WO2017043837A1 - Procédé de préparation de poudre d'argent au moyen de grains d'argent - Google Patents

Procédé de préparation de poudre d'argent au moyen de grains d'argent Download PDF

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Publication number
WO2017043837A1
WO2017043837A1 PCT/KR2016/009970 KR2016009970W WO2017043837A1 WO 2017043837 A1 WO2017043837 A1 WO 2017043837A1 KR 2016009970 W KR2016009970 W KR 2016009970W WO 2017043837 A1 WO2017043837 A1 WO 2017043837A1
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silver
solution
silver nitrate
nitric acid
reaction solution
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PCT/KR2016/009970
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English (en)
Korean (ko)
Inventor
이창근
진우민
권태현
우상덕
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엘에스니꼬동제련 주식회사
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Publication of WO2017043837A1 publication Critical patent/WO2017043837A1/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

Definitions

  • the present invention relates to a method for producing silver powder for conductive paste used in electronic components such as solar cell electrodes, internal electrodes of multilayer capacitors, conductor patterns of circuit boards, and the like.
  • a conductive metal paste is a paste in which electricity flows in a dried coating film having a coating ability capable of forming a coating film.
  • a conductive metal paste is a fluid composition in which a conductive filler (metal filler) is dispersed in a vehicle composed of a resin binder and a solvent. It is widely used for forming external electrodes of
  • the silver paste (Silver Paste) is the most chemically stable and excellent conductivity among the composite-based conductive paste has a wide range of applications in a variety of fields, such as for conductive adhesion and coating, and the formation of microcircuits.
  • silver paste is used in various ways, such as silver through hole (STH), adhesive or coating material.
  • Conventional silver powder is prepared by dissolving a silver ingot having a purity of 99.99% in nitric acid, adjusting the pH to 10-11, and reducing and precipitation by adding a reducing agent.
  • the current forms of silver commonly traded in the industry can be broadly divided into granules and ingots.
  • Granules refer to spherical particles having a diameter of 2 to 8 mm, and are manufactured by dropping molten silver into water to form spherical grains.
  • Ingots are produced by casting silver in the same molten state using a hexahedral mold.
  • the international standard sets 30Kg ingots as standard, but in some cases granules are preferred for the user's convenience.
  • silver powder may be used as a disadvantage in a silver powder manufacturing process for preparing a silver nitrate compound using nitric acid. This is because silver (Granule, Ingot) processed in the form of reducing specific surface area in order to minimize volume during storage and transportation has a small reaction area with silver nitrate, which takes a long time to prepare silver nitrate compounds.
  • the present inventors have conceived a fast and economical process by applying silver now in the form of silver grains having a specific surface area larger than granules and ingots and having the same properties as impurities.
  • the inventors of the present invention have come up with a process that can control the particle size of the silver powder to be deposited by applying a concentration step in the process of producing a silver salt for depositing the silver powder.
  • the present invention is to solve the above problems as a silver powder manufacturing method, by producing a silver salt using silver lip provides a fast, economical method for producing silver powder, silver powder precipitated by applying a concentration process It is to provide a method for producing a silver powder that can control the particle size of.
  • a silver powder manufacturing method comprising ;; silver salt manufacturing step (S1) comprising a silver nitrate concentration step (S12) to obtain a concentrated silver nitrate solution by removing.
  • the silver nitrate manufacturing step (S11) is characterized in that the step of producing a silver nitrate solution so that the nitric acid (HNO 3 ) to 100 to 300 parts by weight based on 100 parts by weight of silver (Ag).
  • the silver nitrate manufacturing step (S11) is characterized in that the step of dissolving the silver (Ag) lip in the nitric acid (HNO 3 ) solution at a temperature of 40 to 80 °C.
  • the concentrated nitric acid is characterized in that the step of adjusting the pH of the solution to 0.1 to 5.0.
  • the silver nitrate concentration step (S12) is characterized in that the step of obtaining a concentrated silver nitrate solution by heating to a temperature of 90 to 150 °C.
  • the present invention after the silver salt manufacturing step (S1), the reaction solution production step (S21) for preparing a second reaction solution containing the first reaction solution containing the concentrated silver nitrate solution and ammonia, and a reducing agent and It provides a silver powder production method further comprising; silver salt reduction step (S2) comprising a precipitation step (S22) of reacting the first reaction solution and the second reaction solution to obtain a silver powder.
