JPH0248635B2 - TETSU * RINDENKIMETSUKYOKU - Google Patents
TETSU * RINDENKIMETSUKYOKUInfo
- Publication number
- JPH0248635B2 JPH0248635B2 JP11963789A JP11963789A JPH0248635B2 JP H0248635 B2 JPH0248635 B2 JP H0248635B2 JP 11963789 A JP11963789 A JP 11963789A JP 11963789 A JP11963789 A JP 11963789A JP H0248635 B2 JPH0248635 B2 JP H0248635B2
- Authority
- JP
- Japan
- Prior art keywords
- iron
- phosphorus
- plating
- bath
- phosphite
- 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.)
- Expired - Lifetime
Links
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 65
- 238000007747 plating Methods 0.000 claims description 39
- 229910052742 iron Inorganic materials 0.000 claims description 36
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 28
- 229910052698 phosphorus Inorganic materials 0.000 claims description 27
- 239000011574 phosphorus Substances 0.000 claims description 27
- -1 iron ions Chemical class 0.000 claims description 14
- 238000009713 electroplating Methods 0.000 claims description 11
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims description 9
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 9
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 4
- 229910000838 Al alloy Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 235000019270 ammonium chloride Nutrition 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
- 239000004327 boric acid Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910017855 NH 4 F Inorganic materials 0.000 description 1
- 235000002597 Solanum melongena Nutrition 0.000 description 1
- 244000061458 Solanum melongena Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000009661 fatigue test Methods 0.000 description 1
- 229960002089 ferrous chloride Drugs 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- SQZYOZWYVFYNFV-UHFFFAOYSA-L iron(2+);disulfamate Chemical compound [Fe+2].NS([O-])(=O)=O.NS([O-])(=O)=O SQZYOZWYVFYNFV-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- DPTATFGPDCLUTF-UHFFFAOYSA-N phosphanylidyneiron Chemical compound [Fe]#P DPTATFGPDCLUTF-UHFFFAOYSA-N 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 description 1
- AQSJGOWTSHOLKH-UHFFFAOYSA-N phosphite(3-) Chemical class [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 description 1
- 241000894007 species Species 0.000 description 1
- NCPXQVVMIXIKTN-UHFFFAOYSA-N trisodium;phosphite Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])[O-] NCPXQVVMIXIKTN-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Electroplating And Plating Baths Therefor (AREA)
Description
〔産業上の利用分野〕
本発明は、クラツクの生じない鉄・リンめつき
被膜を得ることができる鉄・リン電気めつき浴に
関する。
〔従来の技術〕
鉄・リンめつき被膜は、鉄めつき被膜に比べて
硬度が大きく、このためピストンのスカート部な
どの摺動部材に鉄・リンめつき被膜を形成するこ
とにより、耐摩耗性、耐焼付性などを向上させる
ことが期待できるものである。
従来、かかる鉄・リンめつき被膜を形成するた
めの鉄・リン電気めつき浴としては、２価の鉄イ
オンと次亜リン酸又はその塩とを含み、更にホウ
酸や塩化アンモニウム等を含むものが知られてい
る。
〔発明が解決しようとする課題〕
しかし、本発明者らの検討によると、この種の
めつき浴を用いて鉄・リン電気めつきを行つた場
合、得られる鉄・リンめつき被膜の断面に多数の
クラツクが生じ、このクラツクが特に機械的性能
を要求する応用面では大きな障害となることを知
見した。即ち、クラツクの発生した鉄・リンめつ
き被膜はそれ自体のじん性が著しく低い上、クサ
ビ（ノツチ）効果によりめつきが施された素材そ
のもののじん性を低下させるものであつた。
このため、かかるクラツクのない鉄・リンめつ
き被膜を得ることができる鉄・リン電気めつき浴
が望まれる。
課題を解決するための手段及び作用
本発明者らは、上記要望に応えるため検討を進
めた結果、２価の鉄イオンと亜リン酸及び／又は
亜リン酸塩とを主成分とし、更に水溶性アルミニ
ウム化合物を添加しためつき浴を用いた場合、得
られる鉄・リンめつき被膜はクラツクがなく、機
械的特性に優れており、このため摺動部材などに
