CN101065205A - Method of production of high purity silver particles - Google Patents
Method of production of high purity silver particles Download PDFInfo
- Publication number
- CN101065205A CN101065205A CNA2005800348201A CN200580034820A CN101065205A CN 101065205 A CN101065205 A CN 101065205A CN A2005800348201 A CNA2005800348201 A CN A2005800348201A CN 200580034820 A CN200580034820 A CN 200580034820A CN 101065205 A CN101065205 A CN 101065205A
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- CN
- China
- Prior art keywords
- surfactant
- silver
- oxalate
- silver oxalate
- carrier
- Prior art date
- Legal status (The legal status 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 status listed.)
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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
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
-
- 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
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
-
- 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
-
- 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
-
- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
A method for synthesizing high purity silver particles and colloids without requiring the addition of either surfactants or reducing agents thereto, or requiring only a minimal amount thereof is disclosed. The synthesizing process comprises: (i) a silver oxalate synthesizing process; (ii) a process of dispersing silver oxalate into an appropriate carrier; and {iii} a process of heating said silver oxalate dispersed into said carrier at a temperature of at least 100 DEG C. Silver particles and colloids of various form factor and size may be synthesized depending upon the reaction conditions, the carrier, and the type of surfactant.
Description
It is the U.S. Provisional Application No.60/618 of " method for preparing the fine silver particle " that the application requires to enjoy in the title of submitting on October 14th, 2004,876 rights and interests, and the content of this provisional application is with reference to being incorporated into this paper.
Technical field
The present invention relates to a kind of method that forms silver particles, this method comprises silver oxalate is distributed on the suitable carrier, adds the thermal decomposition silver oxalate being greater than or equal under 100 ℃ of temperature then.
Background technology
Developed the method for the synthetic silver particles of many kinds, these methods include but not limited to: the method for electronation, photochemistry, phonochemistry and gas evaporation.In these methods, chemical reduction method is owing to the simplicity of producing is widely used.But, adopt the silver powder of chemical reduction method preparation to be polluted by employed reducing agent, surfactant and foreign ion in the course of reaction, they may be the field of electronic devices of requirement high conductivity or the limiting factor that requires highly purified antibiotic field.
In order to address these problems, needing a kind ofly can not need surfactant and reducing agent, perhaps only needs to prepare under the condition of low quantity of surfactant the method for high-purity silver powder and silver colloid.
Summary of the invention
The objective of the invention is is not needing surfactant and reducing agent, perhaps the method for synthesis of high purity silver particles and silver colloid under the minimum surfactant condition of needs.Among the present invention,, at the temperature thermal decomposition silver oxalate that is greater than or equal to 100 ℃, come synthesis of high purity silver particles and silver colloid, and reach purpose of the present invention then by silver oxalate is distributed to suitable carrier.
Process by the inventive method synthesis of high purity silver particles and silver colloid may further comprise the steps: (i) silver oxalate synthesis step; (ii) silver oxalate is distributed to suitable carrier, for example water, alcohol etc. comprise the step of combination of more than one carrier; (iii) in the temperature that is greater than or equal to 100 ℃, under atmospheric pressure, heating is dispersed in the step of the silver oxalate in the described carrier.
By understanding these features of the present invention and other features, objects and advantages better to the detailed description of preferred implementation and claims below in conjunction with accompanying drawing.
The accompanying drawing summary
Shown in Figure 1 is the microphoto of the silver particles that obtains under embodiment 1 described condition.
Shown in Figure 2 is the microphoto of the silver particles that obtains under embodiment 2 described conditions.
Shown in Figure 3 is the microphoto of the silver particles that obtains under embodiment 3 described conditions.
Shown in Figure 4 is the microphoto of the silver particles that obtains under embodiment 4 described conditions.
Shown in Figure 5 is the microphoto of the silver particles that obtains under embodiment 5 described conditions.
Shown in Figure 6 is the microphoto of the silver particles that obtains under embodiment 6 described conditions.
