JPS6343469B2 - - Google Patents
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- Publication number
- JPS6343469B2 JPS6343469B2 JP55128408A JP12840880A JPS6343469B2 JP S6343469 B2 JPS6343469 B2 JP S6343469B2 JP 55128408 A JP55128408 A JP 55128408A JP 12840880 A JP12840880 A JP 12840880A JP S6343469 B2 JPS6343469 B2 JP S6343469B2
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- JP
- Japan
- Prior art keywords
- plating
- tank
- fine particles
- dispersed
- dispersion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Description
【発明の詳細な説明】
本発明は、微粒子添加物の分散方法に係り、特
に複合めつき用めつき液に含まれる微粒子添加物
を界面活性剤等の分散剤を用いずに分散させるこ
とができるようにした分散方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for dispersing particulate additives, and in particular, to a method for dispersing particulate additives contained in a plating solution for composite plating without using a dispersant such as a surfactant. Regarding the distribution method that has been made possible.
複合めつきは、電解めつきと異なり、めつき液
に含まれている環元剤によつてめつき材を析出さ
せて、金属の表面にめつき層を形成するめつき法
であり、特に自動車のクラツチ用スプラインシヤ
フト等の擦過腐食を生じ易い摺動を伴なう高速重
荷重を受ける機構部品の表面処理に応用され、そ
の自己潤滑性と耐摩耗性を著しく向上させること
ができるものである。このような大きな特長を示
すのは、めつき材の中に、酸化物、炭化物等のセ
ラミツク又は金属等の微粒子添加物が分散析出し
ているためである。この微粒子添加物は、直径
1μ程度の円形微粒子であつて、高い自己潤滑性
と耐摩耗性を金属めつき層に与えている。 Composite plating, unlike electrolytic plating, is a plating method in which a plating material is deposited using a ring agent contained in a plating solution to form a plating layer on the metal surface. It is applied to the surface treatment of mechanical parts such as spline shafts for clutches that undergo high-speed heavy loads that are subject to sliding movements that are likely to cause scratch corrosion, and can significantly improve their self-lubricating properties and wear resistance. . The reason for this great feature is that particulate additives such as ceramics such as oxides and carbides or metals are dispersed and precipitated in the plating material. This particulate additive has a diameter
They are circular fine particles of approximately 1 μm in size and provide high self-lubricating properties and wear resistance to the metal plating layer.
このような複合めつきを施すには、めつき液に
例えばセラミツクの微粒子添加物を混合して分散
させておき、該めつき液中に被めつき物を所定時
間浸漬してめつき材と微粒子添加物を析出させて
めつき層を形成する。 To perform such composite plating, a fine particle additive of ceramic, for example, is mixed and dispersed in a plating solution, and the object to be plated is immersed in the plating solution for a predetermined period of time to combine with the plating material. A plated layer is formed by precipitating the particulate additive.
しかしめつき液中に混合された微粒子添加物
は、その表面張力によつて、極めて凝集し易く、
従つてこれをめつき液中に均一に分散させておく
ことは技術的に相当困難である。 However, fine particle additives mixed into the plating solution tend to aggregate extremely easily due to their surface tension.
Therefore, it is technically quite difficult to uniformly disperse this in the plating solution.
従来は、例えばニツケルの複合めつきの場合、
硫酸ニツケル（NiSO4）に、セラミツク（SiC）
を微粒子添加物として混合し、更に還元剤である
媒介物質として次亜リン酸ソーダ（NaH2PO2）
を加えてメツキ液とし、該めつき液に、セラミツ
ク（SiC）の凝集を防止して分散させるため界面
活性剤等の分散剤を混合し、めつき槽にエアを吹
き込んで常に撹拌させる方法がとられていた。 Conventionally, for example, in the case of composite plating of nickel,
Ceramic (SiC) on nickel sulfate (NiSO 4 )
is mixed as a particulate additive, and sodium hypophosphite (NaH 2 PO 2 ) is added as a reducing agent and mediator.
is added to form a plating solution, a dispersant such as a surfactant is mixed with the plating solution to prevent the ceramic (SiC) from aggregating and dispersed, and air is blown into the plating tank to constantly stir it. It had been taken.
