain a dark brown silver-ammonia complex suspension. And (3) placing a mechanical stirring paddle in the hydrazine hydrate solution, adjusting a proper stirring speed, and slowly pouring the silver-ammonia complex suspension into the hydrazine hydrate solution. After 5min of reaction, the product is separated by filtration under reduced pressure, washed by deionized water until the conductivity of the filtrate is less than 10 mu S/cm, washed by absolute ethyl alcohol for three times and dried in a blast drying oven at 60 ℃ for 24 h. Thus, silver powder prepared by forward feeding was obtained.
COMPARATIVE EXAMPLE 2 (reverse charge)
80 g of silver nitrate, 25 g of hydrazine hydrate and 45 ml of ammonia water are weighed out and dissolved in 250ml of deionized water, 250ml of deionized water and 300 ml of deionized water respectively, and 0.25 g of Arabic gum is weighed out and dissolved in the hydrazine hydrate solution. And stirring the silver nitrate solution at a constant speed by using a glass rod, and slowly pouring the diluted ammonia water into the silver nitrate solution while stirring to finally obtain a dark brown silver-ammonia complex suspension. And (3) placing a mechanical stirring paddle in the silver-ammonia complex suspension, adjusting a proper stirring speed, and slowly pouring the hydrazine hydrate solution into the silver-ammonia complex suspension. After 5min of reaction, the product is separated by filtration under reduced pressure, washed by deionized water until the conductivity of the filtrate is less than 10 mu S/m, washed by absolute ethyl alcohol for three times and dried in a blast drying oven at 60 ℃ for 24 h. Thus, silver powder prepared by reverse feeding is obtained.
The submicron ultrafine silver powder prepared by the invention is compared with the silver powder prepared by the traditional method, a scanning electron microscope, a tap density instrument and a laser particle size analyzer are used for characterizing the powder, the product figures of the silver powder obtained by different feeding methods are shown in figures 1, 2, 3 and 4, and the particle diameter and tap density are shown in the following table.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (5)
1. A method for preparing submicron silver powder is characterized in that: sequentially comprises the following steps
Dissolving silver nitrate in deionized water to obtain a silver nitrate solution, dissolving hydrazine hydrate or ascorbic acid in the deionized water as a reaction bottom solution, and adding a dispersing agent to fully dissolve;
secondly, controlling the stirring speed of the reaction base solution to be 300-600 rpm, and adding an alkali solution and a silver nitrate solution while keeping the feeding speed consistent; wherein the dosage of the hydrazine hydrate or ascorbic acid solution is 1.5 times of the theoretical dosage, the dispersant is 0.3 percent of the mass of the silver nitrate, and the pH value of the reaction solution is 7 +/-1 after the reaction is finished;
and thirdly, separating the silver powder by reduced pressure filtration, washing the silver powder by deionized water until the conductivity of the filtrate is less than 10 mu S/cm, washing the silver powder by absolute ethyl alcohol, and drying the silver powder in a drying box to obtain the submicron silver powder.
2. The method for preparing submicron silver powder according to claim 1, wherein the dispersant is acacia or PVP; the alkali solution is ammonia water or sodium hydroxide solution.
3. The method for preparing submicron silver powder according to claim 2, wherein the first step is to weigh 80 g of silver nitrate, 25 g of hydrazine hydrate and 45 ml of ammonia water and dissolve in 250ml of deionized water, 250ml of hydrazine hydrate and 300 ml of deionized water respectively; weighing 0.25 g of Arabic gum, dissolving in a hydrazine hydrate solution, and putting into a mechanical stirring paddle for stirring; and in the second step, two separating funnels with well-regulated liquid flow rates are placed on two sides of the hydrazine hydrate solution, and a silver nitrate solution and dilute ammonia water are respectively poured into the separating funnels and are slowly added into the hydrazine hydrate solution to react for 5 min.
4. The method for preparing submicron silver powder according to claim 2, wherein the first step is weighing 80 g silver nitrate, 50 g ascorbic acid and 45 ml sodium hydroxide in 250ml deionized water, 250ml deionized water and 300 ml deionized water respectively; weighing 0.25 g of Arabic gum, dissolving in ascorbic acid solution, and stirring with a mechanical stirring paddle; and in the second step, two separating funnels with well-regulated liquid flow rates are placed on two sides of the ascorbic acid solution, the silver nitrate solution and the sodium hydroxide solution are respectively poured into the separating funnels, and the silver nitrate solution and the sodium hydroxide solution are slowly added into the ascorbic acid solution to react for 5 min.
5. The method for preparing submicron silver powder according to claim 2, wherein the first step is weighing 80 g silver nitrate, 50 g ascorbic acid and 45 ml sodium hydroxide in 250ml deionized water, 250ml deionized water and 300 ml deionized water respectively; weighing 0.25 g of PVP, dissolving in ascorbic acid solution, and stirring in a mechanical stirring paddle; and in the second step, two separating funnels with well-regulated liquid flow rates are placed on two sides of the ascorbic acid solution, the silver nitrate solution and the sodium hydroxide solution are respectively poured into the separating funnels, and the silver nitrate solution and the sodium hydroxide solution are slowly added into the ascorbic acid solution to react for 5 min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114472917A (en) * | 2022-02-11 | 2022-05-13 | 西安汇创贵金属新材料研究院有限公司 | Preparation method of high-dispersity submicron silver powder |
| CN116372181A (en) * | 2023-06-07 | 2023-07-04 | 长春黄金研究院有限公司 | Rod-shaped silver powder and preparation method thereof |
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| CN116372181A (en) * | 2023-06-07 | 2023-07-04 | 长春黄金研究院有限公司 | Rod-shaped silver powder and preparation method thereof |
| CN116372181B (en) * | 2023-06-07 | 2023-09-05 | 长春黄金研究院有限公司 | Rod-shaped silver powder and preparation method thereof |
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Application publication date: 20200915 |