KR20170030929A - The manufacturing method of silver - Google Patents
The manufacturing method of silver Download PDFInfo
- Publication number
- KR20170030929A KR20170030929A KR1020150128477A KR20150128477A KR20170030929A KR 20170030929 A KR20170030929 A KR 20170030929A KR 1020150128477 A KR1020150128477 A KR 1020150128477A KR 20150128477 A KR20150128477 A KR 20150128477A KR 20170030929 A KR20170030929 A KR 20170030929A
- Authority
- KR
- South Korea
- Prior art keywords
- silver
- washing
- solution
- parts
- weight
- Prior art date
Links
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
-
- B22F1/0059—
-
- 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
Abstract
The present invention relates to a silver salt reducing step (S2) of adding a reducing agent and ammonia to a silver salt solution to precipitate silver particles; And a purifying step (S3) of purifying the precipitated silver particles by preparing a washing liquid containing ethanol and pure water. The present invention relates to a method for producing silver powder, which comprises p-benzoquinone in silver powder It is possible to provide an optimum ratio of wash water that can minimize the organic matter content.
Description
The present invention relates to a method for producing a silver powder for a conductive paste, which is used for an electrode for a solar cell, an internal electrode of a multilayer capacitor, and a conductor pattern of a circuit board.
The conductive metal paste is a paste in which a conductive film (film) is formed and a conductive paste (metal filler) is dispersed in a vehicle composed of a resin binder and a solvent. And the like.
In particular, Silver Paste is the most chemically stable and excellent in conductivity among the conductive paste of composite system, and has a wide range of applications in various fields such as conductive bonding and coating and fine circuit formation. BACKGROUND ART [0002] The use of silver paste has been widely used for STH (Silver Through Hole), adhesive, or coating materials in electronic parts, such as PCBs (Printed Circuit Boards), where reliability is particularly important.
Generally, in the method for producing silver powder according to the wet method, a slurry in which precipitated silver powder is dispersed can be obtained. As a method of producing the silver powder according to the wet method, for example, an organic reducing agent is added to a silver nitrate solution to obtain a slurry in which silver powder is dispersed by reducing and precipitating silver powder, and the silver powder slurry is dried The silver powder is recovered.
Conventionally, in the process of dewatering and drying silver powder slurry, conventionally, a silver powder slurry is filtered and dehydrated and then dried (air drying), hot-air drying, vacuum drying And the dried product is shredded to recover the silver powder.
However, when the silver powder is precipitated using an organic reducing agent and the silver powder is simply dewatered and dried, the organic material remains on the surface of the powder, and when the organic material content is high, the electric conductivity is lowered in the final application have.
Conventionally, alkaline water can be used to wash an organic matter effectively. However, since a component such as potassium (K) and sodium (Na) contained in alkaline water remains in silver powder and is used as an electrode or the like, There is a problem in that it is economically disadvantageous.
Accordingly, the inventors of the present invention have focused on a process capable of removing an organic matter of silver powder to be precipitated with high efficiency by precipitating silver powder and applying a washing process using ethanol.
Disclosure of Invention Technical Problem [8] The present invention provides a method of manufacturing a silver powder capable of facilitating the washing of an organic matter generated during reduction (precipitation) of a silver powder .
However, the objects of the present invention are not limited to the above-mentioned objects, and other objects not mentioned can be clearly understood by those skilled in the art from the following description.
The present invention relates to a silver salt reducing step (S2) of adding a reducing agent and ammonia to a silver salt solution to precipitate silver particles; And a washing step (S31) of washing the precipitated silver particles by preparing a washing liquid containing ethanol and pure water.
The washing step (S31) is a step of preparing the washing solution so that the ethanol is contained in an amount of 40 to 60 parts by weight based on 100 parts by weight of the washing solution.
The washing step (S31) is a step of preparing a washing solution so that the ethanol is contained in an amount of 50 parts by weight with respect to 100 parts by weight of the washing solution.
The washing step (S31) is a step of washing 30 to 40 parts by weight of the silver particles using 100 parts by weight of the washing solution.
