WO2006049831A1 - Procede de production de particules d'argent de haute purete - Google Patents

Procede de production de particules d'argent de haute purete Download PDF

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Publication number
WO2006049831A1
WO2006049831A1 PCT/US2005/036727 US2005036727W WO2006049831A1 WO 2006049831 A1 WO2006049831 A1 WO 2006049831A1 US 2005036727 W US2005036727 W US 2005036727W WO 2006049831 A1 WO2006049831 A1 WO 2006049831A1
Authority
WO
WIPO (PCT)
Prior art keywords
silver
surfactants
surfactant
oxalate
group
Prior art date
Application number
PCT/US2005/036727
Other languages
English (en)
Inventor
Insoo Kim
Chang Gun Lee
Sang Ho Kim
Charles E. Smith, Jr.
Young Jin Kim
Original Assignee
Tokusen U.S.A., Inc.
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.)
Filing date
Publication date
Application filed by Tokusen U.S.A., Inc. filed Critical Tokusen U.S.A., Inc.
Priority to CNA2005800348201A priority Critical patent/CN101065205A/zh
Priority to JP2007536851A priority patent/JP2008517153A/ja
Priority to KR1020077008295A priority patent/KR100888559B1/ko
Priority to US11/664,640 priority patent/US20080105085A1/en
Priority to EP05851218A priority patent/EP1819467A4/fr
Publication of WO2006049831A1 publication Critical patent/WO2006049831A1/fr

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
    • B22F9/20—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
    • 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