Implement best mode of the present invention
Below, referring to Fig. 1-6, preferred implementation of the present invention is described.
Among the present invention, preparation silver particles and silver colloid comprise following three steps: (i) synthesis of oxalic acid silver (Ag
2C
2O
4) step; (ii) with silver oxalate to suitable carrier, for example water, alcohol etc. comprise the step of more than one carrier combinations; (iii) in the temperature that is greater than or equal to 100 ℃, under atmospheric pressure, heating is dispersed in the silver oxalate in the described carrier, is decomposed to form the step of silver particles or silver colloid by silver oxalate.
First solution of water-soluble silver compound and second solution of oxalates compound are mixed the precipitation silver oxalate.This silver compound can be AgNO
3The oxalates compound can be sodium oxalate or oxalic acid.But, the invention is not restricted to these specific compounds, and can comprise any two kinds of solution that when mixing, can form silver oxalate.Carry out water and clean, preferred water is cleaned twice or multipass, remove foreign ion from the silver oxalate of precipitation after, with the raw material of this silver oxalate as synthetic silver powder or silver colloid.
Synthetic silver oxalate is distributed in the suitable carrier.Silver oxalate is dissolved in this carrier hardly, but can adopt ultrasonic wave to disperse with solids.Suitable carriers comprises can disperse the carrier of silver oxalate with any kind of effective transmission heat.The carrier of selecting has the performance that is similar to surfactant, assembles to prevent the silver particles that forms when the silver oxalate thermal decomposition.For example, the alcohol of forming by alkyl and hydroxyl.Usually, alkyl has hydrophobicity, and the hydroxyl possess hydrophilic property.Effect with hydrophobicity and hydrophilic organic matter mass-energy performance surfactant.But the organic substance with high carbon number can mainly be a hydrophobicity, therefore can lose the ability as surfactant in the method for the invention.Usually, the organic substance of high carbon atom number has the performance of excellent surfactant.But in the present invention, the organic substance of observing the high carbon atom number is assembled silver particles.In addition, the organic substance of high carbon atom number can not mix with water is fine.Therefore, the present invention is limited to the alcohol of low carbon atom number, methyl alcohol, ethanol and propyl alcohol.When enforcement was of the present invention, water was also very effective.Therefore, suitable carrier comprises the combination of ethanol, propyl alcohol, water or more than one these carriers.
The carrier of selecting for enforcement the present invention all is lower boiling: water (100 ℃), methyl alcohol (64.65 ℃), ethanol (78.3 ℃) and propyl alcohol (82 ℃).Therefore, when in a container, when heating was dispersed with the carrier of silver oxalate under being greater than or equal to 100 ℃, pressure was higher than atmospheric pressure all the time.Typical reaction pressure is about 1.86 * 10 when making water as carrier
5N/m
2, when using ethanol, be about 5.31 * 10 as carrier
5N/m
2During the silver oxalate thermal decomposition, according to formula Ag
2C
2O
4=2Ag+2CO
2, silver oxalate (Ag
2C
2O
4) resolve into silver (Ag) and carbon dioxide (CO
2).When needing, can the carbon dioxide and the carrier vapor of emitting during the silver oxalate thermal decomposition be vacuumized, but less than about 6.89 * 10
4N/m
2Pressure drop can not influence the quality of silver particles.
The silver oxalate that is dispersed in the carrier is put into an enclosed reaction vessel, and silver oxalate that heating disperses and carrier synthesize the colloid of silver powder or various form factors at least 100 ℃.This method can be chosen the use surfactant wantonly, to prevent condensing or assembling of silver particles.In in order to preparation water-soluble silver solution of silver oxalate or oxalate solution, add surfactant, perhaps after the silver oxalate that mixed two kinds of formulations prepared from solutions, add surfactant.The surfactant that this method is used can comprise anionic surfactant, cationic surface active agent, amphoteric surfactant, non-ionic surface active agent, fluorochemical surfactant and polymerizable surfactants, perhaps their combination adds these surfactants and helps to form silver particles and broken silver bits or prevent that the silver bits are coalescent.Be applicable to that surfactant of the present invention comprises PVP (PVP) and gelatin.
