EP3725921A1 - Procédé de raffinage de grains cristallins dans un film de placage - Google Patents

Procédé de raffinage de grains cristallins dans un film de placage Download PDF

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Publication number
EP3725921A1
EP3725921A1 EP18887864.9A EP18887864A EP3725921A1 EP 3725921 A1 EP3725921 A1 EP 3725921A1 EP 18887864 A EP18887864 A EP 18887864A EP 3725921 A1 EP3725921 A1 EP 3725921A1
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EP
European Patent Office
Prior art keywords
plating
nanocarbon
plating film
crystal grains
film
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.)
Withdrawn
Application number
EP18887864.9A
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German (de)
English (en)
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EP3725921A4 (fr
Inventor
Mikiharu TAKAGI
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Individual
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Publication of EP3725921A1 publication Critical patent/EP3725921A1/fr
Publication of EP3725921A4 publication Critical patent/EP3725921A4/fr
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/60—Electroplating characterised by the structure or texture of the layers
    • C25D5/615—Microstructure of the layers, e.g. mixed structure
    • C25D5/617—Crystalline layers
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/30—Electroplating: Baths therefor from solutions of tin
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/46—Electroplating: Baths therefor from solutions of silver
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/48—Electroplating: Baths therefor from solutions of gold

Definitions

  • the present invention relates to a method for forming reduced-size crystal grains of a plating film.
  • Patent Document 1 mentions a zinc-nanocarbon composite plating.
  • a zinc plating film is formed on a plating object by using a zinc plating solution into which nanocarbon and polyacrylamide as a dispersion agent for the nanocarbon have been added.
  • Patent Document 1 also mentions that it is preferable that nanocarbon be present in the zinc plating film and that the amount of nanocarbon added into the zinc plating solution be 0.5 to 5.0 g/L. Furthermore, Patent Document 1 indicates that because part of the nanocarbon is exposed out of the zinc plating film, a zinc plating film excellent in sliding characteristic can be made.
  • Patent Document 1 JP 2008-214667A
  • incorporation of nanocarbon into a plating film will reform the surface of the plating film.
  • the incorporation of nanocarbon into the plating film is considered to harden the plating film and improve the anti-abrasion property associated with sliding.
  • the anti-abrasion property of the plating film is not a simple property that depends only on the hardness of the plating film but is affected compositively by carious elements such as the surface roughness (sliding property) and lubricity of plating, and the toughness and crystal grain size of plating metal.
  • a representative construction of a crystal grain size reduction method for a plating film according to the present invention is characterized by performing electroplating in a condition where ions of a plating metal, a nanocarbon, and an anion based surfactant as a dispersion agent for dispersing the nanocarbon have been blended in a plating solution.
  • the nanocarbon is dispersed in the plating solution with molecules of the dispersion agent adsorbed to the nanocarbon. Due to the use of an anion based surfactant as a dispersion agent, the nanocarbon dispersed in the plating solution is not readily incorporated into the surfaces of parts to be plated (plating objects) that are connected to the negative electrode. On the surfaces of the plating objects, epitaxial growth of the plating metal proceeds to form crystal grains. The nanocarbon affects the epitaxial growth of the plating metal so as to reduce the size of the crystal grains of the plating film.
  • the present invention realizes reform of the surface of a plating film by reducing the size of crystal grains of the plating film without substantial incorporation of nanocarbon into the plating film.
  • the nanocarbon be positively charged when in a state of mixture with the plating solution. It is speculated that the nanocarbon positively charged in the plating solution, despite molecules of the anion based surfactant being adsorbed to nanocarbon particles, is attracted to the surface of the part to be plated that is connected to the negative electrode. Due to the attraction to the surface of the part to be plated, the nanocarbon particles can certainly come into contact with and exert forces to crystal grains of the plating film, reliably reducing the size of the crystal grains of the plating film.