Further, the purification step (S3) further comprises a drying step (S32) of recovering the silver particles washed through the washing solution and drying at 70 to 90 DEG C for 5 to 7 hours.
Also, the silver powder prepared by the above silver powder production method is provided with an organic material content of 1.0 wt% or less including p-benzoquinone in silver powder.
When the cleaning method of the present invention is used, it is possible to easily clean the organic material (p-benzoquinone) produced during the production, and thus the silver powder having high purity can be produced, thereby increasing the electrical conductivity of the electrode to be used.
Before describing the present invention in detail, it is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the invention, which is defined solely by the appended claims. shall. All technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art unless otherwise stated.
Throughout this specification and claims, the word "comprise", "comprises", "comprising" means including a stated article, step or group of articles, and steps, , Step, or group of objects, or a group of steps.
On the contrary, the various embodiments of the present invention can be combined with any other embodiments as long as there is no clear counterpoint. Any feature that is specifically or advantageously indicated as being advantageous may be combined with any other feature or feature that is indicated as being preferred or advantageous. Hereinafter, embodiments of the present invention and effects thereof will be described with reference to the accompanying drawings.
A method of manufacturing a silver powder according to an embodiment of the present invention includes: a silver salt producing 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 a silver powder according to the present invention necessarily includes a silver salt reducing step (S2) and a purification step (S3), and the other steps may be omitted.
One. (S1)
The silver salt production step (S1) according to an embodiment of the present invention can produce a silver salt through a silver nitrate silver production step (S11) of dissolving silver lips in a nitric acid solution to produce a silver nitrate solution, The silver salt may be prepared by further including a nitric acid silver concentration step (S12) to obtain a concentrated silver nitrate solution by heating the solution to remove nitric acid.
The silver nitrate silver manufacturing step (S11) according to an embodiment of the present invention is a step of dissolving the silver in the acid in the present embodiment to produce a silver salt. Silver means silver now in the form of a twig. It can be used with silver lips having a length of 1 to 10 mm, which is generated in an electrochemical refining process for increasing the purity in the process of smelting non-ferrous metals.
The silver lips use silver (Ag) lips having a specific surface area of 0.001 to 0.01 m 2 / g. When silver lips with a specific surface area of less than 0.001 m 2 / g are used, the reaction time is slowed to increase the operation time of the equipment due to the increase of the process time, and the energy for maintaining the temperature is excessively used, which is not economical. And the yield is lowered. As the specific surface area increases, the contact area with the nitric acid solution is increased, resulting in a rapid dissolution reaction. As a result, the dissolution time can be shortened by at least 10 times as compared with the ingot. However, in the case of using a silver lip having a specific surface area exceeding 0.01 m 2 / g, it is not easy to handle in the progress of the process, and when the silver is added during the process, There is a problem that the reactor overflow occurs. Therefore, in order to solve this problem, it is more preferable to use silver lips of 0.003 to 0.008 m 2 / g.
The silver lips are dissolved in an acid solution, especially a nitric acid (HNO 3 ) solution to prepare a silver nitrate solution. The silver and the nitric acid solutions are metered and reacted so that 100 parts by weight of silver (Ag) is dissolved in 100 to 300 parts by weight of nitric acid (HNO 3 ). This is because nitric acid equal to or greater than the reaction equivalent necessary for dissolving silver (Ag) can be used to further accelerate the reaction time and induce sufficient dissolution. The prepared silver nitrate silver solution contains an excessive amount of nitric acid, which is effective in easily adjusting the pH in the silver nitrate silver concentration step (S12) described later. When the content of the nitric acid is less than 100 parts by weight, the dissolution rate of the added silver lips is delayed, which increases the processing time and insufficient to dissolve the charged silver lips. If it exceeds 300 parts by weight, the dissolution rate can be increased, but excessive nitric acid may cause excessive NO x gas during the concentration reaction, thereby increasing the environmental treatment cost. Therefore, it is more preferable to conduct the metering so that 100 parts by weight of silver is dissolved in 170 to 230 parts by weight of nitric acid. The nitric acid solution is preferably 30% solution.
