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US20100192728A1 - Spherical Copper Fine Powder and Process for Producing the Same - Google Patents

Spherical Copper Fine Powder and Process for Producing the Same Download PDF

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Publication number
US20100192728A1
US20100192728A1 US12/666,864 US66686408A US2010192728A1 US 20100192728 A1 US20100192728 A1 US 20100192728A1 US 66686408 A US66686408 A US 66686408A US 2010192728 A1 US2010192728 A1 US 2010192728A1
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US
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Prior art keywords
fine powder
copper fine
copper
grain size
producing spherical
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Abandoned
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US12/666,864
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English (en)
Inventor
Takahiro Haga
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JX Nippon Mining and Metals Corp
Nippon Mining Holdings Inc
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Nippon Mining and Metals Co Ltd
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Assigned to NIPPON MINING & METALS CO., LTD. reassignment NIPPON MINING & METALS CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HAGA, TAKAHIRO
Publication of US20100192728A1 publication Critical patent/US20100192728A1/en
Assigned to NIPPON MINING HOLDINGS, INC. reassignment NIPPON MINING HOLDINGS, INC. MERGER (SEE DOCUMENT FOR DETAILS). Assignors: NIPPON MINING & METALS CO., LTD.
Assigned to JX NIPPON MINING & METALS CORPORATION reassignment JX NIPPON MINING & METALS CORPORATION CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: NIPPON MINING HOLDINGS, INC.
Abandoned legal-status Critical Current

