WO2020106120A1 - Procédé de preparation de poudre d'argent monodispersée - Google Patents

Procédé de preparation de poudre d'argent monodispersée

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Publication number
WO2020106120A1
WO2020106120A1 PCT/KR2019/016204 KR2019016204W WO2020106120A1 WO 2020106120 A1 WO2020106120 A1 WO 2020106120A1 KR 2019016204 W KR2019016204 W KR 2019016204W WO 2020106120 A1 WO2020106120 A1 WO 2020106120A1
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WO
WIPO (PCT)
Prior art keywords
silver powder
silver
reaction solution
reaction
acid
Prior art date
Application number
PCT/KR2019/016204
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English (en)
Korean (ko)
Inventor
강태훈
김영환
이미영
이창근
진우민
최재원
Original Assignee
엘에스니꼬동제련 주식회사
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
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Publication of WO2020106120A1 publication Critical patent/WO2020106120A1/fr

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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
    • 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
    • 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
    • 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
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/25—Noble metals, i.e. Ag Au, Ir, Os, Pd, Pt, Rh, Ru
    • B22F2301/255—Silver or gold

Definitions

  • the present invention relates to a method for manufacturing silver powder contained in a conductive paste used in electronic components, such as an electrode for a solar cell, an internal electrode of a multilayer capacitor, and a conductor pattern of a circuit board, and a conductive paste containing silver powder.
  • Silver is widely used as an electrode material in the field of electrical and electronic due to its inherent high electrical conductivity and oxidation stability.
  • an industry for conductive pastes in which silver is powdered and processed into a paste or ink form has been developed.
  • Conductive pastes using silver powder have various uses such as plasma display panel (PDP), solar cell front electrode or rear electrode, and touch screen, as well as traditional conductive electrodes such as through-holes, die-bonding, and chip parts. This is an increasing trend.
  • silver powder for solar cell electrodes often has non-uniform nucleation during synthesis, agglomeration of powders due to difference in reaction rate, and wide particle size distribution, which causes defects due to disconnection and short circuit between electrodes in the printing process after paste preparation. .
  • the present invention is to solve the above problems to solve the agglomeration of the silver powder and to provide an economical manufacturing method capable of mass-producing sub-micro grade fine powder.
  • the present invention is a reaction solution production step (S21) for preparing a first reaction solution containing a silver ion, ammonia (NH 3) and an organic acid alkali metal salt and a second reaction solution containing a reducing agent; And a silver salt reduction step (S2) including a precipitation step (S22) of reacting the first reaction solution and the second reaction solution while freely falling in the air to obtain silver powder.
  • S21 reaction solution production step
  • S2 for preparing a first reaction solution containing a silver ion, ammonia (NH 3) and an organic acid alkali metal salt and a second reaction solution containing a reducing agent
  • S2 silver salt reduction step
  • S22 precipitation step
  • the first reaction solution and the second reaction solution are respectively supplied at a specific height of the reaction tank through a supply line capable of adjusting the flow rate while the first reaction solution and the second reaction solution are freely dropped. It is characterized by reacting.
  • the height (H) to which the first reaction solution and the second reaction solution are supplied is characterized in that the reaction tank and the reaction temperature of the reaction tank are 30 to 50 ° C.
  • the alkali metal salt of the organic acid is acetic acid (CH3COOH), formic acid (CH2O2), oxalic acid (C2H2O4), lactic acid (C3H6O3), citric acid (C6H8O7), fumaric acid (C4H4O4), citric acid (C6H8O7), butyric acid (C4H8O2), butyric acid (C4H8O2) )
  • any one or more organic acids selected from the group consisting of uric acid (C5H4N4O3) and lithium (Li), sodium (Na), potassium (K), calcium (Ca) and magnesium (Mg). Characterized in that it comprises a salt formed by any one or more metals.
  • the organic acid alkali metal salt is characterized in that it is added at a ratio of 300 to 600 g with respect to 1600 ml of the 500 g / L silver nitrate (AgNO3).