Definitions

  • the object of the present invention is to synthesize high purity silver particles and colloids in a process that does not require either surfactants or reducing agents, or only a minimal amount of a surfactant.
  • this object is achieved by dispersing silver oxalates into an appropriate carrier and then thermally decomposing the silver oxalates at a
  • the process of synthesizing silver particles and colloids by the method of the present invention comprises: (i) a silver oxalate synthesizing process; (ii) a process of dispersing silver oxalates into an appropriate carrier, for example, water, alcohol or the like, including a combination of more than one carrier; and (iii) a process of heating said silver oxalates
  • Fig. 1 is a microphotograph of silver particles obtained under the conditions described in Example " ! .
  • Fig. 2 is a microphotograph of silver particles obtained under the conditions described in Example 2.
  • Fig. 3 is a microphotograph of silver particles obtained under the conditions described in Example 3.
  • Fig. 4 is a microphotograph of silver particles obtained under the conditions described in Example 4.
  • Fig. 5 is a microphotograph of silver particles obtained under the conditions described in Example 5.
  • Fig. 6 is a microphotograph of silver particles obtained under the conditions described in Example 6.
  • a method for the production of silver particles and colloids comprises three processes as follows: (i) a silver oxalate (Ag 2 C 2 O 4 ) synthesizing process; (ii) a process of dispersing silver oxalate into an appropriate carrier, for example, water, alcohol or the like, including a combination of more than one carrier; and (iii) a process of heating said
  • a silver oxalate Ag 2 C 2 O 4
  • a first solution of a water soluble silver compound and a second solution of an oxalate compound are mixed together to precipitate silver oxalates.
  • the silver compound may be AgNO 3 .
  • the oxalate compound may be sodium oxalate or oxalic acid.
  • the present invention is not, however, limited to these specific compounds but may include any two solutions of compounds that form silver oxalates upon mixing. After water cleaning processes, preferably two or more rounds of water cleaning processes, are performed to remove impure ions from the precipitated silver oxalate, the silver oxalate is used as the starting material for synthesizing silver powder or colloids.
  • the synthesized silver oxalate is dispersed into an appropriate carrier.
  • the silver oxalate is not dissolved to any substantial extent in the carrier, but is dispersed as solid particles by using ultrasonic treatment.
  • the appropriate carrier may include all types of carriers which can disperse silver oxalate to effectively deliver heat.
  • the carrier is selected to have properties that allow it to behave similarly to a surfactant so as to prevent agglomeration of the silver particles formed from the thermal decomposition of the silver oxalate.
  • alcohols consist of alkyl and hydroxyl groups. Generally, alkyl groups have hydrophobic properties and hydroxyl groups have hydrophilic properties. Organic materials having both hydrophobic and hydrophilic properties can play a role as a surfactant.
  • organic materials having higher carbon numbers tend to be dominantly hydrophobic and may therefore tend to lose the ability to act as a surfactant in the process of the present invention.
  • organic materials having higher numbers of carbon atoms have superior surfactant properties.
  • organic materials with a higher number of carbon atoms is observed to agglomerate silver particles.
  • organic materials with a higher number of carbon atoms do not mix well with water. Therefore, the present invention is limited to methyl, ethyl and propyl alcohols, which have a low number of carbon atoms. Water is also effective in the practice of the present invention.
  • the appropriate carrier may therefore consist of ethyl alcohol, methyl alcohol, propyl alcohol, water or a combination of more than one of the preceding.
  • the carriers selected for the practice of the present invention all have low boiling points: water (10O 0 C), methyl alcohol (64.65°C), ethyl alcohol (78.3°C), and propyl alcohol (82°C). Accordingly, when the carrier with the dispersed silver oxalate is heated in a container at or above 100 0 C, the pressure is always above atmospheric pressure. Typical reaction pressures are about 1.86 * 10 5 N/m 2 when using water as the carrier and about 5.31 * 10 5 N/m 2 when using ethyl alcohol as the carrier.
  • the carbon dioxide gas evolved during the thermal decomposition of the silver oxalate and the carrier vapor may be evacuated as necessary but pressure drops of less than about 6.89 * 10 4 N/m 2 do not affect the quality of the silver particles.
  • the dispersed silver oxalate in the carrier is placed into a closed reactor to heat the dispersed silver oxalate and carrier up to at least 100 0 C to synthesize silver powder or colloids of various form factors.
  • This method may optionally use surfactants in order to prevent coagulation or agglomeration of the silver particles.
  • Surfactants may be added to the water soluble silver or oxalate solutions used to produce silver oxalate, or may be added after the silver oxalate is produced by mixing the two solutions.
  • Surfactants used in this method may include anionic surfactants, cationic surfactants, amphoteric surfactants, nonionic surfactants, fluorochemical surfactants, and polymerizable surfactants, or combinations of the preceding, which may be added to aid in forming silver particles and to break down silver plates or prevent silver plates from coagulation.
  • Surfactants suitable for use in the present invention include PVP (polyvinyl pyrrolidone) and gelatine.
  • silver particles or colloids can be obtained by the method of the present invention, however, it is desirable to limit the amount of surfactant to no more than 80% of the weight of the silver. For example, if 10 grams of silver is placed into the reactor, the weight of the surfactant, such as PVP or gelatin, should be no more than 8 grams.
  • the weight of the surfactant such as PVP or gelatin
  • Example 2 After 2.8 grams of silver oxalate was placed into 300cc of distilled water, ten minutes of ultrasonic treatment was performed to disperse the particles. The dispersed silver oxalate was reacted for 15 minutes at 130 0 C to obtain a solution containing silver particles as shown in Fig. 1.
  • Example 2 After 2.8 grams of silver oxalate was placed into 300cc of distilled water, ten minutes of ultrasonic treatment was performed to disperse the particles. The dispersed silver oxalate was reacted for 15 minutes at 130 0 C to obtain a solution containing silver particles as shown in Fig. 1. Example 2

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Colloid Chemistry (AREA)

Abstract

L'invention concerne un procédé destiné à synthétiser des colloïdes et des particules d'argent de haute pureté et ne requérant aucun ajout de tensioactifs ou d'agents réducteurs ou ne requérant qu'une faible quantité de ceux-ci. Le procédé de synthèse comprend (i) une opération de synthèse d'oxalate d'argent, (ii) une opération de dispersion d'oxalate d'argent dans un support approprié, et (iii) une opération de chauffage de l'oxalate d'argent dispersé dans le support à une température d'au moins 100 °C. On peut synthétiser des particules d'argent et des colloïdes présentant un facteur de forme et une taille variables en fonction des conditions de réaction, du support et du type de tensioactif.
PCT/US2005/036727 2004-10-14 2005-10-13 Procede de production de particules d'argent de haute purete WO2006049831A1 (fr)