しかしながら上記従来方法によると、界面活性
剤は老化し易く、またその量が少なかつたり、生
産能率を高めるため、めつき液の温度を少なくと
も60度Ｃ以上、望ましくは90度Ｃ前後まで上げる
と、セラミツク（SiC）を分散させる効果が薄
れ、微粒子１は、第１図に示すように、めつき槽
２のめつき液３内において凝集してしまい、その
結果金属表面に形成されるニツケルめつき層内に
おいて、セラミツク（SiC）の微粒子１は凝集し
た形で部分的に偏在することになり、均質な複合
めつき層を得ることができない欠点があつた。ま
た界面活性剤の量が多くなると、めつきの付着性
が悪化するので、余りその量を多くすることはで
きなかつた。またエアの吹込みのみでは、セラミ
ツク（SiC）の微粒子１を分散させることは不可
能であり、いずれにしても、従来方法では界面活
性剤の使用が不可避であり、甚だ不都合が多かつ
た。また無電解めつき液に超音波振動を与えるよ
うにした特公昭47−12841の発明もあるが、これ
は無電解めつき液に、その還元反応を促進せし
め、生成皮膜内の析出粒子密度、電気伝導度およ
び機械的性能の向上を達成せしめるために200k
〜1MHzの周波数範囲の超音波振動を印加し、さ
らに還元反応を停止せしめる50k〜50Hzの周波数
範囲の超音波振動を印加し、超音波エネルギによ
り反応系を制御する方法であつて、無電解めつき
液の添加微粒子の分散を行うための具体的方法を
何ら開示したものではなかつた。 However, according to the above conventional method, the surfactant ages easily, the amount of surfactant is small, and in order to increase production efficiency, it is necessary to raise the temperature of the plating solution to at least 60 degrees Celsius or higher, preferably around 90 degrees Celsius. , the effect of dispersing ceramic (SiC) is weakened, and the fine particles 1 aggregate in the plating solution 3 of the plating tank 2, as shown in FIG. In the plating layer, the fine particles 1 of ceramic (SiC) are partially unevenly distributed in an aggregated form, which has the disadvantage that a homogeneous composite plating layer cannot be obtained. Furthermore, if the amount of surfactant increases, the adhesion of plating deteriorates, so it was not possible to increase the amount too much. Further, it is impossible to disperse the ceramic (SiC) fine particles 1 by blowing air alone, and in any case, the conventional method requires the use of a surfactant, which is extremely inconvenient. There is also an invention published in Japanese Patent Publication No. 47-12841 in which ultrasonic vibrations are applied to the electroless plating solution. 200k to achieve improved electrical conductivity and mechanical performance
This method involves applying ultrasonic vibrations in the frequency range of ~1 MHz, and then applying ultrasonic vibrations in the frequency range of 50 kHz to 50 Hz to stop the reduction reaction, and controlling the reaction system with ultrasonic energy. This document does not disclose any specific method for dispersing the fine particles added to the soaking liquid.