  • the present invention is a silver powder produced by the above manufacturing method, wherein the silver powder has a SEM size (DSEM) of 03 to 13 ⁇ m and a PSA size (D50) of 01 to 20 ⁇ m.
  • DSEM SEM size
  • D50 PSA size
  • the silver powder is characterized in that the span value calculated by the following formula (span value) is 10 or less.
  • D90, D10, and D50 mean particle sizes corresponding to 90%, 10%, and 50% of the maximum value in the cumulative distribution of solid particle size, respectively.
  • the silver powder is characterized in that the aggregation degree calculated by the ratio (D50 / DSEM) of PSA size (D50, ⁇ m) to SEM size (DSEM, ⁇ m) is 17 or less.
  • the present invention can obtain a monodispersed silver powder having a size of 03 to 13 ⁇ m (SEM size) by precipitating silver powder by an air-free fall method, and can prevent agglomeration from occurring, and the amount of organic acid alkali metal salt added and the reaction temperature By controlling the, even if a fine powder having a size of about 03 ⁇ m is manufactured, it is possible to maintain monodispersity and prevent aggregation from occurring.
  • SEM size size
  • Figure 1 shows a process schematic diagram of the precipitation step according to an embodiment of the present invention.
  • the terms comprise, comprises, comprising means referring to an article, step or group of articles, and steps, and any other article It is not intended to exclude a stage or group of things or a group of stages.
  • a silver powder having a level of 0.3 to 1.3 ⁇ m can be obtained by preparing a silver powder by adjusting an air-free fall reaction and an input amount of oxalic acid.
  • the method for preparing silver powder according to an embodiment of the present invention includes a silver salt production step (S1); Silver salt reduction step (S2); Purification step such as filtration and washing (S3); Surface treatment step (S4); And a post-treatment step (S5).
  • the method for preparing silver powder according to the present invention necessarily includes a silver salt reduction step (S2), and other steps can be omitted.
  • silver salt solution containing silver ions (Ag +) is prepared by acid treatment of silver (Ag +) in the form of an ingot, a chip, or a granule. It is a step.
  • a silver salt solution may be directly prepared through a silver salt preparation step (S1), and a subsequent step may be performed using a commercially available silver nitrate (AgNO3), silver salt complex, or silver intermediate solution.
  • the silver salt reduction step (S2) is a step of depositing silver particles by reducing silver ions by reacting the silver salt solution and the reduction solution in an air-free fall method.
  • the reaction solution production step (S21) for preparing a first reaction solution containing a silver salt solution, a first reaction solution containing ammonia and an alkali metal salt of an organic acid and a reducing agent (S21), and freely falling the first reaction solution and the second reaction solution It comprises a precipitation step (S22) to obtain a silver powder by reacting in a manner.
  • reaction solution preparation step (S21) ammonia and an organic acid alkali metal salt are added to a silver salt solution containing silver ions and stirred and dissolved to prepare a first reaction solution. More specifically, a first reaction solution is prepared by adding an alkali metal salt of an organic acid to a silver salt solution containing silver ions and adjusting the pH with ammonia.
  • the silver ion is not limited as long as it is in the form of a silver cation.
  • it may be silver nitrate (AgNO3), a silver salt complex, or a silver intermediate. It is preferable to use silver nitrate (AgNO3).
  • AgNO3 silver nitrate
  • the use of silver nitrate (AgNO3) containing silver ions will be described as an example.
  • the content of other components based on 1600 g / L silver nitrate (AgNO3) 1600 mL will be described.
  • the organic acid alkali metal salt is acetic acid (CH3COOH), formic acid (CH2O2), oxalic acid (C2H2O4), lactic acid (C3H6O3), citric acid (C6H8O7), fumaric acid (C4H4O4), citric acid (C6H8O7), butyric acid (C4H8O2), butyric acid (C4H8O2), And one or more organic acids (short-chain fatty acids) selected from the group consisting of uric acid (C5H4N4O3), lithium (Li), sodium (Na), potassium (K), calcium (Ca), and magnesium (Mg). And salts formed by any one or more metals selected from the above.
  • potassium oxalate (C2K2O4) is used, and it is preferable to selectively use potassium sulfide.