The silver nitrate silver production step (S11) preferably dissolves the silver (Ag) grains in the nitric acid (HNO 3 ) solution at a temperature of 40 ° C to 80 ° C. It is generally known that when the metal is dissolved in an acid, the reaction rate can be increased by adding an appropriate temperature. If the reaction temperature is lower than 40 ° C, the dissolution rate of the silver is lowered. If the reaction temperature is higher than 80 ° C, the reaction becomes too fast, and the solution is boiled over in the reactor. Therefore, it is more preferable to dissolve at 60 to 70 占 폚.
The silver nitrate silver concentration step (S12) according to an embodiment of the present invention is a step of concentrating a silver nitrate solution by removing nitric acid from a silver nitrate silver solution prepared using silver lips. The silver nitrate solution can be removed by heating the nitric acid by heating. The pH of the silver nitrate solution can be easily adjusted through the nitric acid silver concentration step (S12) according to the present invention, and the pH of the silver nitrate solution can be easily adjusted by adjusting the pH So that the particle size of the finally prepared silver powder can be easily controlled.
The nitric acid silver concentration step S12 heats the silver nitrate solution to a temperature of 90 to 150 DEG C to remove nitric acid. When the ratio of the volume after heating to the volume before heating of the silver nitrate solution is defined as the concentration (a,%), the concentration (a) is varied in the range of 0.1 to 80%. To the concentrated silver nitrate solution, distilled water is added to the volume before concentration to prepare silver nitrate solution by adjusting the silver concentration in silver nitrate. Whereby the pH value of the concentrated silver nitrate solution can be adjusted in the range of 0.1 to 5.5.
As the concentration of nitric acid is increased by heating, the pH value becomes higher and the particle size can be controlled. The higher the pH value, the smaller the size of the silver powder. Precipitation of silver powder using a first reaction solution containing a silver nitrate solution having a pH value within a range of 0.1 to 5.5 obtained by adjusting the concentration (a) to 0.1 to 80% in a silver salt reducing step (S2) , A silver powder of a desired size can be produced within an average particle size range of from 0.5 [mu] m to 3.0 [mu] m.
2. (S2)
The silver salt reducing step S2 according to an embodiment of the present invention is a step of reducing silver ions by adding a reducing agent and ammonia to a silver salt solution to precipitate silver particles, and silver ions, ammonia, and nitric acid (S21) for producing a second reaction solution containing a first reaction solution containing a reducing agent and a precipitation step (S22) for obtaining a silver powder by reacting the first reaction solution and the second reaction solution .
The silver salt solution may be a concentrated silver nitrate silver solution, which is a silver salt prepared through the silver salt preparation step (S1) according to an embodiment of the present invention. Alternatively, commercially available silver nitrate silver salt complex or silver intermediate solution may be used have.
In the reaction solution preparation step (S21) according to an embodiment of the present invention, ammonia is added to a silver nitrate solution and dissolved by stirring to prepare a first reaction solution. When a silver complex or a silver intermediate solution is used, nitric acid is further added to prepare a first reaction solution. The concentration of the contained silver ions is not limited, but is in the range of 6 g / L to 40 g / L. If it is less than 6 g / L, the yield tends to be low and economical efficiency is problematic. If it exceeds 40 g / L, there is a problem that powder agglomerates.
The reaction solution preparation step (S21) is metered so that ammonia is dissolved in an amount of 30 to 50 ml per 100 g of silver nitrate silver nitrate to prepare a first reaction solution. When ammonia is added in an amount less than 30 ml / 100 gAgNO 3 , ammonia is deficient in ammonia due to lack of ammonia in the complexing reaction, and silver oxide is generated. When ammonia is added in an amount exceeding 50 ml / 100 gAgNO 3, . The ammonia water used in this case is preferably an aqueous 25% ammonia solution for industrial use.
When a silver complex or a silver intermediate solution is used, the amount of nitric acid to be used is preferably 20 to 230 parts by weight based on 100 parts by weight of silver ions. When nitric acid is added in an amount of more than 230 parts by weight, the size and the organic content of the prepared silver powder are greatly increased and the reduction reaction of the silver ions is not completed due to the low pH.