本発明は、上記した従来技術の欠点を除くため
になされたものであつて、その目的とするところ
は、複合めつき用のめつき液に添加される微粒子
添加物を、界面活性剤等の分散剤を一切用いるこ
となく完全に均一に分散させることができるよう
にすることであり、またこれによつて、被めつき
物表面に形成されるめつき層内に均一に分散した
微粒子添加物が析出存在するようにして、自己潤
滑性、耐摩耗性共に優れた複合めつき層を得るこ
とである。また他の目的は、分散剤を用いないこ
とによつて、めつきの付着性を良好に保つと共
に、めつき液の温度を高く保つことを可能として
生産能率の向上を図ることである。また他の目的
は、めつき液に、めつき槽の外部で、即ちめつき
槽よりも容量の小さい分散槽内で超音波振動を与
えて微粒子を分散させることによつて、少ないエ
ネルギでより有効に該微粒子を分散させることが
できるようにすることである。更に他の目的は、
めつき液をめつき槽の底部から該めつき槽の外部
に設けた分散槽に取り出して微粒子添加物を分散
させた後に、これを再びめつき槽の上部に戻すと
いう循環形態をとることにより、めつき槽におけ
る微粒子添加物の沈殿を予防しつつ微粒子添加物
を最も効率よく分散させることができるようにす
ることである。 The present invention has been made in order to eliminate the above-mentioned drawbacks of the prior art, and its purpose is to reduce the amount of fine particle additives, such as surfactants, added to the plating solution for composite plating. The goal is to be able to completely and uniformly disperse the additives without using any dispersants, and by doing so, the fine particle additives can be uniformly dispersed within the plating layer formed on the surface of the object to be plated. The objective is to obtain a composite plated layer with excellent self-lubricating properties and wear resistance by precipitating out. Another purpose is to improve production efficiency by not using a dispersant to maintain good plating adhesion and to maintain a high temperature of the plating solution. Another purpose is to disperse fine particles with less energy by applying ultrasonic vibration to the plating solution outside the plating tank, that is, in a dispersion tank with a smaller capacity than the plating tank. The object is to enable the fine particles to be effectively dispersed. Yet another purpose is
By taking the plating liquid from the bottom of the plating tank to a dispersion tank installed outside the plating tank and dispersing the particulate additives, the plating solution is returned to the top of the plating tank again. The object of the present invention is to enable the most efficient dispersion of particulate additives while preventing precipitation of the particulate additives in a plating tank.
要するに本発明は、酸化物、炭化物、金属等の
微粒子添加物を含む複合めつき用めつき槽のめつ
き液を、前記めつき槽の底部から該めつき槽より
容量が小さい分散槽に取り出し、この分散槽にお
いて前記めつき液に超音波振動を与えて前記微粒
子添加物を分散させ、然る後に該めつき液を分散
槽から前記めつき槽の上部に戻すことを特徴とす
るものである。 In short, in the present invention, a plating solution in a plating tank for composite plating containing particulate additives such as oxides, carbides, metals, etc. is taken out from the bottom of the plating tank to a dispersion tank having a smaller capacity than the plating tank. , characterized in that the fine particle additive is dispersed by applying ultrasonic vibration to the plating liquid in the dispersion tank, and then the plating liquid is returned from the dispersion tank to the upper part of the plating tank. be.
従つて本発明によれば、めつき液に含まれてい
る微粒子添加物がめつき槽の内部で凝集して底部
に沈殿したとしても、このめつき槽の底部に沈殿
した微粒子添加物が分散槽に取り入れられ、この
分散槽において超音波振動を受けて充分に分散し
た後にめつき槽の上部に戻される。またこのよう
に微粒子添加物を分散させるためにめつき槽に循
環接続されている分散槽の容積をめつき槽の容積
よりも小さくしているために、より少ないエネル
ギでめつき液中の微粒子を効率的に分散させるこ
とができる。 Therefore, according to the present invention, even if the particulate additives contained in the plating solution aggregate and precipitate at the bottom of the plating tank, the particulate additives precipitated at the bottom of the plating tank can be transferred to the dispersion tank. After being sufficiently dispersed by ultrasonic vibration in this dispersion tank, it is returned to the upper part of the plating tank. In addition, since the volume of the dispersion tank, which is connected to the plating tank for circulation in order to disperse the particulate additives, is smaller than the volume of the plating tank, the particulates in the plating solution can be dispersed with less energy. can be efficiently dispersed.