  • reaction solution preparing step (S21) is a step of preparing the first reaction solution so that ammonia is dissolved in 30 to 50ml per 100g of silver nitrate, and the second reaction solution is prepared to include 40 to 60g of reducing agent per 100g of nitric acid It is characterized by that.
  • the reducing agent is characterized in that at least one member selected from the group consisting of hydroquinone, ascorbic acid, alkanolamine, hydrazine and formalin.
  • the present invention is prepared by selecting the concentrated silver nitrate solution in the pH range 0.1 to 5.5 when the first reaction solution in the reaction solution production step (S21), the average particle size of the silver powder precipitated in the precipitation step (S22) It provides a method for producing a silver powder to adjust to 0.1 to 2.0 ⁇ m.
  • silver (Ag) granules having a large specific surface area and excess nitric acid are used to dissolve the silver granules in nitric acid at a fast reaction rate, thereby reducing the production time of the nitrate and reducing the operating time of the equipment, thereby maintaining the reaction conditions such as temperature. It is possible to provide an economical method for producing silver powder by reducing the use of energy.
  • the pH of the silver nitrate solution can be easily adjusted through the process of concentrating the silver nitrate solution prepared using the excess nitric acid, thereby controlling the particle size of the finally produced silver powder.
  • the dispersant for controlling the particle size when added, it may act as an impurity when used in the conductive paste to inhibit the electrical conductivity, the present invention can effectively control the particle size without addition of the dispersant.
  • 1 is a graph showing the relationship between the specific surface area and the dissolution time.
  • Figure 3 shows the relationship between the pH and particle size of nitric acid according to an embodiment of the present invention.
  • Method for producing a silver powder according to an embodiment of the present invention is a silver salt manufacturing step (S1); Silver salt reduction step (S2); Purification step such as filtration and washing (S3); And a surface treatment step (S4).
  • the method for producing silver powder according to the present invention necessarily includes a silver salt preparation step (S1) and a silver salt reduction step (S2), and other steps may be omitted.
  • Silver salt preparation step (S1) can be prepared by the silver nitrate manufacturing step (S11) to dissolve the silver lip in the nitric acid solution to prepare a silver nitrate solution, and the prepared silver nitrate The silver nitrate may be further prepared by heating the solution to remove the nitric acid, thereby obtaining a silver nitrate solution.
  • Silver nitrate manufacturing step (S11) is a step of preparing a silver salt by dissolving the silver lip in the acid in the current form.
  • Silver lip refers to silver flakes in the form of twigs, and silver lip having a length of 1 to 10 mm generated in an electrorefining process to increase the purity of the non-ferrous metal smelting process can be used.
  • the silver lip uses silver (Ag) lip having a specific surface area of 0.001 to 0.01 m 2 / g.
  • the use of silver particles with a specific surface area of less than 0.001m 2 / g slows down the reaction time and increases the process time, increasing the operating time of the equipment, and using too much energy to maintain the temperature. There is a problem that the yield is lowered due to stagnation. As the specific surface area increases, the contact area with the nitric acid solution is wider, so that a quick dissolution reaction occurs, and thus the dissolution time can be shortened by 10 times or more compared with the ingot.
  • the silver lip is dissolved in an acid solution, especially a nitric acid (HNO 3 ) solution, to prepare a silver nitrate solution.
  • an acid solution especially a nitric acid (HNO 3 ) solution
  • the silver granules and the nitric acid solution are reacted by metering so that 100 parts by weight of silver (Ag) is dissolved in 100 to 300 parts by weight of nitric acid (HNO 3 ).
  • This can lead to faster reaction times and induce sufficient dissolution using nitric acid above the reaction equivalent required to dissolve Ag (Ag).
  • the prepared nitric acid will be contained in excess of nitric acid in the solution, which has the effect that the pH can be easily adjusted in the concentration step (S12) is nitric acid to be described later.