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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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • 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
    • B22F9/18—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 spherical metal copper particles having a controlled grain shape or grain size, and in particular to a method of producing spherical copper fine powder which can achieve speedy, efficient and stable production of metallic copper particles controlled in particle shape or particle size, as well as to the spherical copper fine powder obtained thereby.
  • the electrolytic method and the atomization method have been used conventionally.
  • the copper powder prepared based on these methods can be favorably used in powder metallurgy of oil retaining bearings and electrical brushes, but finer particles with controlled grain size and grain shape are being demanded for use as conductive fillers such as paint, paste and resin in which the demands thereof are expected to increase in the near future.
  • the method of reacting cuprous oxide particles and acid enables the favorable control of the grain shape and grain size of the metal copper particles to be created, and by additionally managing the reactive conditions such as the pH, temperature, and average retention time, it is possible to adjust the prescribed grain shape and grain size, and produce high purity metal copper fine particles.
  • Patent Document 1 was published in 1985, and was extremely high technology in terms copper powder production at that time.
  • the present inventors proposed a method of producing copper fine powder in which the disproportionation start temperature is set to 10° C. or less upon producing copper fine powder by performing acid-based disproportionation to cuprous oxide in an aqueous solution containing an additive of natural resin, polysaccharide or a derivative thereof (refer to Patent Document 2).
  • This method enables the speedy production of fine copper fine powder, and is extremely effective. Nevertheless, the average grain size of this copper fine powder is at a level of 0.5 ⁇ m to 3.0 ⁇ m, and the present inventors were searching for a method for even finer copper powder.
  • An object of the present invention is to provide a method of producing spherical copper fine powder which provides speedy, efficient and stable production of metallic copper particles controlled in particle shape or particle size, particularly copper fine powder having smaller particle sizes, as well as to provide the spherical copper fine powder obtained thereby.
  • the present invention provides:
  • the term “spherical” means a shape in which the ratio of the short diameter and long diameter of the individual copper particles is 150% or less, and in particular 120% or less.
  • a shape in which the ratio of the short diameter and long diameter exceeds 150% is of a flat shape, and is not referred to as “spherical.”
  • the amount thereof is 20% or less of the overall amount, preferably 10% or less, and more preferably 5% or less. In reality, desirably, such flat copper fine powder is not contained.
  • the present invention additionally provides:
  • natural rubber or gelatin may be used as the additive.
  • pine resin, gelatin, glue, carboxymethylcellulose (CMC), starch, dextrin, gum arabic, casein and the like are effective.
  • the slurry concentration of the cuprous oxide is suitably 500 g/L or less, the process is usually carried out at 300 g/L or less. This slurry concentration can be suitably selected without any particular limitation. If the slurry concentration of the cuprous oxide is made to be extremely low, since the reaction will not progress, it will just increase costs.
  • the molar ratio (predetermined number of acids/number of moles of slurry) is desirably 1.00 to 2.00 upon implementing the process. There will be no problem with the reaction so long as the molar ratio is equivalent (1.0) or higher. The effect will not change even if acid is added excessively. Contrarily, if the acid concentration is too high, the calorific value upon adding acid to the cuprous oxide slurry will increase, the temperature of the reaction system will increase, which is expected to be disadvantageous in obtaining finer powder, and in terms of cost, disadvantageous as well.
  • the reaction rate will consequently deteriorate, and this will be disadvantageous in obtaining finer powder.
  • the molar ratio predetermined number of acids/number of moles of slurry
  • the disproportionation start temperature is set to 10° C. or less in producing copper fine powder by performing acid-based disproportionation in an aqueous medium. This is effective in forming copper fine powder with fine particles.
  • this acid aqueous solution be added at a time, namely, at a time within 15 minutes. It is thereby possible to obtain spherical copper fine powder having an average grain size of 0.25 ⁇ m or less.
  • the disproportionation based on the speedy addition of acid aqueous solution is able to achieve fine spherical copper powder. The reason why this collective addition in a short time is effective in producing copper fine powder is not necessarily clear.
  • the adding time of the acid aqueous solution is short, that is, 3 minutes or less, and more preferably 1 minute or less.
  • the present invention further provides:
  • the method of producing copper fine powder according to the present invention yields superior effects of achieving a spherical grain shape and arbitrarily controlling the grain size, and enabling speedy, efficient and stable production of copper fine powder having smaller particle sizes.