Irrelevant with the addition of surfactant when adopting the inventive method to prepare silver particles or silver colloid, still, requirement is limited to amount of surfactant less than 80% of silver-colored weight.For example, if put into 10 gram silver in reactor, the weight of surfactant such as PVP or gelatin should be less than 8 grams.
After silver oxalates put into 300cc distilled water with 2.8 grams, carry out 10 minutes ultrasonic processing, to disperse this particle.The silver oxalate that disperses obtains to contain the solution of silver particles shown in Figure 1 130 ℃ of reactions 15 minutes.
After silver oxalates put into 1000cc ethanol with 28 grams, carry out 10 minutes ultrasonic processing, to disperse this particle.The silver oxalate that disperses obtains to contain the solution of silver particles shown in Figure 2 134 ℃ of reactions 15 minutes.
After 70 milligrams of silver oxalates are put into 1000cc ethanol, carry out 10 minutes ultrasonic processing, to disperse this particle.The silver oxalate that disperses obtains to contain the solution of nanometer-level silver particle shown in Figure 3 135 ℃ of reactions 25 minutes.
After silver oxalates put into the mixed solution of water (50 volume %) and ethanol (50 volume %) with 4.2 grams, this solution synthesized 0.5 micron silver particles shown in Figure 4 130 ℃ of reactions 15 minutes.
Embodiment 5
30 weight %PVP (polyvinylpyrrolidone/ base ketone) are placed in the gram of 4.2 in 1 premium on currency silver oxalate, carry out ultrasonic processing with dispersed particle.The particle that disperses synthesizes 0.5 micron silver particles shown in Figure 5 135 ℃ of reactions 20 minutes.
10 gram gelatin are placed in the gram of 28 in 1 premium on currency silver oxalate, carry out ultrasonic processing with dispersed particle.The particle that disperses synthesizes the silver particles that is less than or equal to 50 nanometers shown in Figure 6 135 ℃ of reactions 15 minutes.
Commercial Application
Because intrinsic high conductivity and the antibiotic property of silver particles, silver particles is widely used in electronics industry and other requires antibiotic industry.Preferably described the present invention with selectable embodiment with reference to some, these embodiments only are used for example, do not constitute the restriction to the scope of the present invention that is proposed by appended claims.
Claims (19)
1. method for preparing silver particles, this method may further comprise the steps:
(a) solid silver oxalate particle is dispersed in the carrier; With
(b) silver oxalate of the described dispersion of heating is decomposed into silver particles at least 100 ℃ with described silver oxalate under greater than atmospheric pressure.
2. the method for claim 1 is characterized in that, this method also is included in the step that step (a) prepares described silver oxalate before, and first solution that is about to silver compound mixes with second solution of oxalates compound, forms silver oxalate.
3. method as claimed in claim 1 or 2 is characterized in that, this method also is included in before the heating steps of (b), adds the step of surfactant in the silver oxalate of described dispersion.
4. method as claimed in claim 3, it is characterized in that, described surfactant is selected from: the surfactant of anion surfactant, cationic surfactant, amphoteric surfactant, non-ionic surface active agent, fluorochemical, polymerizable surfactants, and their any combination.
5. method as claimed in claim 2 is characterized in that, this method also is included in described blend step adds surfactant before in described first solution step.
6. method as claimed in claim 5, it is characterized in that, described surfactant is selected from: the surfactant of anion surfactant, cationic surfactant, amphoteric surfactant, non-ionic surface active agent, fluorochemical, polymerizable surfactants, and their any combination.
7. method as claimed in claim 2 is characterized in that, this method also is included in described blend step adds surfactant before in described second solution step.