  • the added silver granules When the content of nitric acid is less than 100 parts by weight, the added silver granules have a slow dissolution rate, which increases the processing time and is insufficient to dissolve the injected silver granules. If the amount exceeds 300 parts by weight, the dissolution rate may be increased, but excessive NOx gas may be generated during the concentration reaction due to the addition of nitric acid, which causes an increase in the environmental treatment cost. Therefore, more preferably, it is preferable to react by metering so that 100 parts by weight of silver is dissolved in 170 to 230 parts by weight of nitric acid. For nitric acid solution, 30% solution is recommended.
  • Silver nitrate manufacturing step (S11) is preferably dissolved in the silver (Ag) granules in the nitric acid (HNO 3 ) solution at a temperature of 40 °C to 80 °C.
  • the reaction rate can be increased by applying an appropriate temperature when dissolving a metal in an acid.
  • the reaction temperature is less than 40 °C has a problem that the speed of dissolving the silver is slow, if the reaction temperature is higher than 80 °C because the solution is boiled in the reactor, there is a problem to reduce the input speed of the silver. Therefore, it is more preferable to dissolve at 60 to 70 ° C.
  • Concentrating the silver nitrate (S12) is a step of concentrating the silver nitrate solution by removing the nitric acid from the silver nitrate solution prepared using the silver lip.
  • the silver nitrate solution can be heated to remove the nitric acid by vaporization.
  • the nitric acid solution has a low pH value of 1 or less due to excessive addition of nitric acid.
  • the silver nitrate according to the present invention can easily adjust the pH of silver nitrate through the concentration step (S12), and pH It is possible to easily control the particle size of the finally produced silver powder by controlling the.
  • concentration (a) is changed in the range of 0.1 to 80%.
  • the concentrated silver nitrate was added to distilled water until the volume before concentration was adjusted to adjust the silver concentration in silver nitrate to prepare a silver nitrate solution.
  • the concentrated nitric acid can thereby adjust the pH value of the solution in the range of 0.1 to 5.5.
  • the pH value is increased, thereby controlling the particle size.
  • the higher the pH value the smaller the size of the silver powder can be produced.
  • Silver powder of desired size can be prepared within an average particle size range of 0.1 to 2.0 ⁇ m.
  • Silver salt reduction step (S2) is a step of depositing silver particles by reducing the silver ions by adding a reducing agent and ammonia to the silver salt solution, silver ions, ammonia and nitric acid It includes a reaction solution manufacturing step (S21) for producing a second reaction solution containing a first reaction solution and a reducing agent including and a precipitation step (S22) of reacting the first reaction solution and the second reaction solution to obtain a silver powder. .
  • the silver salt solution may be a concentrated silver nitrate solution, which is a silver salt prepared through the silver salt preparation step (S1) according to an embodiment of the present invention, and may also use a commercially available silver nitrate, silver salt complex or silver intermediate solution. have.
  • reaction solution preparation step (S21) ammonia is added to the silver nitrate solution, and stirred to dissolve to prepare a first reaction solution.
  • nitric acid is further added to prepare a first reaction solution.
  • concentration of silver ions included is not limited but may be in the range of 6 g / L to 40 g / L. If it is less than 6g / L yield is low economic problem, and if more than 40g / L there is a problem that causes the aggregation of the powder.
  • the first reaction solution was prepared by weighing silver nitrate to dissolve 30 to 50 ml of ammonia per 100 g of silver nitrate.
  • ammonia When ammonia is added below 30ml / 100gAgNO 3 , ammonia lacks ammonia in the complex salting reaction to produce silver oxide.
  • ammonia When ammonia is added above 50ml / 100gAgNO 3, the size of silver powder produced is large. There is a decreasing problem. At this time, it is preferable to use industrial 25% aqueous ammonia solution.
  • the amount of nitric acid is preferably added in an amount of 20 to 230 parts by weight based on 100 parts by weight of silver ions. If the nitric acid is added in excess of 230 parts by weight, the size (size) and organic matter content of the prepared silver powder is greatly increased, and the reduction reaction of silver ions is not completed due to the low pH, thereby greatly reducing the recovery rate.
  • the first reaction solution containing silver ions, ammonia, and nitric acid may be prepared in an aqueous state by adding silver nitrate solution and aqueous ammonia solution to a solvent such as water and stirring the solution, or adding silver ions, aqueous ammonia solution, and nitric acid solution, stirring, and dissolving the solution. It may also be prepared in the form of a slurry.