以下本発明を図面を参照しながら詳細に説明す
る。第２図において、分散槽４には、酸化物、炭
化物、金属等、主としてセラミツク（SiC）の微
粒子１の添加物及び還元剤としての次亜リン酸ソ
ーダ（NaH2PO2）を含む硫酸ニツケル（NiSO4）
からなるめつき液３が入れてあり、該分散槽の底
部４ａの下側には、超音波発振装置５が取り付け
てあり、該超音波発振装置から発生する20kHz以
上の超音波振動がめつき液３及びセラミツク
（SiC）の微粒子１に伝わり、該微粒子が超音波
振動してその表面張力による凝集力よりも振動に
より分散しようとする力が勝り、微粒子１は図示
のようにめつき液３中に分散する。分散槽４は、
第３図に示すようなめつき槽６の外部に設けられ
ており、その容量は該めつき槽の容量よりも小さ
くしてあるので、超音波振動のエネルギがより有
効にめつき液３中の微粒子１に作用することとな
り、少ないエネルギで微粒子１を分散させること
ができる。そして分散槽４内で微粒子１が分散し
ためつき液３は、めつき槽６に注入される。この
注入は以下に説明するようにポンプ８を用いて連
続的に行つてもよく、また分散槽４で分散を行う
ごとに、その全量又は一部をめつき槽６に注入す
るようにしてもよい。例えば、めつき液３の微粒
子１の分散処理は、めつき槽６におけるめつき作
業の開始時に１回だけ行うのみでもかなり十分で
あるが、めつき作業の途中で減量した分だけの分
散処理されためつき液３を継ぎ足すようにしても
よい。 The present invention will be explained in detail below with reference to the drawings. In FIG. 2, a dispersion tank 4 contains nickel sulfate containing oxides, carbides, metals, etc., mainly fine particles 1 of ceramic (SiC), and sodium hypophosphite (NaH 2 PO 2 ) as a reducing agent. ( NiSO4 )
An ultrasonic oscillator 5 is attached to the lower side of the bottom 4a of the dispersion tank, and the ultrasonic vibrations of 20 kHz or more generated by the ultrasonic oscillator are applied to the plating liquid 3. 3 and ceramic (SiC) fine particles 1, the fine particles undergo ultrasonic vibration, and the force of dispersion due to the vibration exceeds the cohesive force due to the surface tension, and the fine particles 1 are dispersed in the plating liquid 3 as shown in the figure. dispersed into The dispersion tank 4 is
It is provided outside the plating tank 6 as shown in FIG. 3, and its capacity is smaller than that of the plating tank, so that the energy of the ultrasonic vibrations is more effectively transferred to the plating liquid 3. This acts on the fine particles 1, and the fine particles 1 can be dispersed with a small amount of energy. Then, the plating liquid 3 in which the fine particles 1 are dispersed in the dispersion tank 4 is poured into the plating tank 6. This injection may be carried out continuously using the pump 8 as described below, or the entire amount or a portion thereof may be injected into the plating tank 6 each time dispersion is performed in the dispersion tank 4. good. For example, it is quite sufficient to perform the dispersion treatment of the fine particles 1 in the plating solution 3 only once at the start of the plating operation in the plating tank 6, but the dispersion treatment is performed only for the amount lost during the plating operation. It is also possible to replenish the pampering liquid 3.
上記本発明をめつき作業中に連続的に行うに
は、第３図に示すように、めつき槽６の底部６ａ
にパイプ７を連通接続し、ポンプ８を介して該パ
イプを超音波発振装置５を備えた分散槽４に連通
接続し、ホース９を該分散層の吐出口４ｂに接続
して、該ホースの一端９ａをめつき槽６の上部６
ｂに配置し、該めつき槽の底部６ａからポンプ８
によりめつき液３を吸引して取り出し、分散槽４
に送つて、ここでめつき液３に超音波発信装置５
により超音波振動を与えて微粒子１を分散させ、
しかる後に該めつき液をめつき槽６の上部６ｂに
ホース９で戻すようにしてある。 In order to carry out the above-mentioned invention continuously during plating work, as shown in FIG.
A pipe 7 is connected in communication with the dispersion tank 4 equipped with an ultrasonic oscillator 5 via a pump 8, and a hose 9 is connected to the discharge port 4b of the dispersion layer. One end 9a is plated on the upper part 6 of the tank 6.
b, and a pump 8 is placed from the bottom 6a of the plating tank.
The plating liquid 3 is sucked out and transferred to the dispersion tank 4.
Here, the plating solution 3 is sent to the ultrasonic transmitter 5.
to disperse the fine particles 1 by applying ultrasonic vibration,
Thereafter, the plating liquid is returned to the upper part 6b of the plating tank 6 through a hose 9.
