WO2014189025A1 - 銀粒子の製造方法 - Google Patents

銀粒子の製造方法 Download PDF

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Publication number
WO2014189025A1
WO2014189025A1 PCT/JP2014/063281 JP2014063281W WO2014189025A1 WO 2014189025 A1 WO2014189025 A1 WO 2014189025A1 JP 2014063281 W JP2014063281 W JP 2014063281W WO 2014189025 A1 WO2014189025 A1 WO 2014189025A1
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Prior art keywords
silver
silver particles
amine
particle size
producing
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PCT/JP2014/063281
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English (en)
French (fr)
Japanese (ja)
Inventor
久保　仁志
勇一 牧田
優輔 大嶋
英和 松田
紀章 中村
淳一 谷内
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田中貴金属工業株式会社
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Application filed by 田中貴金属工業株式会社 filed Critical 田中貴金属工業株式会社
Priority to CN201480029945.4A priority Critical patent/CN105263656B/zh
Priority to KR1020157034618A priority patent/KR102019536B1/ko
Priority to KR1020187009441A priority patent/KR20180039174A/ko
Priority to DE112014002552.6T priority patent/DE112014002552B4/de
Publication of WO2014189025A1 publication Critical patent/WO2014189025A1/ja

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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
    • B22F9/30—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
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/056—Submicron particles having a size above 100 nm up to 300 nm
    • 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