鉄・リンめつき被膜を形成させるためのめつき浴
として非常に有効であることを知見した。
即ち、従来は上述したようにリン供給源として
次亜リン酸や次亜リン酸塩を用いためつき浴を使
用しており、この種のめつき浴は光沢のあるめつ
き被膜が得られるものであるが、その断面を観察
するとクラツクが多数発生しているものであつ
た。しかし、リン供給源として亜リン酸や亜リン
酸塩を使用し、更にアルミニウム化合物を添加し
た場合、断面にクラツクのない鉄・リンめつき被
膜を確実に形成し得ることを見い出し、本発明を
なすに至つたものである。
以下、本発明につき更に詳しく説明する。
本発明に係る鉄・リン電気めつき浴は、２価の
鉄イオンと、亜リン酸及び／又は亜リン酸塩を主
成分としてなるものである。
ここで、２価の鉄イオンの供給源は特に制限さ
れないが、例示すると硫酸第１鉄、塩化第１鉄、
スルフアミン酸第１鉄、ホウフツ化第１鉄などを
挙げることができ、これらの１種を単独で又は２
種以上を併用して使用することができる。また、
２価の鉄イオンの含有量も必ずしも限定されない
が、めつき浴１当り20〜80ｇとすることが好ま
しい。
本発明においては、鉄・リンめつき被膜に対す
るリンの供給源として亜リン酸及び／又は亜リン
酸塩を使用するもので、これにより上述したよう
にクラツクのない鉄・リンめつき被膜を得ること
ができるものである。この場合、亜リン酸や亜リ
ン酸塩の含有量は、要求する鉄・リンめつき被膜
のリン含量等により相違し、また亜リン酸や亜リ
ン酸塩のめつき浴に対する溶解度によつて制限さ
れるが、通常めつき浴１当りNaH2PO3・
2H2Oとして0.01〜20ｇ、特に0.1〜10ｇとするこ
とが好ましい。本発明浴によれば、亜リン酸や亜
リン酸塩の含有量を変えることにより、通常0.05
〜10％のリン含量を有する鉄・リンめつき被膜を
得ることができる。なお、亜リン酸塩としては、
亜リン酸ナトリウム等が使用し得る。
本発明に係るめつき浴には、上述した成分に加
え、更に硫酸アルミニウム、塩化アルミニウム等
のアルミニウム化合物を添加するもので、めつき
浴中にアルミニウムイオンを含有させることによ
り、クラツクの発生を更に確実に防止することが
できる。アルミニウム化合物の添加量は、アルミ
ニウムイオンとしてめつき液１当り好ましくは
0.05〜５ｇ、特に0.1〜２ｇを添加することがで
きる。
なお、めつき浴には、必要によつては電導度塩
として硫酸アンモニウム、塩化アンモニウム等を
０〜200ｇ／、特に20〜150ｇ／、PH緩衝剤と
してホウ酸等を０〜60ｇ／、特に20〜50ｇ／
、３価の鉄イオンの錯化剤として酸性フツ化ア
ンモニウム等を０〜20ｇ／、特に１〜10ｇ／
添加することができる。また、本発明めつき浴の
PHは0.5〜3.5とすることが好ましい。
上述した鉄・リン電気めつき浴を用いて所望の
被めつき物をめつきする場合、浴温は室温〜80
℃、特に30〜70℃とすることができ、また陰極電
流密度は0.5〜30A／ｄm2、特に２〜20A／ｄm2と
することができる。更に、攪拌は必ずしも必要と
しないが、カソードロツカー、スターラーによる
浴攪拌を採用することもできる。
なお、陽極には一般に鉄板が用いられる。
〔発明の効果〕
本発明の鉄・リン電気めつき浴を使用して得ら
れる鉄・リンめつき被膜の外観は、一般に半光沢
の均一な面であり、また得られためつき被膜はク
ラツクがなく、機械的特性に優れたものであるの
で、例えばピストンのスカート部などの摺動部材
その他のめつきに好適に用いられる。
以下、実施例と比較例を示し、本発明を具体的
に説明するが、本発明は下記の実施例に制限され
るものではない。
〔実施例〕
FeCl2・4H2O 220ｇ／
NH4F・HF 10 〃
Al2（SO4）3・14−18H2O ５ 〃
H3PO3 1.5 〃
PH 1.2
次に、上記めつき浴を使用し、浴温60℃、Dk
4A／ｄm2の条件において公知の方法により前処
理したAC8A・T6のアルミニウム合金に20μの
鉄・リン電気めつきを施した。
また比較のため、下記比較例のめつき浴を使用
し、浴温55℃、Dk 10A／ｄm2の条件でAC8A・
T6のアルミニウム合金に20μの鉄・リン電気めつ
きを施した。
〔比較例〕
FeCl2・4H2O 80ｇ／
FeSO4・7H2O 100 〃
NaH2PO2・H2O 10 〃
PH 1.4
得られた鉄・リンめつき被膜の外観、硬度、リ
ン含量を第１表に示す。
また、めつき被膜を切断し、その切断面を５％
ナイタールにて２秒間エツチングした後、金属顕
微鏡（倍率400倍）にてクラツクの有無を調べた。
結果を第１表に併記する。
[Industrial Field of Application] The present invention relates to an iron/phosphorous electroplating bath capable of obtaining an iron/phosphorous plating film without cracks. [Conventional technology] Iron/phosphorus plating has a higher hardness than iron plating. Therefore, forming an iron/phosphorus plating on sliding parts such as the piston skirt improves wear resistance. It can be expected to improve properties such as hardness and seizure resistance. Conventionally, iron/phosphorous electroplating baths for forming such iron/phosphorus plating films contain divalent iron ions and hypophosphorous acid or its salts, and further contain boric acid, ammonium chloride, etc. something is known. [Problems to be Solved by the Invention] However, according to studies by the present inventors, when iron/phosphorus electroplating is performed using this type of plating bath, the cross section of the iron/phosphorus plating film obtained is It was discovered that many cracks were generated in the process, and that these cracks were a major hindrance especially in applications requiring mechanical performance. That is, the cracked iron/phosphor plating film itself has extremely low toughness, and the wedge (notch) effect