  • Reaction liquid preparation step (S21) according to an embodiment of the present invention also prepares a second reaction liquid containing a reducing agent.
  • the reducing agent may be at least one selected from the group consisting of ascorbic acid, alkanolamine, hydroquinone, hydrazine and formalin, and among these, hydroquinone may be preferably selected.
  • the second reaction solution is prepared by weighing the reducing agent in an amount of 40 to 60 g per 100 g of silver nitrate included in the first reaction solution when the silver nitrate solution is used, and 100 weight of silver ions when using a silver salt or silver intermediate solution. It is preferable to prepare to include from 40 to 60 parts by weight relative to the part. When the reducing agent is used below the above range, all of the silver ions may not be reduced, and when used beyond the above range, the organic content may increase, which may be a problem.
  • the second reaction solution containing a reducing agent may be prepared in an aqueous solution state by adding a reducing agent to a solvent such as water and stirring the solution.
  • Precipitation step (S22) is a step of obtaining a silver powder by reacting the first reaction solution and the second reaction solution, stirring the first reaction solution prepared by the reaction solution preparation step (S21)
  • the second reaction liquid can be slowly added dropwise or added in a batch to react.
  • the batch reaction may be completed in a short time to collectively add the bulk to prevent aggregation of the particles and to improve dispersibility.
  • dispersant examples include fatty acids, fatty acid salts, surfactants, organometallics, chelate formers and protective colloids.
  • the dispersant for controlling the particle size when added, it can act as an impurity when used in the conductive paste to inhibit the electrical conductivity, the present invention has the advantage that can effectively control the particle size without addition of the dispersant .
  • Purification step (S3) is a silver salt reduction step (S2) after completing the silver particle precipitation reaction to remove and wash the silver powder dispersed in an aqueous solution or slurry using filtration and the like Step S31 is included. More specifically, after the silver particles in the silver powder dispersion are precipitated, the supernatant of the dispersion is discarded and filtered using a centrifuge, and the filter medium is washed with pure water. In addition to the centrifuge mentioned in the present invention, the application of various methods for solid-liquid separation such as filter press and decanter is not excluded from the scope of the right. The washing process is performed by completely removing the washing water from which the powder has been washed. Therefore, the water content is reduced to less than 10%. It is also possible to optionally add the aforementioned dispersants to the reaction complete solution prior to filtration to prevent aggregation of the silver powder.
  • the purification step (S3) may further comprise a drying and disintegration step (S34) after washing.
  • Surface treatment step (S4) is a step of hydrophobizing the hydrophilic surface of the silver powder, it may be made selectively. More specifically, after controlling the moisture content of the wet cake (wet cake) obtained after filtration to less than 10% can be added to the surface treatment agent for the surface treatment of the silver powder and the moisture content can be adjusted to 70% to 85%. Thereafter, silver powder can be obtained through drying and pulverization. When surface treatment of silver powder, the powder should be well dispersed, and the surface treatment is sufficient. If the water content is low, the dispersion efficiency is poor, so it is better to surface-treat a certain amount with water content.
  • Silver powder prepared according to an embodiment of the present invention by measuring the diameter size of each of the 100 powders by using a scanning electron microscope (SEM) and the average size measured within the range of 0.1um to 2.0um,
  • SEM scanning electron microscope
  • the organic matter content measured by TGA analysis in the range from normal temperature to 500 degreeC at the temperature increase rate of 10 degreeC / min is 1.0 weight% or less.
  • Example 1 Silver Crystal 0.0058 605 Comparative Example 1 Silver Granule 0.00017 2890 Comparative Example 2 Silver Ingot 0.00038 6060
  • Example 1 in which silver particles having a specific surface area of 0.0058 m 2 / g were dissolved in the same nitric acid solution, 0.00017 m 2 / g of Comparative Example 1 was four times or more than the silver granule of Comparative Example 2, and 0.00038 of Comparative Example 2 m 2 / g of silver can reduce the dissolution time by more than 10 times than the ingot.
  • 1 is a graph showing the relationship between the specific surface area and the dissolution time.