The first reaction solution containing silver ions, ammonia and nitric acid may be prepared by adding a silver nitrate solution and an aqueous ammonia solution to a solvent such as water and stirring or adding an aqueous solution of silver nitrate, an aqueous solution of ammonia and an aqueous solution of nitric acid, And can also be prepared in the form of slurries.
The reaction solution preparation step (S21) according to an embodiment of the present invention also produces a second reaction solution containing a reducing agent.
The reducing agent may be at least one member selected from the group consisting of ascorbic acid, alkanolamine, hydroquinone, hydrazine and formalin, and among them, hydroquinone can be preferably selected. In the case of using a silver nitrate solution, the second reaction solution is prepared by weighing 40 to 60 g of a reducing agent per 100 g of silver nitrate contained in the first reaction solution. When a silver complex or silver intermediate solution is used, And 40 to 60 parts by weight based on 100 parts by weight of the resin. When the reducing agent is used in an amount less than the above range, silver ions may not be all reduced. If the reducing agent is used in excess of the above range, the organic matter content may increase, which may be a problem.
The second reaction solution containing a reducing agent can be prepared in an aqueous solution state by adding a reducing agent to a solvent such as water and dissolving it by stirring.
The precipitation step (S22) according to an embodiment of the present invention is a step of reacting the first reaction solution and the second reaction solution to obtain a silver powder, wherein the first reaction solution produced by the reaction solution production step (S21) The second reaction solution may be slowly added dropwise or may be added in a batch to react. Preferably, the addition of the components in a batch may terminate the reduction reaction in a short period of time, thereby preventing agglomeration of particles and increasing dispersibility.
In the meantime, in the embodiment of the present invention, the addition of the above-mentioned dispersant is not excluded from the scope of right to improve the dispersibility of silver particles and to prevent agglomeration. Examples of the dispersing agent include fatty acids, fatty acid salts, surfactants, organic metals, chelating agents and protective colloids.
However, when a dispersant for controlling the particle size is added, it acts as an impurity when used in a conductive paste, thereby deteriorating the electrical conductivity. According to the present invention, the particle size can be effectively controlled without adding a dispersant .
3. Purification step (S3)
In the refining step S3 according to an embodiment of the present invention, the silver powder dispersed in the aqueous solution or slurry is separated and washed by filtration after completing the silver particle precipitation reaction through the silver salt reducing step S2 And a cleaning step S31.
The washing step S31 according to an embodiment of the present invention is a step of washing the precipitated silver particles by preparing a washing liquid containing ethanol and pure water.
More specifically, after precipitating silver particles in the silver particle dispersion, the supernatant of the dispersion is discarded, filtered using a centrifugal separator, and the filter material is washed with washing water.
The washing step (S31) first produces wash water containing ethanol and pure water. The washing water is prepared so that 40 to 60 parts by weight of ethanol is contained per 100 parts by weight of the washing liquid. Preferably, 50 parts by weight of ethanol is contained per 100 parts by weight of the washing liquid. When the washing water contains less than 40 parts by weight or more than 60 parts by weight of the washing water, it is impossible to purify the organic matter to less than 0.1 wt% by washing within three times as shown in the experimental example to be described later, It is preferable to prepare a washing solution having the above content range.
In the washing step S31, 30 to 40 parts by weight of the silver particles precipitated are washed using 100 parts by weight of the washing solution. When 100 parts by weight of the washing liquid is used to wash silver particles of less than 30 parts by weight, there is a problem in that the cleaning cost is increased compared to the washing efficiency. When 100 parts by weight of the washing liquid is used to wash silver particles in excess of 40 parts by weight, The number of times of cleaning is increased, and the cleaning cost is increased.
The washing step (S31) is completed after completely removing the washing water from which the silver particles have been washed. If the water content is less than approximately 10%, the wash water is considered to be completely removed. It is also possible to prevent agglomeration of the silver powder by optionally adding the above-mentioned dispersant to the reaction-completed solution before filtration.