  • FIG. 1 A diagram showing the outline of the production flow of the spherical copper fine powder
  • FIG. 2 An FE-SEM photograph of the spherical copper fine powder
  • the cuprous oxide particles may be produced with a publicly known method such as from a copper salt aqueous solution via cuprous chloride. Specifically, since there is no direct relationship between the grain size of the cuprous oxide particles to be used and the grain size of the metal copper particles obtained by the method of the present invention, coarse cuprous oxide particles may be used.
  • Sulfuric acid is commonly used for acid, but nitric acid, phosphoric acid, or acetic acid may be used. It is not necessary to specify the type of acid. In case sulfuric acid is used, disproportionation is to generate a copper sulfate aqueous solution and metal copper particles based on the following reaction formula.
  • the pH of the reaction system will decrease, and the pH will increase in the opposite case.
  • the pH can be controlled based on the additive ratio of acid or cuprous oxide.
  • the pH is maintained to be 2.5 or less, and desirably in the vicinity of 1.0 in order to avoid the generation of precipitation of impurities during the reaction and to promptly advance the reaction without leaving any residual cuprous oxide.
  • acid-based disproportionation is performed in an aqueous medium including an additive (protective colloid) of natural resin, polysaccharide or a derivative thereof. This is a major characteristic of this invention.
  • This additive works to inhibit the growth of particles, and also works to reduce the frequency that the particles come in contact with each other. Accordingly, this is effective in producing fine particles.
  • natural rubber or gelatin may be used.
  • pine resin, gelatin, glue, carboxymethylcellulose (CMC), starch, dextrin, gum arabic, casein and the like are effective.
  • glue it is possible to achieve fine powder having an average grain size of 0.25 ⁇ m or less, and yield an agglomeration inhibiting effect.
  • the liquid temperature during the reaction is set to 30° C. or less, and preferably to 10° C. or less upon producing metal copper fine particles. If the liquid temperature exceeds 30° C., there is tendency of the metal copper fine particles becoming agglomerated and bonded with each other. In particular, it is desirable to set the disproportionation start temperature to 10° C. or less in order to seek finer powder. As a result of lowering the reaction temperature, the growth of particles can be effectively inhibited, and even finer powder can be obtained.
  • reaction temperature With temperature of 10° C. or less being maintained till the end of the reaction, there will be a better effect. It is also possible to set the reaction temperature to exceed 30° C.
  • a special grain shape can be obtained by leveraging the tendency of the metal copper particles becoming agglomerated and bonded with each other. As described above, the grain shape and grain size of the metal copper particles to be generated can be controlled based on the reaction temperature. The present invention covers this kind of temperature control.
  • this acid aqueous solution be added at a time. Specifically, the acid aqueous solution needs to be added at a time within 15 minutes, preferably within 3 minutes and more preferably within 1 minute. It is thereby possible to obtain spherical copper fine powder having an average grain size of 0.25 ⁇ m or less.
  • the disproportionation based on the speedy addition of acid aqueous solution is able to achieve fine spherical copper powder.
  • nucleation will prevail over the growth of particles, and a finer copper powder can be obtained.
  • This short-period disproportionation is considered to have an effect of inhibiting the growth of copper particles.
  • collective addition in a short time is essential in achieving finer powder.
  • the average grain size of the present invention is desirably a small value, but if the value is smaller than the average grain size (D 50 ), the actual value of D 10 becomes 0.06 ⁇ m, and D min as the minimum value of grain size distribution will become even smaller.
  • the average grain size is set to 0.05 ⁇ m.
  • the average grain size is set to 0.05 ⁇ m.
  • the measured value and the theoretical value of the specific surface area are different.
  • the true density of copper is 8.93 g/cm 3
  • the tendency is: the smaller the average grain size becomes, the less the difference between the theoretical value and the measured value becomes. This is considered to be because the surface state (irregularities on the outermost surface) will affect the specific surface area when the average grain size is large, while in case the average grain size becomes small, the influence of the size itself becomes greater than the surface state and the difference between the theoretical value and the measured value becomes less.
  • the upper limit of the specific surface area was set to 15.0 m 2 /g.
  • the ultrafine spherical copper powder obtained as described above could become agglomerated in the air or liquid. Nevertheless, the agglomerate itself can be dispersed once again with a means such as applying ultrasonic waves in the aqueous solution. It should be understood that this is based on the premise that the initial particles are spherical copper fine powder having an average grain size of 0.25 ⁇ m or less. This is because spherical fine copper powder cannot be obtained by attempting to achieve finer powder by way of pulverization.
  • acid When performing batch-type reaction, acid may be added to the slurry of cuprous oxide particles, or contrarily cuprous oxide particles or a slurry of cuprous oxide particles may be added to the acid solution.