  • the particle diameter of the nanocarbon be 2.6 ⁇ 0.5 nm. With the particle diameter of the nanocarbon being in this range, the nanocarbon particles in the plating solution certainly undergo Brownian motion and, when contacting crystal grains of the plating film, exert to the crystal grains appropriate forces that reduces the size of the crystal grains. A reason why the size reduction of the crystal grains becomes insufficient if the particle diameter of the nanocarbon is above the aforementioned range is speculated to be that the Brownian motion of the nanocarbon particles is not sufficient and therefore cannot exert appropriate forces to the crystal grains.
  • the amount of the nanocarbon added into the plating solution be less than or equal to 0.2 g/L.
  • the amount of the nanocarbon added into the plating solution be less than or equal to 0.2 g/L.
  • the plating metal be silver (Ag), nickel (Ni), tin (Sn), or gold (Au). Therefore, the plating solution that is neutral or weakly acidic may be used.
  • the present invention it is possible to provide a crystal grain size reduction method for a plating film which is capable of reforming a surface of a plating film without substantial incorporation of nanocarbon into the plating film.
  • Fig. 1 generally illustrates a crystal grain size reduction method for a plating film according to an exemplary embodiment.
  • the size reduction method of this exemplary embodiment is carried out by, for example, using a plating apparatus 100.
  • the plating apparatus 100 is an apparatus for carrying out electroplating and includes a container 102, a plating solution 104 in the container 102, a negative electrode 106 and a positive electrode 108 immersed in the plating solution 104, and an electricity source 110 that applies voltage between the two electrodes.
  • Blended in the plating solution 104 are ions of a plating metal 112, a nanocarbon 114, and a dispersion agent 116.
  • the plating metal 112 in this example is a monovalent cation of silver (Ag).
  • the dispersion agent 116 used in this example is an anion based surfactant. As illustrated in Fig. 1 , when molecules of the surfactant are adsorbed to a nanocarbon particle 114, the liphophilic group 118b of each surfactant molecule becomes attached to the nanocarbon particle 114, with the hydrophilic group 118a of each surfactant molecule positioned outward. Therefore, the nanocarbon particles 114 do not aggregate but are dispersed in the plating solution 104 due to the dispersion agent 116.
  • the amount added to the plating solution 104 was set to 0.2 g/L, and the particle diameter of the nanocarbon 114 was set to 2.6 ⁇ 0.5 nm. Furthermore, the nanocarbon particles 114 in a mixture with the plating solution 104 are positively charged. The plating solution 104 is neutral because the plating metal 112 is silver (Ag).
  • Figs. 2A and 2B show microscopic photographs of a plating film 122 formed as illustrated in Fig. 1 and a plating film 122A formed as a comparative example.
  • the plating film 122 shown in Fig. 2A was obtained by adding the nanocarbon 114 into the plating solution 104 according to the crystal grain size reduction method of the exemplary embodiment.
  • the plating film 122A of the comparative example shown in Fig. 2B was obtained without adding the nanocarbon 114 into the plating solution 104.
  • the crystal grain size reduction method of this exemplary embodiment is capable of reducing the size of the crystal grains (forming nanocrystal grains) of the plating film 122.
  • Table 1 presented below, compares the carbon contents of the plating films 122 and 122A. Table 1 Addition of nanocarbon Carbon content of plating film (mass%) No 0.00182 Yes 0.00178
  • the carbon content of the plating film 122 according to this exemplary embodiment in which the nanocarbon 114 was added was substantially the same as the carbon content of the plating film 122A of the comparative example in which the nanocarbon 114 was not added.
  • the plating film 122 formed by the crystal grain size reduction method of the exemplary embodiment did not substantially incorporate the nanocarbon 114.
  • size reduction of the crystal grains of the plating film 122 is achieved by the nanocarbon 114 functioning as if it was a catalyst, without substantial incorporation of the nanocarbon into the plating film 122. This phenomenon will be discussed below.
  • the nanocarbon 114 dispersed in the plating solution 104 is not readily incorporated into the plating film 122 on the surface of the plating object 120 that is connected to the negative electrode 106 because an anion based surfactant is used as the dispersion agent 116.
  • the amount of the nanocarbon 114 added is as small as 0.2 g/L, incorporation of the nanocarbon 114 into the plating film 122 does not easily occur in the first place.
  • the nanocarbon 114 was, actually, hardly incorporated into the plating film 122.
  • the molecules of the anion based surfactant adsorbed to the nanocarbon particles 114 do not prevent the nanocarbon particles 114 from being attracted to the surface of the plating object 120 connected to the negative electrode 106, so that the nanocarbon particles 114 affect the epitaxial growth of the plating metal 112.