Further, the purification step S3 according to an embodiment of the present invention may further include a drying step (S32) for drying after washing. The drying step (S32) is a step of recovering the silver particles washed through the washing liquid and drying at 70 to 90 DEG C for 5 to 7 hours.
Further, the purification step S3 according to an embodiment of the present invention may further include a smoothing step (S33) of smashing the silver particles after drying.
4. In the surface treatment step (S4)
The surface treatment step S4 according to an embodiment of the present invention is a step of hydrophobizing the hydrophilic surface of the silver powder, and may be selectively performed. More specifically, after adjusting the moisture content of the wet cake obtained after filtration to less than 10%, a surface treating agent may be added to the surface of the powder to adjust the water content to 70% to 85%. After that, the silver powder can be obtained through drying and decolorizing process. When the powder is surface-treated, the powder should be well dispersed to achieve sufficient surface treatment. If the water content is low, the dispersion efficiency is lowered.
The silver powder prepared according to an embodiment of the present invention has a size of 0.5 to 3.0 .mu.m, which is measured by measuring a diameter of each of 100 powders using a scanning electron microscope (SEM) The content of organic substances including p-benzoquinone measured by performing TGA analysis at a temperature raising rate of 10 占 폚 / min from room temperature to 500 占 폚 is 1.0% by weight or less.
Examples and Experimental Examples
≪ Precipitation of silver powder &
10 ml of pure water and 60% of industrial nitric acid were weighed to prepare a 30% nitric acid solution, and the mixture was heated and stirred at 60 ° C to prepare an acid solution. 5 g of a silver lip having a specific surface area of 0.0058 m 2 / g was dissolved at a rate of 1 kg / min while the flow of the acid solution was smooth through the stirring.
The silver nitrate solution was concentrated so that the ratio of the volume of the silver nitrate solution to the volume of the silver nitrate solution after heating to the volume of the silver nitrate solution before heating was heated to 150 DEG C while stirring the silver nitrate solution completely melted at 60 DEG C . The pH value of the concentrated silver nitrate solution was 3.9.
22 mL of concentrated silver nitrate solution and 17.6 mL of ammonia (concentration 25%) were added to 960.4 g of pure water at room temperature and dissolved by stirring to prepare a first aqueous solution. On the other hand, 5.5 g of hydroquinone was added to 1000 g of pure water at room temperature and dissolved by stirring to prepare a second aqueous solution.
Subsequently, the first aqueous solution was stirred, and the second aqueous solution was added all at once to the first aqueous solution, and the mixture was further stirred for 5 minutes from the completion of the addition to grow particles in the mixed solution. After that, stirring was stopped and the silver particles and the reaction solution were subjected to solid-liquid separation using a centrifugal separator.
<Cleaning of Silver Particles>
(1) Example 1
400 g of ethanol and 600 g of pure water were mixed to prepare 1 kg of washing solution. 350 g of the separated silver particles and 1 kg of the washing solution were added and stirred thoroughly, and the silver particles were recovered through centrifugation. The silver powder was recovered while increasing the number of washing cycles, dried in a hot air drier at 80 ° C for 6 hours, and the organic content determined through a thermogravimetric analyzer is shown in Table 1.
(2) Example 2
500 g of ethanol and 500 g of pure water were mixed to prepare 1 kg of washing solution. 350 g of the separated silver particles and 1 kg of the washing solution were added and stirred thoroughly, and the silver particles were recovered through centrifugation. The silver powder was recovered while increasing the number of washing cycles, dried in a hot air drier at 80 ° C for 6 hours, and the organic content determined through a thermogravimetric analyzer is shown in Table 1.
(3) Example 3
600 g of ethanol and 400 g of pure water were mixed to prepare 1 kg of washing solution. 350 g of the separated silver particles and 1 kg of the washing solution were added and stirred thoroughly, and the silver particles were recovered through centrifugation. The silver powder was recovered while increasing the number of washing cycles, dried in a hot air drier at 80 ° C for 6 hours, and the organic content determined through a thermogravimetric analyzer is shown in Table 1.