本発明は、上記のように構成されており、以下
その作用について説明する。第３図において、め
つき槽６のめつき液３には、従来方法と異なり、
界面活性剤等の分散剤は混入されていないので、
セラミツク（SiC）の微粒子１は凝集してめつき
槽６の底部６ａに沈殿しようとするが、ポンプ８
により該底部からめつき液３が吸引されて取り出
され、分散槽４に送られ、超音波発振装置５から
超音波振動を与えられて該分散槽で微粒子１は分
散し、それ以後は容易に微粒子１が凝集しない乳
白色のめつき液３となつてホース９によりめつき
槽６の上部６ｂに戻される。従つて、この循環作
用を繰り返していることによつて、めつき液３の
すべてが微粒子１がきれいに分散した乳白色のめ
つき液３となり、該めつき液中に浸漬される被め
つき物１０には、セラミツク（SiC）の微粒子１
が均一に分散した複合めつき層を形成することが
できる。 The present invention is configured as described above, and its operation will be explained below. In FIG. 3, the plating liquid 3 in the plating tank 6 contains, unlike the conventional method,
No dispersants such as surfactants are mixed in, so
Ceramic (SiC) fine particles 1 try to aggregate and settle on the bottom 6a of the plating tank 6, but the pump 8
The plating liquid 3 is sucked out from the bottom and sent to the dispersion tank 4, where ultrasonic vibrations are applied from the ultrasonic oscillator 5 to disperse the fine particles 1. After that, the fine particles 1 are easily dispersed. 1 becomes a milky white plating liquid 3 that does not aggregate and is returned to the upper part 6b of the plating tank 6 through a hose 9. Therefore, by repeating this circulation action, all of the plating liquid 3 becomes a milky white plating liquid 3 in which the fine particles 1 are neatly dispersed, and the object 10 to be plated is immersed in the plating liquid. contains ceramic (SiC) fine particles 1.
It is possible to form a composite plated layer in which the particles are uniformly dispersed.
本発明は、上記のように構成され、作用するも
のであるから、複合めつき用のめつき液に添加さ
れる微粒子添加物を、界面活性剤等の分散剤を一
切用いることなく完全に均一に分散させることが
できる効果が得られる。またこれによつて、被め
つき物表面に形成されるめつき層内に均一に分散
した微粒子添加物が析出存在することになるの
で、自己潤滑性、耐摩耗性共に優れた複合めつき
層を得ることができる効果が得られる。更には、
界面活性剤等の分散剤が一切不要となるので、め
つきの付着性を良好に保つことができ、かつめつ
き液の温度を高くすることができるので、生産能
率の向上を図ることができる効果が得られる。ま
ためつき液に、めつき槽の外部で、即ちめつき槽
よりも容量の小さい分散槽内で超音波振動を与え
て微粒子を分散させるようにしたので、少ないエ
ネルギでより有効に該微粒子を分散させることが
できる効果がある。まためつき液をめつき槽の底
部から取り出してめつき槽の外部で微粒子添加物
を分散させて後めつき液槽の上部に戻すようにし
たので、微粒子添加物の沈澱を防止し、最も効率
的に微粒子添加物を分散させることができる効果
が得られる。 Since the present invention is constructed and operates as described above, the fine particle additives added to the plating solution for composite plating can be completely uniformly added without using any dispersants such as surfactants. This provides the effect of being able to be dispersed into In addition, as a result of this, evenly dispersed fine particle additives are precipitated in the plating layer formed on the surface of the plated object, so the composite plating layer has excellent self-lubricating properties and wear resistance. The effect that can be obtained is obtained. Furthermore,
Since dispersants such as surfactants are not required at all, it is possible to maintain good adhesion of plating, and the temperature of the plating liquid can be raised, which has the effect of improving production efficiency. is obtained. In addition, the fine particles are dispersed by applying ultrasonic vibration to the plating solution outside the plating tank, that is, in a dispersion tank with a smaller capacity than the plating tank, so the fine particles can be dispersed more effectively with less energy. It has the effect of being able to be dispersed. In addition, the plating solution is taken out from the bottom of the plating tank, the particulate additives are dispersed outside the plating tank, and the particulate additives are then returned to the top of the plating tank, which prevents the particulate additives from settling. The effect of efficiently dispersing the particulate additive can be obtained.