  • FIG. 1 shows the outline of the production flow of the spherical copper fine powder.
  • the spherical copper fine powder is produced through the processes as shown in FIG. 1 : dissolving additive ⁇ obtaining slurry (process of adding cuprous oxide into an aqueous medium containing an additive to form a slurry) ⁇ disproportionation (addition of acid aqueous solution) ⁇ cleaning ⁇ rust prevention ⁇ filtering ⁇ drying ⁇ pulverizing ⁇ sorting.
  • Glue of 8 g was dissolved in 7 liters of deionized water, 1000 g of cuprous oxide was added and suspended therein in mixing the solution, and cuprous oxide slurry was cooled to 7° C. Cuprous oxide in the slurry was approximately 143 g/L.
  • the FE-SEM photograph of the spherical copper fine powder obtained as described above is shown in FIG. 2 .
  • the average grain size of the copper fine powder was 0.09 ⁇ m. It is evident that the addition of cooled diluted sulfuric acid in 1 minute is extremely effective in attaining copper fine powder.
  • the specific surface area BET was 6.66 m 2 /g. This Example 1 is a particularly favorable example even among the conditions of the other Examples.
  • Example 1 Examples of cases using, as the additive, pine resin, gelatin, carboxymethylcellulose (CMC), starch, dextrin, gum arabic, and casein are shown.
  • the copper powder was created under all the same conditions as Example 1 other than substituting the additive. Consequently, the foregoing additives are all effective, but the addition of “glue” in Example 1 yielded the most favorable result.
  • the copper fine powder was inspected in each case with polyethylene glycol (PEG) selected as the additive and without it. The results are shown in Comparative Examples 1 and 2. Then, the copper powder was created under the same conditions as Example 1 except the change of additive. Consequently, the additive of Comparative Example 1 yielded no effect, and in the case without additive showed inferior results as well; the grain size of the copper powder increased and copper powder having a low BET specific surface area was obtained.
  • PEG polyethylene glycol
  • the average grain size and the specific surface area of the spherical copper fine powder pertaining to the foregoing Examples and Comparative Examples were measured.
  • the average grain size was measured based on the laser diffraction/dispersion grain size distribution measurement method, and the value of the weight cumulative grain size D 50 was adopted.
  • the specific surface area was measured based on the BET method.
  • Example 9 to Example 12, Example 16
  • Example 9 to Example 12 results from changing the acid addition time are shown in Example 9 to Example 12. Then, the acid addition time was changed from 5 seconds to 15 minutes.
  • the copper powder was created under the same conditions as Example 1. Consequently, with the acid addition time being shorter, it was possible to obtain copper powder having a small grain size and a low BET specific surface area. Since the acid addition time also affects the grain size and BET specific surface area, desirably the acid addition time is as short as possible. Though there is no need to take time in adding the acid, it is desirable to add the acid within approximately 15 minutes. The results were the same even when using the additives of pine resin, gelatin, carboxymethylcellulose (CMC), starch, dextrin, gum arabic, and casein.
  • CMC carboxymethylcellulose
  • Comparative Example 3 the cases when the acid addition time was 16 minutes and 80 minutes, which are outside the conditions of the present invention, are shown in Comparative Example 3 and Comparative Example 4. Then, conditions other than changing the acid addition time and the copper powder, were the same as Example 1. In all cases, the grain size of the copper powder increased and copper powder having a low BET specific surface area was obtained, and yielded inferior results.
  • Example 9 The results of Example 9 to Example 12 and Comparative Example 3 to Comparative Example 4 are shown in Table 2.
  • Example 13 results from changing the reaction start temperature are shown in Example 13 to Example 17. Then, the reaction start temperature was changed from 0 to 30° C. Here, other than changing the reaction start temperature, the copper powder was created under the same conditions as Example 1.
  • Comparative Example 5 a case where the reaction start temperature was 50° C., which is outside the conditions of the present invention, is shown in Comparative Example 5. Then, other than changing the reaction start temperature, the copper powder was created under the same conditions as Example 1. In all cases, the grain size of the copper powder increased and copper powder having a low BET specific surface area was obtained, and yielded inferior results.
  • Example 13 The results of Example 13 to Example 17 and Comparative Example 5 are shown in Table 3.
  • cuprous oxide in an aqueous medium including an additive of natural resin, polysaccharide or a derivative thereof in order to prepare a slurry containing 10 to 300 g/L of cuprous oxide adding 5 to 50% of an acid aqueous solution at a molar ratio (predetermined number of acids/number of moles of slurry) of 1.00 to 2.00 at a time to the slurry within 3 minutes, and thereby performing disproportionation, it is possible to obtain favorable spherical copper fine powder.
  • a spherical copper fine powder produced according to the present invention is very effective since the grain size of the powder is small and uniform.
  • the powder is useful not only for oil retaining bearings and electrical brushes, but also as conductive fillers to be used as paint, paste, resin and the like.