(4) Comparative Example 1
The silver particles solid-liquid separated from the reaction solution using the centrifugal separator were dried in a hot-air drier at 80 ° C for 6 hours without washing, and the organic content determined through a thermogravimetric analyzer is shown in Table 1.
(5) Comparative Example 2
350 g of the separated silver particles and 1 kg of ethanol were added and thoroughly stirred. Then, the silver particles were recovered through centrifugal separation. The silver powder was recovered while increasing the number of washing cycles, dried in a hot air drier at 80 ° C for 6 hours, and the organic content determined through a thermogravimetric analyzer is shown in Table 1.
(6) Comparative Example 3
350 g of the separated silver particles and 1 kg of pure water were added and thoroughly stirred. Then, the silver particles were recovered through centrifugation. The silver powder was recovered while increasing the number of washing cycles, dried in a hot air drier at 80 ° C for 6 hours, and the organic content determined through a thermogravimetric analyzer is shown in Table 1.
(7) Comparative Example 4
300 g of ethanol and 700 g of pure water were mixed to prepare 1 kg of washing solution. 350 g of the separated silver particles and 1 kg of the washing solution were added and stirred thoroughly, and the silver particles were recovered through centrifugation. The silver powder was recovered while increasing the number of washing cycles, dried in a hot air drier at 80 ° C for 6 hours, and the organic content determined through a thermogravimetric analyzer is shown in Table 1.
(8) Comparative Example 5
700 g of ethanol and 300 g of pure water were mixed to prepare 1 kg of washing solution. 350 g of the separated silver particles and 1 kg of the washing solution were added and stirred thoroughly, and the silver particles were recovered through centrifugation. The silver powder was recovered while increasing the number of washing cycles, dried in a hot air drier at 80 ° C for 6 hours, and the organic content determined through a thermogravimetric analyzer is shown in Table 1.
(9) Comparative Example 6
800 g of ethanol and 200 g of pure water were mixed to prepare 1 kg of washing solution. 350 g of the separated silver particles and 1 kg of the washing solution were added and stirred thoroughly, and the silver particles were recovered through centrifugation. The silver powder was recovered while increasing the number of washing cycles, dried in a hot air drier at 80 ° C for 6 hours, and the organic content determined through a thermogravimetric analyzer is shown in Table 1.
(10) Comparative Example 7
900 g of ethanol and 100 g of pure water were mixed to prepare 1 kg of washing solution. 350 g of the separated silver particles and 1 kg of the washing solution were added and stirred thoroughly, and the silver particles were recovered through centrifugation. The silver powder was recovered while increasing the number of washing cycles, dried in a hot air drier at 80 ° C for 6 hours, and the organic content determined through a thermogravimetric analyzer is shown in Table 1.
As shown in Table 1, the ratio of ethanol in which the reduction of organic matter is maximized before cleaning is 40% to 60% of the pure water in Examples 1 to 3, Which is 50% of the pure water.
The features, structures, effects, and the like illustrated in the above-described embodiments can be combined and modified in other embodiments by those skilled in the art to which the embodiments belong. Therefore, it should be understood that the present invention is not limited to these combinations and modifications.
Claims (6)
And a washing step (S31) of washing the precipitated silver particles by preparing a washing liquid containing ethanol and pure water.
Wherein the washing step S31 is a step of preparing a washing solution such that the ethanol is included in an amount of 40 to 60 parts by weight based on 100 parts by weight of the washing solution.
Wherein the washing step S31 is a step of preparing a washing solution so that the ethanol is contained in an amount of 50 parts by weight with respect to 100 parts by weight of the washing solution.
Wherein the washing step (S31) is a step of washing 30 to 40 parts by weight of the silver particles using 100 parts by weight of the washing liquid.
Wherein the purifying step (S3) further comprises a drying step (S32) of recovering the silver particles washed through the washing solution and drying the silver particles at 70 to 90 DEG C for 5 to 7 hours.