実施例 １
硫酸ニツケル（NiSO4）に、還元剤としての媒
介物質として次亜リン酸ソーダ（NaH2PO2）を
混合し、これに直径1μ程度のセラミツク（SiC）
の微粒子を添加して複合めつき用のめつき液を作
り、これを容器に入れてその底部から超音波発振
装置により45kHzの超音波振動を１分間与えたと
ころ、ベージユ色に容器底部に凝集沈澱していた
微粒子が完全に分散し、めつき液は乳白色とな
り、従来の複合めつき用のめつき液と全く異な
り、これを３日乃至４日間放置しても微粒子の凝
集や沈澱は生ぜず、めつき液は乳白色のままであ
つた。Example 1 Sodium hypophosphite (NaH 2 PO 2 ) is mixed with nickel sulfate (NiSO 4 ) as a mediating substance as a reducing agent, and ceramic (SiC) with a diameter of about 1 μ is mixed with this mixture.
A plating solution for composite plating was made by adding fine particles of The precipitated fine particles are completely dispersed, and the plating solution becomes milky white, which is completely different from the plating solution for conventional composite plating, and even if it is left for 3 to 4 days, no agglomeration or precipitation of the fine particles occurs. However, the plating solution remained milky white.
第１図は微粒子添加物が凝集した状態を示すめ
つき槽の縦断面図、第２図は本発明方法を用いて
微粒子添加物を分散させた状態を示す分散槽の縦
断面図、第３図は本発明方法を実施するための装
置の概略縦断面図である。
１は微粒子、３はめつき液、４は分散層、５は
超音波発振装置、６はめつき槽、６ａは底部、６
ｂは上部、７はパイプ、８はポンプ、９はホー
ス、１０は被めつき物である。
FIG. 1 is a longitudinal sectional view of a plating tank showing a state in which particulate additives are aggregated; FIG. 2 is a longitudinal sectional view of a dispersion tank showing a state in which particulate additives are dispersed using the method of the present invention; The figure is a schematic longitudinal sectional view of an apparatus for carrying out the method of the invention. 1 is fine particles, 3 is a plating liquid, 4 is a dispersion layer, 5 is an ultrasonic oscillator, 6 is a plating tank, 6a is a bottom, 6
b is the upper part, 7 is a pipe, 8 is a pump, 9 is a hose, and 10 is a covered item.
Claims (1)
む複合めつき用めつき層のめつき液を、前記めつ
き槽の底部から該めつき槽より容量が小さい分散
槽に取り出し、該分散槽において前記めつき液に
超音波振動を与えて前記微粒子添加物を分散さ
せ、しかる後に該めつき液を分散槽から前記めつ
き槽の上部に戻すことを特徴とする微粒子添加物
の分散方法。1. A plating solution for a plating layer for composite plating containing particulate additives such as oxides, carbides, metals, etc. is taken out from the bottom of the plating tank to a dispersion tank having a smaller capacity than the plating tank, and the dispersion tank A method for dispersing particulate additives, which comprises applying ultrasonic vibration to the plating liquid to disperse the particulate additives, and then returning the plating liquid from the dispersion tank to the upper part of the plating tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12840880A JPS5754262A (en) | 1980-09-17 | 1980-09-17 | Dispersion of fine particle additive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12840880A JPS5754262A (en) | 1980-09-17 | 1980-09-17 | Dispersion of fine particle additive |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5754262A JPS5754262A (en) | 1982-03-31 |
| JPS6343469B2 true JPS6343469B2 (en) | 1988-08-30 |
Family
ID=14984036
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12840880A Granted JPS5754262A (en) | 1980-09-17 | 1980-09-17 | Dispersion of fine particle additive |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5754262A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5923861A (en) * | 1982-07-29 | 1984-02-07 | Hino Motors Ltd | Recirculation plating method and apparatus |
-
1980
- 1980-09-17 JP JP12840880A patent/JPS5754262A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5754262A (en) | 1982-03-31 |
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