Definitions

  • the present invention relates to a method for producing silver particles. Specifically, the present invention relates to a method for producing silver particles having a uniform particle size while controlling the size in producing silver particles having a particle size in the range of tens of nm to hundreds of tens of nm.
  • Silver (Ag) is a kind of noble metal that has long been known for use as a decorative product, but has excellent conductivity, light reflectivity, and unique properties such as catalytic action and antibacterial action. Therefore, the metal is expected to be used for various industrial applications such as electrodes / wiring materials, reflective film materials, catalysts, and antibacterial materials.
  • As a utilization form of silver for these various uses there is one in which silver particles are dispersed and suspended in an appropriate solvent.
  • this metal paste is formed by pasting silver particles into electrodes / wiring formation, adhesives / bonding materials, conductive adhesives / conductive bonding materials, and heat conductive materials of wiring boards mounted on electronic components such as semiconductor devices.
  • the desired electrode, wiring, joint, and pattern can be formed by applying and baking.
  • a generally known method for producing silver particles is a liquid phase reduction method.
  • a silver compound as a precursor is dissolved in a solvent, and silver is precipitated by adding a reducing agent thereto.
  • a compound called a protective agent it is usual to add a compound called a protective agent.
  • the protective agent binds to the silver particles that have been reduced and deposited, and suppresses the silver particles from contacting each other, thereby preventing aggregation of the silver particles.
  • the method for producing silver particles by the liquid phase reduction method can produce silver particles efficiently by adjusting the concentration of the silver compound in the solvent, the type and amount of the reducing agent, and further selecting an appropriate protective agent.
  • silver particles produced by the liquid phase reduction method tend to be usually as large as several ⁇ m or more, and the particle size distribution tends to vary due to the concentration gradient of the reactants in the solvent.
  • the thermal decomposition method of a silver complex is reported as a manufacturing method of the silver particle replaced with a liquid phase reduction method (patent document 1).
  • This method basically utilizes the characteristics of a silver compound having thermal decomposability such as silver oxalate (Ag 2 C 2 0 4 ).
  • a complex is formed by such a silver compound and an organic compound that serves as a protective agent, and this is heated as a precursor to obtain silver particles.
  • an amine is added to silver oxalate as a protective agent to form a silver-amine complex, which is heated to a predetermined temperature, and silver particles are produced by thermal decomposition.
  • this pyrolysis method extremely fine silver fine particles of several nm to several tens of nm can be produced, and silver fine particles having a relatively uniform particle diameter can be produced.
  • the field of use of silver particles tends to expand. Therefore, not only silver fine particles having a fine particle size of 10 nm or less, but also medium or larger sizes (for example, about several tens of nm) depending on applications. Silver particles are required.
  • a production method capable of controlling the size of the silver particles obtained according to the purpose of use is required.
  • the conventional method for producing silver particles described above is insufficient from the viewpoint of particle size control.
  • the thermal decomposition method is a production method for fine silver particles of several nm to several tens of nm.
  • the particle size of the silver particles to be produced also has little variation.
  • the silver particles obtained by the thermal decomposition method have a certain particle size, but as described above, the particle size suitable for production was a minute size depending on the type of silver compound. For this reason, when silver particles having a large particle size (for example, a particle size of several tens of nanometers or more) are produced by a thermal decomposition method, it is difficult to obtain a uniform particle size.
  • silver particles having a relatively uniform particle size can be obtained with respect to the size of about tens of nanometers, larger silver particles such as tens of nanometers can be obtained.
  • the particle size distribution tends to vary.
  • the present invention provides a method for producing silver particles, the size of which can be controlled within the range of several tens of nanometers to one hundred and several tens of nanometers, with a uniform particle diameter.
  • the inventors of the present invention as a method for solving the above problems, first decided to conduct a study based on a method for producing silver particles by a thermal decomposition method.
  • the thermal decomposition method can produce silver particles having a relatively uniform particle size, and it is considered that the particle size adjustment is easier than the liquid phase reduction method.
  • the present inventors considered the generation mechanism of silver particles by the pyrolysis method with reference to the general Lamer rule, which is the precipitation mechanism of monodisperse fine particles in a closed solution system, as follows.
  • a case where silver particles are produced by thermally decomposing a silver oxalate complex coordinated with hexylamine is taken as an example.
  • silver “nucleation” starts at 80 to 90 ° C., that is, slightly lower than the decomposition temperature of the complex (about 110 ° C.).
  • heating is continued and the temperature is raised to the vicinity of the decomposition temperature (90 ° C. to 110 ° C.)
  • decomposition of the complex proceeds on the surface of the generated nucleus and “nuclear growth” occurs.
  • the particle diameter of the generated silver particles varies depending on the heating rate. That is, it is considered that silver particles having a small particle size are generated by increasing the heating rate, and silver particles having a large particle size are generated when the heating rate is low.
  • the heating rate is adjusted, the above-mentioned tendency is observed as a whole, but it is not easy to obtain uniform silver particles having no variation in particle size distribution.
  • the inventors of the present invention have come up with the present invention that uniformly heats the silver-amine complex in consideration of the temperature difference in the reaction system in the heating process as one of the causes of such particle size variation.
  • the present invention is a method for producing silver particles by mixing a silver compound having thermal decomposability and an amine to produce a precursor silver-amine complex and heating the reaction system containing the precursor.
  • the present invention relates to a method for producing silver particles, wherein the water content of the reaction system before heating is 30 to 100 parts by weight with respect to 100 parts by weight of the silver compound.
  • the present invention is based on a method for producing silver particles by a thermal decomposition method, and allows a predetermined range of moisture to be present in the reaction system in the heating step of the silver-amine complex.