  • the behavior of the nanocarbon particles 114 during this process is not clearly known, it can be speculated that, due to the Brownian motion in the plating solution 104, the nanocarbon particles 114 come into contact with and exert forces to crystal grains, thereby achieving size reduction of the crystal grains. Specifically, it can be speculated that the positively charged nanocarbon 114 in the plating solution 104 is attracted to the surface of the plating object 120 so as to certainly come into contact with and exert forces to crystal grains of the plating film, so that the crystal grains of the plating film can be certainly reduced in size.
  • the particle diameter of the nanocarbon 114 is set within the range of 2.6 ⁇ 0.5 nm, the particles of the nanocarbon 114 in the plating solution 104 certainly undergo Brownian motion, so that as nanocarbon particles 114 come into contact with crystal grains of the plating film, the nanocarbon particles 114 exert to the crystal grains appropriate forces that reduce the size of the crystal grains.
  • a reason why the size reduction of the crystal grains becomes insufficient if the particle diameter of the nanocarbon 114 is above the aforementioned range is speculated to be that the Brownian motion of the nanocarbon particles is not sufficient and therefore cannot exert appropriate forces to the crystal grains.
  • the plating object 120 provided with the plating film 122 is used as an electrical contact. Therefore, the plating film 122 is required to have a low electric resistivity (contact resistance). Furthermore, since the plating object 120 is repeatedly inserted into a socket or the like, the plating film 122 is also required to be high in durability (i.e., the anti-abrasion property associated with sliding).
  • FIGS. 3A and 3B are schematic diagrams that correspond to the plating films 122 and 122A shown in Figs. 2A and 2B .
  • the metal can be viewed as a crystal grain aggregate which includes crystal grains and grain boundaries that surround the crystal grains (defects of crystals or impurities) and in which crystal grains are bound to each other at grain boundaries.
  • the abrasion of metal caused by sliding occurs in two different ways: crystal grains themselves undergo transgranular fracture; and boundaries fracture and the metal chips and erodes in block units of crystal grains.
  • it is an object to restrain the grain boundary fracture in which the metal chips off grain by grain and therefore increase the durability.
  • the chipped-off volume that is, the amount of erosion
  • erosion of a small crystal grain means a small amount of erosion.
  • crystal structure features of a metal that are needed in order to realize a highly durable plating film are that the crystal grains are small and that the binding force at grain boundaries that binds crystal grains together is strong.
  • the crystal grains 124 are smaller than the crystal grains 124A of the plating film 122A illustrated in Fig. 3B and the grain boundaries 126 where crystal grains 124 are bound together outnumber the grain boundaries 126A of the plating film 122A. Therefore, the plating film 122 is less easily erodable to sliding and therefore more durable than the plating film 122A.
  • the plating film 122A of the comparative example, in which the crystal grains 124A were not reduced in size had a Vickers hardness of 90 to 110 Hv.
  • the plating film 122 of the exemplary embodiment, in which the crystal grains 124 were reduced in size had a Vickers hardness of 100 to 110 Hv, making it clear that size reduction of the crystal grains 124 does not make the plating film 122 harder.
  • the electrical contact resistance of the plating film 122 will be described. It is considered that when the crystal grains of metal are made smaller, grain boundaries generally increase, so that the electrical contact resistance increases. However, in the plating film 122 according to the exemplary embodiment, although the crystal grains 124 are small, the contact resistance is not high but about 3 ⁇ 10 -6 to about 3.5 ⁇ 10 -6 ⁇ cm. Incidentally, the contact resistance of a super hard silver plating that has substantially the same crystal grain diameter is as high as greater than or equal to 8 ⁇ 10 -6 ⁇ cm.
  • Figs. 4A and 4B are graphs indicating the durability and the contact resistance of the plating films 122 and 122A illustrated in Figs. 2A and 2B , respectively.
  • the horizontal axis represents the number of back-and-forth movements (number of sliding movements) and the vertical axis represents the friction force (N) or the resistance value (m ⁇ ).
  • N the friction force
  • m ⁇ the resistance value