  • the organic acid alkali metal salt may be added in a ratio of 300 to 600 g with respect to 1600 ml of the 500 g / L silver nitrate (AgNO3). It is possible to provide an effect of increasing the shrinkage rate by adding the organic acid alkali metal salt in the above range, and it is also possible to control the size of the precipitated silver powder as supported by the experimental examples to be described later.
  • the addition amount of the alkali metal salt of the organic acid is outside the above range, the pH of the first reaction solution is lowered, and thus, the reaction rate is significantly reduced. Therefore, it is difficult to secure the height for free falling in the air in the precipitation step, which will be described later.
  • the silver particles can be grown non-uniformly with the same result as reacting.
  • the addition amount of the alkali metal salt of the organic acid is adjusted within the above range, the particle size of the precipitated silver powder can be controlled, and when added beyond the above range, the powder aggregates, and there is a problem in that a silver powder of uniform size cannot be obtained.
  • Ammonia can be used in the form of an aqueous solution.
  • a 25% aqueous ammonia solution may be added at a rate of 2000 ml to 3000 ml with respect to 1600 ml of 500 g / L silver nitrate (AgNO3).
  • ammonia serves to control the pH.
  • a 25% aqueous ammonia solution When a 25% aqueous ammonia solution is added in a proportion of less than 2000 ml with respect to 1600 ml of 500 g / L silver nitrate (AgNO3), all silver ions may not be reduced or it may be difficult to form a uniform particle distribution.
  • 25% ammonia aqueous solution is added in a proportion exceeding 3000 ml with respect to 1600 ml of 500 g / L silver nitrate (AgNO3), the spheroidization or monodispersity of the powder improves as the pH increases, but the organic content in the prepared silver powder After the conductive paste is higher than the desired standard, carbon may be accumulated and conductivity may be deteriorated.
  • the ammonia includes its derivatives.
  • the reduction rate should be fast when reacting in the air free fall method.
  • the ammonia serves to control the pH and the reduction rate, and when the ammonia is included below the content, the reduction rate is lowered and the reaction rate is slowed down. Therefore, there is a problem that particles are grown non-uniformly at the bottom of the reaction tank, and if it is included in excess of the above content, the reaction rate becomes too fast, and the second reaction liquids are captured in the powder, causing a slight increase in organic matter ( ⁇ 1.5%). Can occur.
  • the above-described first reaction solution may be prepared in an aqueous solution state by adding silver ions, an alkali metal salt of an organic acid and an aqueous ammonia solution to a solvent such as water and stirring it to dissolve, and may also be prepared in a slurry form.
  • the reaction solution preparation step (S21) according to an embodiment of the present invention also prepares a second reaction solution containing a reducing agent.
  • the reducing agent may be at least one selected from the group consisting of alkanolamine, hydroquinone, hydrazine and formalin, and among them, hydroquinone may be preferably selected.
  • the reducing agent may be included in 300 to 500g with respect to 1600ml of 500g / L nitric acid contained in the first reaction solution.
  • 500g / L silver nitrate may reduce all of the silver ions when the reducing agent is less than 300g for 1600ml, and 500g / L silver nitrate may increase the organic content when reducing agent exceeds 500g for 1600ml. there is a problem.
  • the reducing agent should be included in an amount capable of reducing all of the silver ions, and by adjusting the concentration of the reducing agent included in the second reaction solution. The reduction rate can be adjusted.
  • the reduction rate may be increased by increasing the concentration of the reducing agent or increasing the reduction rate or decreasing the concentration of the reducing agent.
  • the second reaction solution containing the reducing agent may be prepared by adding a reducing agent to a solvent such as water, stirring and dissolving it to form an aqueous solution having a concentration of 5% or less.
  • Precipitation step (S22) is a step of obtaining a silver powder by reacting the first reaction solution and the second reaction solution, the first reaction solution and the preparation prepared by the reaction solution production step (S21) 2
  • the reaction solution can be reacted in a free-falling manner.
  • an appropriate amount of the reaction solution reacts uniformly and continuously during the free-fall of the reaction solutions to prevent aggregation between particles and increase dispersibility.