  • the water in the reaction system acts as a so-called buffering agent in the heating step for decomposing the complex so that the heating can proceed uniformly.
  • the temperature difference in the reaction system during heating is reduced, and the nucleation and growth of silver particles proceed uniformly. It becomes easy to do.
  • the water content of the reaction system needs to be in the range of 30 to 100 parts by weight with respect to 100 parts by weight of the silver compound.
  • a preferred range for the water content is 30 to 95 parts by weight, and a more preferred range is 30 to 80 parts by weight.
  • the amount of water is small (less than 30 parts by weight), the particle size of the obtained silver particles is limited to a very small one, and silver particles having a targeted particle size cannot be produced.
  • the amount of water is large (exceeding 100 parts by weight), the particle size of silver particles tends to vary.
  • the water content of this reaction system is the water content immediately before the heating process, and it is necessary to consider the amount of water added to the reaction system so far.
  • the silver compound may be used in a wet state to which water has been added in advance, but the amount of water added in advance is also included in the amount of water. For this reason, when it falls within the specified range of the water content only by the amount added in advance to the silver compound or the homogenizing agent, it can be heated as it is without separately adjusting the water content of the reaction system.
  • the amount added in advance is less than the lower limit (30 parts by weight) of the water content, it is necessary to adjust the water content, for example, by adding water separately.
  • the timing of adding water may be before the heating step, and may be added at any stage before formation of the silver-amine complex or after formation of the complex.
  • the silver-amine complex that is the precursor of the silver particles is assumed to be thermally decomposable.
  • a thermally decomposable silver compound is used, and silver oxalate, silver nitrate, silver acetate, silver carbonate, silver oxide, silver nitrite, silver benzoate, silver cyanate, silver citrate, silver lactate, etc. are applied it can.
  • silver oxalate (Ag 2 C 2 O 4 ) or silver carbonate (Ag 2 CO 3 ) is particularly preferable.
  • Silver oxalate and silver carbonate can be decomposed at a relatively low temperature without requiring a reducing agent to produce silver particles. Further, since carbon dioxide generated by the decomposition is released as a gas, no impurities remain in the solution.
  • silver oxalate is an explosive powdery solid, water or an organic solvent (alcohol, alkane, alkene, alkyne, ketone, ether, ester, carboxylic acid, fatty acid, aromatic, amine, It is preferable to use a mixture obtained by mixing amide, nitrile, etc.) as a dispersion solvent and making it wet. By making it wet, explosiveness is remarkably lowered and handling becomes easy. At this time, a mixture of 10 to 200 parts by weight of a dispersion solvent with respect to 100 parts by weight of silver oxalate is preferable. However, as described above, since the present invention strictly regulates the amount of water in the reaction system, the mixing of water needs to be within a range not exceeding the specified amount.
  • the amine reacted with the silver compound preferably has a total carbon number of hydrocarbon groups of 4 to 10, particularly preferably 4 to 8.
  • the preferable range for the total number of carbon atoms of the hydrocarbon group is defined by the silver particles produced by changing the stability and decomposition temperature of the silver-amine complex formed by the amine coordinated to the silver compound. This is because the particle size of the material is changed.
  • the resulting silver particles have a particle size of several tens of nm to several ⁇ m, and the particle size distribution tends to vary greatly.
  • an amine having a total carbon number exceeding 10 is applied, the silver-amine complex is hardly thermally decomposed during synthesis, and many unreacted substances other than silver particles are likely to remain.
  • (mono) amine having one amino group or diamine having two amino groups can be applied.
  • An amine having one hydrocarbon group bonded to an amino group that is, a primary amine (RNH 2 ) is preferable.
  • RNH 2 primary amine
  • at least one amino group is preferably a primary amine.
  • Tertiary amines tend not to form complexes with silver compounds.
  • the hydrocarbon group bonded to the amino group is preferably a straight chain or branched chain hydrocarbon that does not contain a cyclic structure, and particularly preferably a saturated hydrocarbon that does not contain an unsaturated hydrocarbon.
  • the particle size of silver particles is controlled by selecting the type of amine. Can do. According to the configuration of the present invention, for example, when hexylamine is applied, silver particles having a particle diameter of 50 to 190 nm can be produced. Further, when octylamine is applied, finer silver particles can be formed than when hexylamine is applied, and silver particles having a particle diameter of 15 to 50 nm can be produced. Moreover, the amine made to react with a silver compound in this invention can apply 2 or more types.
  • intermediate stability complexes are formed for the respective amines, and silver particles having a particle size corresponding to the complex can be produced.
  • silver particles having an intermediate particle size can be produced with respect to the particle size range in which both can be produced.
  • the mixing ratio of the silver compound and the amine is the ratio of the number of moles of amino groups (mol NH2 ) to the number of moles of silver ions (Ag + ) of the silver compound (mol Ag + ) (mol NH2 / mol Ag + ).
  • the above is preferable. If the amine is insufficient, unreacted silver compounds may remain, and sufficient silver particles cannot be produced, and the particle size distribution of the silver particles varies.
  • the upper limit of the amine addition amount is not particularly limited, but is preferably 6 or less in consideration of the purity of the obtained silver particles.
  • the reaction system in the present invention may be composed of a silver-amine complex and an appropriate range of moisture, and silver particles having a uniform particle diameter can be produced without any other additive.
  • an additive that further stabilizes the complex is not excluded.
  • the additive applicable in the present invention include oleic acid, myristic acid, palmitoleic acid, linoleic acid and the like. These additives have a ratio (mol additive / mol Ag + ) of the number of moles of additive (mol additive ) to the number of moles of silver ion (Ag + ) (mol Ag + ). It is preferable to do this.
  • the reaction system is heated to deposit silver particles after confirming that the water content is in an appropriate range.
  • the heating temperature is preferably equal to or higher than the decomposition temperature of the silver-amine complex.
  • the decomposition temperature of the silver-amine complex varies depending on the type of amine coordinated to the silver compound. When the above-described amine suitable for the present invention is applied, the decomposition temperature is 90 to 130 ° C.