8. method as claimed in claim 7, it is characterized in that, described surfactant is selected from: the surfactant of anion surfactant, cationic surfactant, amphoteric surfactant, non-ionic surface active agent, fluorochemical, polymerizable surfactants, and their any combination.
9. method as claimed in claim 1 or 2 is characterized in that, dispersion steps (a) comprises silver oxalate is added described carrier, and the mixture of silver oxalate and carrier is carried out ultrasonic processing.
10. method as claimed in claim 1 or 2 is characterized in that, described carrier is selected from: water, methyl alcohol, ethanol, propyl alcohol, and their any mixture.
11. method as claimed in claim 2 is characterized in that, described silver compound is AgNO
3
12. method as claimed in claim 2 is characterized in that, described oxalates compound is selected from: sodium oxalate and oxalic acid.
13. method as claimed in claim 2 is characterized in that, water cleaned silver oxalate after this method also was included in the preparation silver oxalate, to remove the step of impurity.
14. method as claimed in claim 4 is characterized in that, described surfactant is selected from PVP (PVP) or gelatin.
15. method as claimed in claim 6 is characterized in that, described surfactant is selected from PVP (PVP) or gelatin.
16. method as claimed in claim 8 is characterized in that, described surfactant is selected from PVP (PVP) or gelatin.
17. method as claimed in claim 3 is characterized in that, is not more than 80 weight % of silver in amount of surfactant described in the step (b).
18. method as claimed in claim 5 is characterized in that, is not more than 80 weight % of silver in amount of surfactant described in the step (b).
19. method as claimed in claim 7 is characterized in that, is not more than 80 weight % of silver in amount of surfactant described in the step (b).
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US61887604P | 2004-10-14 | 2004-10-14 | |
| US60/618,876 | 2004-10-14 | ||
| PCT/US2005/036727 WO2006049831A1 (en) | 2004-10-14 | 2005-10-13 | Method of production of high purity silver particles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101065205A true CN101065205A (en) | 2007-10-31 |
Family
ID=36319502
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2005800348201A Pending CN101065205A (en) | 2004-10-14 | 2005-10-13 | Method of production of high purity silver particles |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US20080105085A1 (en) |
| EP (1) | EP1819467A4 (en) |
| JP (1) | JP2008517153A (en) |
| KR (1) | KR100888559B1 (en) |
| CN (1) | CN101065205A (en) |
| WO (1) | WO2006049831A1 (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102413968A (en) * | 2009-05-01 | 2012-04-11 | E.I.内穆尔杜邦公司 | Silver particles and a process for making them |
| CN102740997A (en) * | 2009-11-27 | 2012-10-17 | 特线工业株式会社 | Composition containing metal microparticles |
| CN103602019A (en) * | 2013-11-15 | 2014-02-26 | 李泽国 | Novel method for large-scale preparation of silver-containing inorganic antimicrobial master batch for high-transparency plastics |
| CN103846451A (en) * | 2012-12-06 | 2014-06-11 | 中国钢铁股份有限公司 | Method for synthesizing silver powder with adjustable particle size |
| CN104884193A (en) * | 2012-08-30 | 2015-09-02 | 康宁股份有限公司 | Solvent-free syntheses of silver and silver products produced thereby |
| US9637806B2 (en) | 2012-08-31 | 2017-05-02 | Corning Incorporated | Silver recovery methods and silver products produced thereby |
| US9670564B2 (en) | 2012-08-31 | 2017-06-06 | Corning Incorporated | Low-temperature dispersion-based syntheses of silver and silver products produced thereby |