  • silver particles may be precipitated in a free-falling manner using a reaction liquid tank and a reaction tank as shown in FIG. 1.
  • the first reaction liquid and the second reaction liquid may be prepared in a first reaction liquid production tank and a second reaction liquid production tank, respectively.
  • the reaction liquids prepared in each tank are respectively supplied to the reaction tanks through a supply line capable of adjusting the flow rate.
  • a supply line capable of adjusting the flow rate.
  • the reaction liquid is injected through a nozzle having a diameter of 15 ⁇ to the reaction tank, it is preferable to be supplied at a flow rate of 3.8L / min to 4.5L / min.
  • the first reaction liquid and the second reaction liquid react while being supplied to the reaction tank through a nozzle and dropping in the air.
  • the height (H) at which the first reaction solution and the second reaction solution are supplied is dropped from the height of 3 m or more relative to the bottom of the reaction tank.
  • aggregation of silver powder produced when falling in the air below 3 m occurs.
  • monodisperse particles having better air-falling at a height of 5 m to 7 m can be obtained.
  • the reaction temperature of the reaction tank is adjusted to 30 to 50 ° C to react.
  • the size of the precipitated silver powder can be controlled by controlling the reaction temperature to the above range, as supported by the experimental examples described later.
  • the reaction temperature is increased, it is possible to increase the density of the powder surface, increase the crystallinity, and affect the coating degree of the coating agent, and increase the reaction temperature when the content of the organic acid alkali metal salt added to the first reaction solution is the same.
  • the particle size of the precipitated silver powder can be reduced.
  • Purification step (S3) is a step of separating and washing the silver powder dispersed in the silver powder dispersion obtained at the bottom of the reaction tank through filtration through silver salt (S31) (S31) ). More specifically, after the silver particles in the silver powder dispersion are precipitated, the supernatant of the dispersion is discarded, filtered using a centrifuge, and the filter medium is washed with pure water. The washing process can completely remove the washing water from washing the powder.
  • the purification step (S3) may further include a drying and disintegration step (S32) after washing.
  • the water content may be 10% or less, but the present invention is not limited thereto.
  • the surface treatment step (S4) is a step of hydrophobicizing the hydrophilic surface of the silver powder, and may be selectively performed. This is because if the silver powder has a hydrophilic surface, properties may change due to moisture and surface oxidation during long-term storage, and may have a great influence on compatibility with organic solvents and final printing properties when prepared with a conductive paste.
  • the surface treatment agent a single or multiple compounds in the form of a salt or emulsion may be used.
  • hydrophobicity may be imparted to the silver powder by adding a surface treatment agent containing octadecylamine to the silver powder obtained after filtration.
  • octadecylamine may contain 0.01 to 0.1 parts by weight (eg, 0.03 parts by weight) with respect to 100 parts by weight of silver nitrate.
  • the silver powder can be obtained again through filtration, washing, drying, and crushing.
  • the silver powder is surface-treated, the powder must be well dispersed, so that the surface treatment is sufficiently achieved. If the water content is low, the dispersion efficiency decreases, so that the surface treatment is performed with a certain amount of water content (for example, 70 to 85%). good.
  • the post-treatment step (S5) may include a crushing process for dispersing the agglomerated powder and drying the silver powder obtained after the surface treatment, and a classification process for removing the coarse powder.
  • the crushing process may be performed at a constant air pressure (for example, 0.4 kgf) and a feeding speed (for example, 30 to 60 g / min) using a jet mill or the like, but the present invention is limited thereto. It does not work.
  • the silver powder prepared according to the method of manufacturing a silver powder according to an embodiment of the present invention has a SEM size (DSEM) of 0.3 to 1.3 ⁇ m, a PSA size (D50) of 1.0 to 2.0 ⁇ m, and is measured in an experimental example to be described later.
  • the resulting span value is 1.0 or less, and the degree of aggregation (D50 / DSEM) measured in the experimental examples to be described later is 1.7 or less.