  • the plating film 122 described in Fig. 4A produces a smaller friction force as a whole than the plating film 122A described in Fig. 4B , and therefore is higher in anti-abrasion property. In fact, the plating film 122 remained unfractured even when the number of back-and-force movements reached 1000. On the other hand, the plating film 122A, being low in anti-abrasion property, was destroyed as exhibited in Fig. 4B when the number of back-and-force movements was about 600. Furthermore, the plating film 122 exhibited stable electrical resistance at low resistance values, compared with the plating film 122A. On the other hand, the plating film 122A exhibited unstable electrical resistance values as a whole. Furthermore, the resistance value of the plating film 122A rapidly increased as the plating film 122A was fractured at the time of about 600 back-and-forth movements.
  • the plating film 122 formed by the crystal grain size reduction method according to the exemplary embodiment was lower in contact resistance and higher in durability than the plating film 122A of the comparative example, in which nanocarbon 114 was not added into the plating solution 104. That is, in the crystal grain size reduction method according to the exemplary embodiment, reform of the surface of the plating film 122 is realized by reducing the size of the crystal grains of the plating film 122 without substantial incorporation of the nanocarbon 114 into the plating film 122 although the nanocarbon 114 is added into the plating solution 104.
  • Examples and comparative examples in which different amounts of the nanocarbon 114 were added will be described below.
  • Table 2 describes Examples 1 and 2 and Comparative Examples 1 and 2.
  • the amounts of the nanocarbon 114 added were 0.1 g/L and 0.2 g/L, respectively.
  • Comparative Example 1 the amount of the nanocarbon 114 added was zero, that is, no nanocarbon 114 was added.
  • Comparative Example 2 the amount of the nanocarbon 114 added was 0.3 g/L.
  • Table 2 The amount of nanocarbon added (g/L) Evaluations Size of crystal grains Anti-abrasion property Volume resistance Comparative Example 1 0 Large No good and soft Low Example 1 0.1 Quite small Acceptable Low Example 2 0.2 Quite small Acceptable Low Comparative Example 2 0.3 or larger Intermediate Acceptable High
  • Figs. 5A and 5B show microscopic photographs exhibiting a plating film 128 according to another exemplary embodiment and a plating film 128A of another comparative example.
  • the plating film 128 according to the another exemplary embodiment exhibited in Fig. 5A is different from the above-described plating film 122 in that the plating metal 112 of the plating film 128 was nickel (Ni) instead of silver (Ag).
  • the plating film 128A of the another comparative example exhibited in Fig. 5B was obtained by using as the plating metal 112 nickel (Ni) instead of silver (Ag) and by omitting addition of the nanocarbon 114 into the plating solution 104. Note that, due to the use of nickel (Ni) as a plating metal, the plating solution 104 was weakly acidic.
  • the plating film 128A of the comparative example was formed by blending nickel sulfamate in the plating solution 104 and omitting addition of the nanocarbon 114 into the plating solution 104. As indicated in Table 3, the plating film 128A was subjected to repeated sliding with a load of 50 g and was destroyed when the number of sliding cycles reached, averagely, 425.4.
  • the plating film 128 according to the another exemplary embodiment was formed by blending nickel sulfamate in the plating solution 104 and adding the nanocarbon 114 into the plating solution 104. As indicated in Table 3, the plating film 128 was destroyed when the number of sliding movements reached, averagely, 523.2. This clarifies that the plating film 128 was more durable than the plating film 128A of the another comparative example.
  • reform of the surfaces of the plating films 122 and 128 can be realized by making the crystal grains of the plating films 122 and 128 quite small without incorporation of the nanocarbon 114 into the plating films 122 and 128, respectively.
  • the plating metal 112 is silver (Ag) or nickel (Ni) as an example, this is not restrictive.
  • the plating metal 112 may also be tin (Sn) or gold (Au).
  • the crystal grains of the plating film can be made quite small to reform the surface of the plating film by causing the nanocarbon 114 to function as if the nanocarbon 114 was a catalyst, while avoiding incorporation of the nanocarbon 114 into the plating film.
  • the invention can be utilized as a method for forming reduced-size crystal grains of a plating film.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
EP18887864.9A 2017-12-15 2018-12-14 Procédé de raffinage de grains cristallins dans un film de placage Withdrawn EP3725921A4 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2017240928A JP2021042397A (ja) 2017-12-15 2017-12-15 めっき皮膜の結晶粒の微細化方法
PCT/JP2018/046031 WO2019117279A1 (fr) 2017-12-15 2018-12-14 Procédé de raffinage de grains cristallins dans un film de placage