Priority Applications (5)

Application Number Priority Date Filing Date Title
CNA2005800348201A CN101065205A (zh) 2004-10-14 2005-10-13 制备高纯度银粒子的方法
JP2007536851A JP2008517153A (ja) 2004-10-14 2005-10-13 高純度銀粒子の製造方法
KR1020077008295A KR100888559B1 (ko) 2004-10-14 2005-10-13 고순도 은 입자의 제조방법
US11/664,640 US20080105085A1 (en) 2004-10-14 2005-10-13 Method Of Production Of High Purity Silver Particles
EP05851218A EP1819467A4 (fr) 2004-10-14 2005-10-13 Procede de production de particules d'argent de haute purete

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US61887604P 2004-10-14 2004-10-14
US60/618,876 2004-10-14

Publications (1)

Publication Number Publication Date
WO2006049831A1 true WO2006049831A1 (fr) 2006-05-11

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/US2005/036727 WO2006049831A1 (fr) 2004-10-14 2005-10-13 Procede de production de particules d'argent de haute purete

Country Status (6)

Country Link
US (1) US20080105085A1 (fr)
EP (1) EP1819467A4 (fr)
JP (1) JP2008517153A (fr)
KR (1) KR100888559B1 (fr)
CN (1) CN101065205A (fr)
WO (1) WO2006049831A1 (fr)

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JP2008214695A (ja) * 2007-03-05 2008-09-18 Shoei Chem Ind Co 銀超微粒子の製造方法

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KR101396803B1 (ko) * 2006-09-21 2014-05-21 토쿠센, 유.에스.에이. 인코포레이티드 나노 사이즈의 이산화티탄 입자들을 제조하기 위한 저온 방법
US8231704B2 (en) * 2009-05-01 2012-07-31 E I Du Pont De Nemours And Company Silver particles and processes for making them
WO2011013542A1 (fr) * 2009-07-30 2011-02-03 国立大学法人京都大学 Nanoparticules métalliques, dispersion les contenant et procédé de production de ces particules
CN102740997B (zh) * 2009-11-27 2016-02-24 特线工业株式会社 含有微小金属粒子的组合物
KR20110113877A (ko) * 2010-04-12 2011-10-19 서울대학교산학협력단 균일한 크기를 가지는 은 나노입자의 대량 제조 방법
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
JP6182294B2 (ja) * 2011-01-28 2017-08-16 宣政 奥田 殺菌組成物及び医薬
FR2977178B1 (fr) * 2011-06-30 2014-05-16 Thales Sa Procede de fabrication d'un dispositif comprenant des brasures realisees a partir d'oxalate metallique
JP5872440B2 (ja) * 2012-02-13 2016-03-01 Ｄｏｗａエレクトロニクス株式会社 球状銀粉およびその製造方法
JP2015533193A (ja) * 2012-08-30 2015-11-19 コーニング インコーポレイテッド 銀の無溶媒合成及びそれによって製造される銀生成物
CN104755639B (zh) 2012-08-31 2017-12-15 康宁股份有限公司 银回收方法和由此制备的银产物
JP2015531432A (ja) 2012-08-31 2015-11-02 コーニング インコーポレイテッド 銀の低温分散系合成及びそれによって製造される銀生成物
TWI508799B (zh) * 2012-12-06 2015-11-21 China Steel Corp A Method for Synthesis of Silver Powder with Adjustable Particle Size
JP6157104B2 (ja) * 2012-12-14 2017-07-05 田中貴金属工業株式会社 銀化合物を製造するための銀前駆体及びその製造方法、並びに、銀化合物の製造方法
CN103602019B (zh) * 2013-11-15 2015-12-02 三河市京纳环保技术有限公司 一种新型大规模制备高透明塑料用含银无机抗菌母粒的方法

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Also Published As

Publication number Publication date
EP1819467A1 (fr) 2007-08-22
US20080105085A1 (en) 2008-05-08
CN101065205A (zh) 2007-10-31
EP1819467A4 (fr) 2010-01-20
KR20070073775A (ko) 2007-07-10
KR100888559B1 (ko) 2009-03-16
JP2008517153A (ja) 2008-05-22

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