  • the SEM size is less than 0.3 ⁇ m, and even fine silver powder, which appears to be monodisperse on the SEM image, can be manufactured.
  • the present invention also provides a conductive paste comprising silver powder prepared according to one embodiment of the present invention. More specifically, the conductive paste according to the present invention can be suitably used for forming a solar cell electrode, including silver powder, glass frit, and organic vehicle prepared according to the present invention.
  • the conductive paste composition according to the present invention may further include additives commonly known as necessary, for example, dispersants, plasticizers, viscosity modifiers, surfactants, oxidizing agents, metal oxides, metal organic compounds, and the like.
  • the present invention also provides a method for forming an electrode of a solar cell, characterized in that the conductive paste is applied onto a substrate, dried and fired, and a solar cell electrode produced by the method. Except for using the conductive paste containing the silver powder of the above characteristics in the method for forming a solar cell electrode of the present invention, substrates, printing, drying and firing can be used, as well as methods commonly used in the manufacture of solar cells. to be.
  • the substrate may be a silicon wafer.
  • a first reaction solution was prepared by adding and stirring 1600 ml of silver nitrate (500 g / L), 380 g of potassium oxalate, and 2560 ml of ammonia (concentration 25%) in 15840 g of pure water at room temperature in the first reaction solution tank. Meanwhile, in the second reaction liquid tank, 400 g of hydroquinone was added to 20000 g of pure water at room temperature and stirred to prepare a second reaction liquid.
  • the flow rate was controlled at 3.8L / min 4.5L / min using a chemical pump from WILO, and the reaction solution was transferred to the reaction tank, respectively, and then sprayed from the nozzle (air-dropping method) to generate the first reaction solution and the second reaction solution.
  • the silver powder dispersion liquid containing silver powder that reacted and precipitated while falling in the air was recovered from the bottom of the reaction tank.
  • the reaction temperature of the reaction tank was 35 ° C, and the drop heights of the first reaction solution and the second reaction solution were 6 m.
  • the supernatant of the dispersion is discarded, filtered using a centrifuge, and the filter medium is washed with pure water. Thereafter, the washing water was removed to a water content of less than 10%. After this, a surface treatment agent was added, and the water content was adjusted to 70 to 85%, and the final silver powder was obtained through drying and crushing.
  • Silver powder was obtained in the same manner as in Example 1, except that the drop heights of the first reaction solution and the second reaction solution were 3 m.
  • Silver powder was obtained in the same manner as in Example 1, except that the reaction tank had a reaction temperature of 50 ° C.
  • Silver powder was obtained in the same manner as in Example 1, except that the drop heights of the first reaction solution and the second reaction solution were 2 m.
  • Example 1 15480 1600 380 2560 20000 400 Airdrop 35 6
  • Example 2 15480 1600 380 2560 20000 400 Airdrop 35 3
  • Example 3 15480 1600 380 2560 20000 400 Airdrop 50 6
  • Example 4 15480 1600 570 2560 20000 400 Airdrop 50 6 Comparative Example 1 15480 1600 380 2560 20000 400 Airdrop 35 2 Comparative Example 2 15480 1600 380 2560 20000 400 Airdrop 35 -
  • the silver powder prepared according to the Examples and Comparative Examples of the present invention was measured using a scanning electron microscope manufactured by JEOL, and the diameter of each of the 100 powders was measured and averaged to measure the SEM size ( ⁇ m). It is shown in Table 2 below. In addition, SEM images of silver powders prepared according to Examples and Comparative Examples are shown in FIGS. 2 to 7.
  • D90, D10, and D50 mean particle sizes corresponding to 90%, 10%, and 50% of the maximum value in the cumulative distribution of solid particle size, respectively.
  • the span value is small, it means that the distribution of the particle size is narrow, and it can be seen that a silver powder of uniform size was produced.
  • the ratio (D50 / DSEM) of PSA size (D50, ⁇ m) to SEM size (DSEM, ⁇ m) was calculated. It means that the PSA particle size, in which particle size analysis of particles dispersed by light scattering into one particle, is smaller than the particle size measured by SEM imaging, has better dispersion.