  • Example 2 Silver Nitrate Concentration (%) Silver Nitrate pH Example 2 0.1 0.4 Example 3 15.8 0.8 Example 4 46 1.6 Example 5 60 2 Example 6 67 3.9 Example 7 77.5 5.1
  • the pH of the silver nitrate solution can be easily adjusted from 0.4 to 5.1 by adjusting the concentration of nitric acid from 0.1% to 77.5%, and in FIG. 2, the relationship between the concentration of nitric acid and pH is shown. .
  • the 1st aqueous solution was made to stir, the 2nd aqueous solution was added collectively to this 1st aqueous solution, and further stirred for 5 minutes after completion
  • stirring was stopped the particles in the mixed solution were allowed to settle, the supernatant of the mixed solution was discarded, the mixed solution was filtered using a centrifuge, the media was washed with pure water, dried, and silver powder was obtained.
  • the SEM size was measured by measuring the diameter size of each of 100 powders using a scanning electron microscope manufactured by JEOL, and the results are shown in Table 3.
  • Example 8 Used silver nitrate Silver Nitrate pH SEM size (m)
  • Example 8 Example 2 0.4 1.6
  • Example 9 Example 3 0.8 1.5
  • Example 10 Example 4 1.6 1.3
  • Example 11 Example 5 2 One
  • Example 12 Example 6 3.9 0.8
  • Example 13 Example 7 5.1 0.6
  • each particle size was prepared from 1.6 ⁇ m to 0.6 ⁇ m using silver nitrate having a pH value of 0.4 to 5.1, and FIG. Indicated.

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  • Chemical & Material Sciences (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, le procédé comprenant une étape de préparation de sel d'argent (S1) comprenant : une étape de préparation de nitrate d'argent (S11) destinée à dissoudre des grains d'argent (Ag) ayant une surface spécifique de 0,001 à 0,01 m2/g dans une solution d'acide nitrique (HNO3), de sorte à préparer une solution de nitrate d'argent ; et une étape de concentration de nitrate d'argent (S12) destinée à chauffer la solution de nitrate d'argent préparée afin d'éliminer l'acide nitrique, ce qui permet d'obtenir une solution concentrée de nitrate d'argent. L'invention apporte un procédé de préparation rapide et économique par la préparation d'un sel d'argent au moyen de grains d'argent, et elle apporte un procédé de préparation capable de réguler la taille des particules d'une poudre d'argent précipitée par l'application d'un traitement de concentration.
PCT/KR2016/009970 2015-09-10 2016-09-06 Procédé de préparation de poudre d'argent au moyen de grains d'argent WO2017043837A1 (fr)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114160803A (zh) * 2021-11-17 2022-03-11 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） 一种高分散性球状金粉的高效制备方法
CN115780824A (zh) * 2023-01-29 2023-03-14 苏州银瑞光电材料科技有限公司 一种高烧结活性银粉的制备方法及应用

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KR102017177B1 (ko) * 2019-05-02 2019-09-02 파워팩 주식회사 습식공정을 이용한 고순도 은 나노 분말의 제조 방법
KR102023711B1 (ko) * 2019-05-02 2019-11-04 파워팩 주식회사 특정 온도에서 경도가 향상되는 고순도의 은 나노 분말
WO2020222542A1 (fr) * 2019-05-02 2020-11-05 파워팩 주식회사 Nanopoudre d'argent à stabilité à l'oxydation améliorée préparée par traitement humide et son procédé de préparation
KR102023714B1 (ko) * 2019-05-15 2019-11-04 파워팩 주식회사 습식공정에 의해 제조되는 산화 안정성이 향상된 은 나노 분말

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US5000928A (en) * 1986-03-17 1991-03-19 Eastman Kodak Company Preparation of ultra-pure silver nitrate
KR100713662B1 (ko) * 2005-10-20 2007-05-02 한국지질자원연구원 은 스크랩으로부터 구상 은분말 제조방법
KR20090045508A (ko) * 2007-11-02 2009-05-08 주식회사 지오션 더블-제트형 연속식 용액환원에 의해 은 분말을 제조하기위한 장치 및 방법
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114160803A (zh) * 2021-11-17 2022-03-11 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） 一种高分散性球状金粉的高效制备方法
CN115780824A (zh) * 2023-01-29 2023-03-14 苏州银瑞光电材料科技有限公司 一种高烧结活性银粉的制备方法及应用

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