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| JP2008516880A (en) * | 2004-10-14 | 2008-05-22 | トクセン ユー．エス．エー．、インコーポレイテッド | Method for synthesizing nano-sized titanium dioxide particles |
| EP2074064A4 (en) * | 2006-09-21 | 2013-06-05 | Tokusen U S A Inc | Low temperature process for producing nano-sized titanium dioxide particles |
| JP4978242B2 (en) * | 2007-03-05 | 2012-07-18 | 昭栄化学工業株式会社 | Method for producing silver ultrafine particles |
| JP5119362B2 (en) * | 2009-07-30 | 2013-01-16 | 国立大学法人京都大学 | Metal-based nanoparticles, dispersion containing the same, and method for producing the same |
| KR20110113877A (en) * | 2010-04-12 | 2011-10-19 | 서울대학교산학협력단 | Process for large-scale production of uniform silver nanoparticle |
| US20110088593A1 (en) * | 2010-12-23 | 2011-04-21 | Mansour Hemmati | Silver dz nano-fluid composition for nano-fin formation and a method of producing the same |
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| FR2977178B1 (en) * | 2011-06-30 | 2014-05-16 | Thales Sa | METHOD FOR MANUFACTURING A DEVICE COMPRISING BRASURES REALIZED FROM METAL OXALATE |
| JP5872440B2 (en) * | 2012-02-13 | 2016-03-01 | Ｄｏｗａエレクトロニクス株式会社 | Spherical silver powder and method for producing the same |
| JP6157104B2 (en) * | 2012-12-14 | 2017-07-05 | 田中貴金属工業株式会社 | Silver precursor for producing silver compound, method for producing the same, and method for producing silver compound |
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-
2005
- 2005-10-13 JP JP2007536851A patent/JP2008517153A/en active Pending
- 2005-10-13 WO PCT/US2005/036727 patent/WO2006049831A1/en active Application Filing
- 2005-10-13 US US11/664,640 patent/US20080105085A1/en not_active Abandoned
- 2005-10-13 CN CNA2005800348201A patent/CN101065205A/en active Pending
- 2005-10-13 EP EP05851218A patent/EP1819467A4/en not_active Withdrawn
- 2005-10-13 KR KR1020077008295A patent/KR100888559B1/en active IP Right Grant
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102413968A (en) * | 2009-05-01 | 2012-04-11 | E.I.内穆尔杜邦公司 | Silver particles and a process for making them |
| CN102740997A (en) * | 2009-11-27 | 2012-10-17 | 特线工业株式会社 | Composition containing metal microparticles |
| CN102740997B (en) * | 2009-11-27 | 2016-02-24 | 特线工业株式会社 | Composition containing small metal particles |
| CN104884193A (en) * | 2012-08-30 | 2015-09-02 | 康宁股份有限公司 | Solvent-free syntheses of silver and silver products produced thereby |
| CN104884193B (en) * | 2012-08-30 | 2017-03-08 | 康宁股份有限公司 | Not solvent-laden silver synthesis and the silver-colored product thus prepared |
| US9982322B2 (en) | 2012-08-30 | 2018-05-29 | Corning Incorporated | Solvent-free syntheses of silver products produced thereby |
| US9637806B2 (en) | 2012-08-31 | 2017-05-02 | Corning Incorporated | Silver recovery methods and silver products produced thereby |
| US9670564B2 (en) | 2012-08-31 | 2017-06-06 | Corning Incorporated | Low-temperature dispersion-based syntheses of silver and silver products produced thereby |
| CN103846451A (en) * | 2012-12-06 | 2014-06-11 | 中国钢铁股份有限公司 | Method for synthesizing silver powder with adjustable particle size |
| CN103602019A (en) * | 2013-11-15 | 2014-02-26 | 李泽国 | Novel method for large-scale preparation of silver-containing inorganic antimicrobial master batch for high-transparency plastics |
Also Published As
| Publication number | Publication date |
|---|---|
| KR20070073775A (en) | 2007-07-10 |
| KR100888559B1 (en) | 2009-03-16 |
| EP1819467A1 (en) | 2007-08-22 |
| JP2008517153A (en) | 2008-05-22 |
| US20080105085A1 (en) | 2008-05-08 |
| WO2006049831A1 (en) | 2006-05-11 |
| EP1819467A4 (en) | 2010-01-20 |
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