A silver powder having an organic content of 1.0 wt% or less including p-benzoquinone in the silver powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020150128477A KR20170030929A (en) | 2015-09-10 | 2015-09-10 | The manufacturing method of silver |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020150128477A KR20170030929A (en) | 2015-09-10 | 2015-09-10 | The manufacturing method of silver |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| KR20170030929A true KR20170030929A (en) | 2017-03-20 |
Family
ID=58502773
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| KR1020150128477A KR20170030929A (en) | 2015-09-10 | 2015-09-10 | The manufacturing method of silver |
Country Status (1)
| Country | Link |
|---|---|
| KR (1) | KR20170030929A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019074336A1 (en) * | 2017-10-13 | 2019-04-18 | 엘에스니꼬동제련 주식회사 | Method for preparing silver powder having improved dispersibility |
| KR20190048317A (en) * | 2017-10-31 | 2019-05-09 | 엘에스니꼬동제련 주식회사 | The manufacturing method of silver |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101244201B1 (en) | 2005-02-02 | 2013-03-18 | 도와 일렉트로닉스 가부시키가이샤 | Silver particle powder and process for producing the same |
-
2015
- 2015-09-10 KR KR1020150128477A patent/KR20170030929A/en active Search and Examination
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101244201B1 (en) | 2005-02-02 | 2013-03-18 | 도와 일렉트로닉스 가부시키가이샤 | Silver particle powder and process for producing the same |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019074336A1 (en) * | 2017-10-13 | 2019-04-18 | 엘에스니꼬동제련 주식회사 | Method for preparing silver powder having improved dispersibility |
| KR20190041592A (en) * | 2017-10-13 | 2019-04-23 | 엘에스니꼬동제련 주식회사 | The manufacturing method of silver powder with improved dispersibility |
| KR20190048317A (en) * | 2017-10-31 | 2019-05-09 | 엘에스니꼬동제련 주식회사 | The manufacturing method of silver |
| WO2019088510A1 (en) * | 2017-10-31 | 2019-05-09 | 엘에스니꼬동제련 주식회사 | Method for producing silver powder |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101764218B1 (en) | The manufacturing method of silver powder using the silver crystal | |
| KR101927476B1 (en) | Silver powder and manufacturing method of the same | |
| JP4821014B2 (en) | Copper powder manufacturing method | |
| JP2018523758A (en) | Method for producing silver powder for high-temperature sintered conductive paste | |
| KR101800605B1 (en) | The manufacturing method of silver powder | |
| CN103624267A (en) | Method for preparing silver powder in continuous mode | |
| KR101733169B1 (en) | silver particles and manufacturing method thereof | |
| CN104843770A (en) | Method of resource utilization of tin sludge | |
| KR101905033B1 (en) | silver powder and manufacturing method of the same | |
| KR101764219B1 (en) | The manufacturing method of silver powder | |
| KR20170030929A (en) | The manufacturing method of silver | |
| KR100851815B1 (en) | A method of preparing nano silver powder | |
| JP5803830B2 (en) | Silver powder manufacturing method | |
| KR102031753B1 (en) | A method for preparing copper nano powder improved in oxidation stability | |
| JPH0557324B2 (en) | ||
| KR101853420B1 (en) | Silver powder sintered at high temperature and method of manufacturing the same | |
| KR100850009B1 (en) | A manufacturing method of high degree of purity indium oxide from ito target | |
| KR102023711B1 (en) | A silver nano powder of high purity | |
| KR102017177B1 (en) | A method for preparing high-purity silver nano powder using wet process | |
| CN104599740A (en) | Conductive silver paste with nanocarbon | |
| KR102061719B1 (en) | Silver powder and method for manufacturing the same | |
| KR102023714B1 (en) | A silver nano powder improved in oxidation stability prepared by a wet process | |
| JP7069311B2 (en) | How to make silver powder and conductive paste containing silver powder | |
| JPH04176806A (en) | Production of fine copper particles | |
| KR20180058389A (en) | Synthesis of monodispersed spherical silver particles |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A201 | Request for examination | ||
| E902 | Notification of reason for refusal | ||
| AMND | Amendment | ||
| E601 | Decision to refuse application | ||
| AMND | Amendment |