  • the heating rate affects the particle size of the silver particles that are precipitated. That is, in the present invention, the particle size of silver particles can be adjusted by two means: the type of amine that forms a silver-amine complex (the amine that reacts with the silver compound) and the heating rate of the heating step. By these two means, silver particles having a targeted particle diameter can be produced within an average particle diameter of 10 to 200 nm. When the particle size is 10 to 100 nm, it is easy to obtain silver particles having a uniform particle size, and when the particle size is 15 to 50 nm, the particle size is more likely to be uniform.
  • the heating rate in the heating step is preferably adjusted in the range of 2 to 50 ° C./min up to the decomposition temperature. Further, temperature control at 5 ° C./min or more is easy.
  • Silver particles are deposited through the heating step. With respect to this reaction system, silver particles can be taken out through appropriate washing and solid-liquid separation. In some cases, the silver particles may be fixed to each other, but this can be easily crushed and separated. The recovered silver particles can be stored and used in ink, paste, slurry, or dried powder dispersed in an appropriate solvent.
  • the size of the silver particles can be easily controlled. Further, the obtained silver particles are uniform in size.
  • Test No. 1 of the first embodiment SEM photograph of 1 to 4 silver particles. Test No. 1 of the first embodiment. SEM photographs of silver particles 5 and 6. Test No. 1 of the first embodiment. SEM photograph of silver particles 7-11. Test No. 1 of the first embodiment. SEM photograph of 14 silver particles. Test No. 1 of the first embodiment. SEM photographs of 15 and 16 silver particles. Test No. 1 of the first embodiment. SEM photograph of 17-21 silver particles. The particle size distribution figure of the silver particle of Test No.6,10,11 of 1st Embodiment. Test No. 2 of the second embodiment. SEM photograph of 22 silver particles.
  • silver particles were produced while changing various conditions along the process of FIG. 1, and their properties were evaluated.
  • silver oxalate (Ag 2 C 2 O 4 ) (silver ion (Ag + ) 9.9 mmol) or 1.38 g of silver carbonate (Ag 2 CO 3 ) as a thermally decomposable silver compound ( Silver ion (Ag +) 10 mmol) was used.
  • silver oxalate there were prepared a case where it was used in a dry state and a wet state by adding 0.3 g of water (20 parts by weight to 100 parts by weight of silver oxalate). To this silver compound, the amines shown in the following table were added to produce a silver-amine complex. The silver compound and amine were mixed at room temperature and kneaded until a white cream was formed. When oleic acid was used as an additive, it was added to the silver-amine complex prepared above.
  • water was added as necessary to keep the water content within a predetermined range. Specifically, when the water content in the reaction system was 20 parts by weight, the following heating was performed without adding water separately if the raw material was wet silver oxalate (20 parts by weight of water). When the water content of the reaction system was 47 parts by weight using the same raw material, water was added to adjust the water content.
  • the reaction system was heated from room temperature to decompose the silver-amine complex and precipitate silver particles.
  • the heating temperature at this time assumed 110 degreeC as a decomposition temperature of a complex, and made this the ultimate temperature.
  • the heating rate was 10 ° C./min.
  • the present invention is based on a thermal decomposition method in which silver particles are produced by thermal decomposition of a silver-amine complex, but it is essential that a predetermined amount of water be present in the reaction system.
  • the water content of the reaction system Test Nos. 1 to 4 and 7 to 11
  • the size of the silver particles is silver.
  • the object of the present invention to obtain silver particles having a target particle size of about a few dozen to a few tens of nm, limited to fine ones (average particle size less than 10 nm) depending on the type of amine complex I can't.
  • those having an appropriate water content can produce silver particles having a uniform particle size, and the effectiveness of the present invention can be confirmed.
  • water is required, but it can confirm that the upper limit also exists (test No. 3, 4, 10, 11).
  • the amount of water becomes a factor of variation in the particle size.
  • silver particles having a uniform particle size can be produced using an amine having a total number of carbon atoms of alkyl groups of 4 to 10 as an amine for forming a silver-amine complex.
  • an amine having a total number of carbon atoms of alkyl groups of 4 to 10 as an amine for forming a silver-amine complex.
  • a mixed amine of n-hexylamine and n-octylamine is used as the amine (Test No. 6, 12-14)
  • silver particles having a larger particle diameter are produced as the mixing ratio of n-hexylamine is higher. (Test Nos. 6 and 14).
  • silver particles having an intermediate particle size can be produced.
  • the heating rate up to the decomposition temperature is common, it can be confirmed that the particle size can be adjusted by selecting an amine.
  • the amount of amine mixed to produce a silver-amine complex was such that the ratio of the number of moles of amino groups to the number of moles of silver ions was 1.6 or more. Is obtained (Test No. 6).
  • oleic acid which is an additive
  • addition of additives such as an oleic acid, is not essential.
  • Oleic acid is thought to be effective in maintaining a suitable particle size distribution, but suitable silver particles can be produced without the addition of oleic acid.
  • the particle size of silver particles varies depending on the amine for forming a silver-amine complex.
  • the heating rate of the reaction system it is possible to cope with the heating rate of the reaction system as a means for adjusting the particle size. is there. Therefore, next, the above test No.
  • the heating rate was changed about 6 and the silver particle was manufactured.
  • the heating rate is 10 ° C./min, but here the heating rate is 2 ° C./min (Test No. 22).
  • the evaluation results for the silver particles produced here are shown in Table 4.
  • Table 4 shows that the particle size can be adjusted by changing the heating rate. By reducing the heating rate, the particle size of the silver particles tends to increase. As described above, in the present invention, it is possible to adjust the particle size of the silver particles to be manufactured from different approaches of selecting an amine and adjusting the heating rate. Even when the heating rate is adjusted in this way, a good particle size distribution will not be lost.
  • uniform silver particles can be produced while controlling the particle size.
  • the present invention relates to silver particles used in various applications such as electrodes / wiring materials, adhesives / bonding materials, conductive adhesives / conductive bonding materials, thermal conductive materials, reflective film materials, catalysts, antibacterial materials, etc. High quality products can be manufactured.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
PCT/JP2014/063281 2013-05-24 2014-05-20 銀粒子の製造方法 WO2014189025A1 (ja)