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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

La présente invention concerne un procédé de préparation d'une poudre d'argent comprenant : une étape de préparation de solution de réaction (S21) pour préparer une première solution de réaction comprenant un ion argent, de l'ammoniac (NH3) et un sel de métal alcalin d'acide organique et une seconde solution de réaction comprenant un agent réducteur ; et une étape de réduction de sel (S2) comprenant une étape de dépôt (S22) pour acquérir une poudre d'argent en permettant à la première solution de réaction et à la seconde solution de réaction de tomber librement dans l'air et de réagir, une poudre d'argent monodispersée ayant une taille de MEB de 0,3 à 1,3 µm pouvant être acquise par dépôt de la poudre d'argent par le biais du procédé de chute libre d'air moyen.
PCT/KR2019/016204 2018-11-23 2019-11-22 Procédé de preparation de poudre d'argent monodispersée WO2020106120A1 (fr)

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KR1020180146665A KR20200061193A (ko) 2018-11-23 2018-11-23 단분산 은 분말의 제조방법
KR10-2018-0146665 2018-11-23

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115555575A (zh) * 2022-09-21 2023-01-03 安徽格派锂电循环科技有限公司 一种利用热喷雾法制备纳米钴颗粒的方法

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JPS5925350B2 (ja) * 1980-06-13 1984-06-16 日立化成工業株式会社 電機用ブラシ
KR970025799A (ko) * 1995-11-02 1997-06-24 김화중 은 분말의 제조방법
JP2008050697A (ja) * 2006-07-28 2008-03-06 Mitsubishi Materials Corp 銀微粒子とその製造方法および製造装置
JP2010236007A (ja) * 2009-03-31 2010-10-21 Mitsubishi Materials Corp 球状銀粒子及び該銀粒子の製造方法並びに製造装置
KR20180047529A (ko) * 2016-10-31 2018-05-10 엘에스니꼬동제련 주식회사 은 분말 및 이의 제조방법

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KR20010107101A (ko) 2000-05-25 2001-12-07 윤종용 반도체 소자의 금속 배선 형성 방법

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Publication number Priority date Publication date Assignee Title
JPS5925350B2 (ja) * 1980-06-13 1984-06-16 日立化成工業株式会社 電機用ブラシ
KR970025799A (ko) * 1995-11-02 1997-06-24 김화중 은 분말의 제조방법
JP2008050697A (ja) * 2006-07-28 2008-03-06 Mitsubishi Materials Corp 銀微粒子とその製造方法および製造装置
JP2010236007A (ja) * 2009-03-31 2010-10-21 Mitsubishi Materials Corp 球状銀粒子及び該銀粒子の製造方法並びに製造装置
KR20180047529A (ko) * 2016-10-31 2018-05-10 엘에스니꼬동제련 주식회사 은 분말 및 이의 제조방법

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115555575A (zh) * 2022-09-21 2023-01-03 安徽格派锂电循环科技有限公司 一种利用热喷雾法制备纳米钴颗粒的方法
CN115555575B (zh) * 2022-09-21 2024-03-29 安徽格派锂电循环科技有限公司 一种利用热喷雾法制备纳米钴颗粒的方法

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TW202030033A (zh) 2020-08-16

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