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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)
  • Powder Metallurgy (AREA)
US12/666,864 2007-06-28 2008-06-17 Spherical Copper Fine Powder and Process for Producing the Same Abandoned US20100192728A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2007169869 2007-06-28
JP2007-169869 2007-06-28
PCT/JP2008/061033 WO2009001710A1 (ja) 2007-06-28 2008-06-17 球状銅微粉及びその製造方法

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US (1) US20100192728A1 (zh)
JP (2) JP5235193B2 (zh)
KR (2) KR20100024431A (zh)
CN (1) CN101687253A (zh)
TW (1) TW200914166A (zh)
WO (1) WO2009001710A1 (zh)

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US9248504B2 (en) 2010-09-30 2016-02-02 Dowa Electronics Materials Co., Ltd. Copper powder for conductive paste and method for producing same

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GB2462189B (en) 2008-08-01 2013-05-29 Lab Impex Systems Ltd Method and apparatus for measuring radioactivity
JP2011174144A (ja) * 2010-02-25 2011-09-08 Jx Nippon Mining & Metals Corp 銅微粉及びその製造方法
JP5571435B2 (ja) * 2010-03-31 2014-08-13 Ｊｘ日鉱日石金属株式会社 銀メッキ銅微粉の製造方法
JP6031571B2 (ja) * 2010-09-30 2016-11-24 Ｄｏｗａエレクトロニクス株式会社 導電性ペースト用銅粉およびその製造方法
JP2012126942A (ja) * 2010-12-14 2012-07-05 Jx Nippon Mining & Metals Corp 球状銅微粉及びその製造方法
JP2014034697A (ja) * 2012-08-08 2014-02-24 Furukawa Co Ltd 銅微粒子の製造方法、導電性ペーストおよび導電性ペーストの製造方法
JP5960543B2 (ja) * 2012-08-08 2016-08-02 古河機械金属株式会社 銅微粒子の製造方法、および導電性ペーストの製造方法
WO2014080662A1 (ja) * 2012-11-26 2014-05-30 三井金属鉱業株式会社 銅粉及びその製造方法
JP2014129609A (ja) * 2014-03-07 2014-07-10 Hokkaido Univ 銅微粒子の製造方法
US10773311B2 (en) * 2015-09-03 2020-09-15 Dowa Electronics Materials Co., Ltd. Phosphorus-containing copper powder and method for producing the same
JP6561100B2 (ja) * 2017-10-04 2019-08-14 Ｊｘ金属株式会社 表面処理銅微粒子の製造方法
JP6549298B1 (ja) 2018-09-21 2019-07-24 Ｊｘ金属株式会社 易解砕性銅粉及びその製造方法
TWI792540B (zh) * 2020-09-15 2023-02-11 日商Ｊｘ金屬股份有限公司 銅粉及銅粉之製造方法
WO2023126830A1 (en) 2021-12-27 2023-07-06 Tata Steel Limited A method of producing spherical copper powder and a product thereof

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US9248504B2 (en) 2010-09-30 2016-02-02 Dowa Electronics Materials Co., Ltd. Copper powder for conductive paste and method for producing same
EP2614904A4 (en) * 2010-09-30 2017-06-07 DOWA Electronics Materials Co., Ltd. Copper powder for conductive paste and method for manufacturing same

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JP5235193B2 (ja) 2013-07-10
KR20100024431A (ko) 2010-03-05
WO2009001710A1 (ja) 2008-12-31
JP2013057128A (ja) 2013-03-28
TWI370033B (zh) 2012-08-11
CN101687253A (zh) 2010-03-31
KR20120116013A (ko) 2012-10-19
JPWO2009001710A1 (ja) 2010-08-26
TW200914166A (en) 2009-04-01

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Free format text: MERGER;ASSIGNOR:NIPPON MINING & METALS CO., LTD.;REEL/FRAME:025115/0675

Effective date: 20100701

AS Assignment

Owner name: JX NIPPON MINING & METALS CORPORATION, JAPAN

Free format text: CHANGE OF NAME;ASSIGNOR:NIPPON MINING HOLDINGS, INC.;REEL/FRAME:025123/0420

Effective date: 20100701

STCB Information on status: application discontinuation

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