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EP3725921A1 true EP3725921A1 (fr) 2020-10-21
EP3725921A4 EP3725921A4 (fr) 2021-01-27

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EP18887864.9A Withdrawn EP3725921A4 (fr) 2017-12-15 2018-12-14 Procédé de raffinage de grains cristallins dans un film de placage

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US (1) US20210156044A1 (fr)
EP (1) EP3725921A4 (fr)
JP (1) JP2021042397A (fr)
CN (1) CN111511964A (fr)
WO (1) WO2019117279A1 (fr)

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Publication number Priority date Publication date Assignee Title
US3371020A (en) * 1964-12-14 1968-02-27 Union Carbide Corp Process for the electrodeposition of metals
JP3913118B2 (ja) * 2002-06-13 2007-05-09 忠正 藤村 超微粒ダイヤモンド粒子を分散した金属薄膜層、該薄膜層を有する金属材料、及びそれらの製造方法
WO2005056885A1 (fr) * 2003-12-08 2005-06-23 Toyo Kohan Co., Ltd. Tole d'acier plaquee de metal destinee a un boitier d'accumulateur, boitier d'accumulateur utilisant cette tole d'acier plaque et accumulateurs utilisant ce boitier
JP5041809B2 (ja) * 2004-04-30 2012-10-03 東洋鋼鈑株式会社 電池容器用めっき鋼板、その製造方法、その電池容器用めっき鋼板を用いた電池容器およびその電池容器を用いた電池
US7320832B2 (en) * 2004-12-17 2008-01-22 Integran Technologies Inc. Fine-grained metallic coatings having the coefficient of thermal expansion matched to the one of the substrate
JP2008214667A (ja) 2007-02-28 2008-09-18 Shinshu Univ 亜鉛−ナノカーボン複合めっき物およびその製造方法
JP5435477B2 (ja) * 2010-01-22 2014-03-05 アイテック株式会社 ダイヤモンド微粒子を分散させた複合めっき液及びその製造方法
JP5857339B2 (ja) * 2012-03-07 2016-02-10 国立大学法人信州大学 Ｎｉ−Ｗ合金／ＣＮＴ複合めっき方法およびＮｉ−Ｗ合金／ＣＮＴ複合めっき液
CN102703943B (zh) * 2012-05-23 2016-04-13 江苏仪征金派内燃机配件有限公司 一种纳米复合表面活塞环的生产方法
CN103469264B (zh) * 2013-09-16 2015-10-21 中国电子科技集团公司第三十八研究所 电镀沉积制备纳米晶结构金锡合金镀层的方法
JP6536819B2 (ja) * 2015-12-03 2019-07-03 トヨタ自動車株式会社 銅皮膜の成膜方法

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CN111511964A (zh) 2020-08-07
WO2019117279A1 (fr) 2019-06-20
US20210156044A1 (en) 2021-05-27
EP3725921A4 (fr) 2021-01-27
JP2021042397A (ja) 2021-03-18

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