Priority Applications (4)

Application Number Priority Date Filing Date Title
CN201480029945.4A CN105263656B (zh) 2013-05-24 2014-05-20 银粒子的制造方法
KR1020157034618A KR102019536B1 (ko) 2013-05-24 2014-05-20 은 입자의 제조 방법
KR1020187009441A KR20180039174A (ko) 2013-05-24 2014-05-20 은 입자의 제조 방법
DE112014002552.6T DE112014002552B4 (de) 2013-05-24 2014-05-20 Verfahren zum Herstellen von Silberteilchen

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JP2013109524 2013-05-24
JP2013-109524 2013-05-24
JP2013-263595 2013-12-20
JP2013263595A JP6189740B2 (ja) 2013-05-24 2013-12-20 銀粒子の製造方法

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MY (1) MY174074A (zh)
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CN105625028A (zh) * 2016-04-01 2016-06-01 吴江市林旺纺织厂 一种防辐射纺织纤维及其制备方法
EP3498398B1 (en) * 2016-08-10 2021-04-14 Bando Chemical Industries, Ltd. Method for producing metallic silver fine particles
CN106601368A (zh) * 2016-12-02 2017-04-26 天津宝兴威科技股份有限公司 一种基于银纳米颗粒墨水在基材表面制备导电膜的方法
CN111565872A (zh) 2018-01-09 2020-08-21 株式会社则武 银纳米微粒的制造方法和包含银纳米微粒的银糊
JP7320515B2 (ja) 2018-08-30 2023-08-03 田中貴金属工業株式会社 低温焼成用の銀インク

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WO2015087967A1 (ja) * 2013-12-11 2015-06-18 田中貴金属工業株式会社 銀粒子の製造方法及び当該方法により製造される銀粒子
JP2015113488A (ja) * 2013-12-11 2015-06-22 田中貴金属工業株式会社 銀粒子の製造方法及び当該方法により製造される銀粒子
US10486235B2 (en) 2013-12-11 2019-11-26 Tanaka Kikinzoku Kogyo K.K. Method for producing silver particles, and silver particles produced by the method

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KR20180039174A (ko) 2018-04-17
DE112014002552T5 (de) 2016-03-10
TWI579074B (zh) 2017-04-21
MY174074A (en) 2020-03-09
TW201509567A (zh) 2015-03-16
JP2015004123A (ja) 2015-01-08
KR102019536B1 (ko) 2019-09-06
KR20160007562A (ko) 2016-01-20
DE112014002552B4 (de) 2020-08-06
JP6189740B2 (ja) 2017-08-30
CN105263656B (zh) 2018-01-23

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