reduces the toughness of the plated material itself. For this reason, an iron/phosphorus electroplating bath is desired that can produce an iron/phosphorus plating film free of such cracks. Means and Effects for Solving the Problems As a result of conducting studies in order to meet the above-mentioned needs, the present inventors have discovered that the main components are divalent iron ions, phosphorous acid and/or phosphites, and water-soluble When using a toughening bath containing aluminum compounds, the resulting iron/phosphorus plating film is free of cracks and has excellent mechanical properties.For this reason, it is possible to form iron/phosphorus plating films on sliding parts, etc. It was found that it is very effective as a plating bath for That is, conventionally, as mentioned above, a plating bath using hypophosphorous acid or hypophosphite as a phosphorus source has been used, and this type of plating bath can produce a glossy plating film. However, when observing the cross section, it was found that many cracks had occurred. However, it was discovered that when phosphorous acid or phosphite is used as a phosphorus source and an aluminum compound is added, an iron/phosphorus plating film with no cracks can be reliably formed on the cross section, and the present invention has been developed. This is what led to the eggplant. The present invention will be explained in more detail below. The iron/phosphorus electroplating bath according to the present invention has divalent iron ions and phosphorous acid and/or phosphite as main components. Here, the source of divalent iron ions is not particularly limited, but examples include ferrous sulfate, ferrous chloride,
Examples include ferrous sulfamate, ferrous borofluoride, etc., and one of these may be used alone or in combination with two others.
More than one species can be used in combination. Also,
Although the content of divalent iron ions is not necessarily limited, it is preferably 20 to 80 g per plating bath. In the present invention, phosphorous acid and/or phosphite is used as a source of phosphorus for the iron/phosphorus plating film, thereby obtaining an iron/phosphorus plating film without cracks as described above. It is something that can be done. In this case, the content of phosphorous acid or phosphite varies depending on the phosphorus content of the iron/phosphorus plating film required, and also depends on the solubility of the phosphorous acid or phosphite in the plating bath. Although limited, usually NaH 2 PO 3 per plating bath.
The amount of 2H 2 O is preferably 0.01 to 20 g, particularly 0.1 to 10 g. According to the bath of the present invention, by changing the content of phosphorous acid or phosphite, it is usually 0.05
Iron-phosphorus plating coatings with a phosphorus content of ~10% can be obtained. In addition, as phosphite,
Sodium phosphite and the like can be used. In addition to the above-mentioned components, the plating bath according to the present invention further contains aluminum compounds such as aluminum sulfate and aluminum chloride.By containing aluminum ions in the plating bath, the occurrence of cracks can be further suppressed. This can be reliably prevented. The amount of aluminum compound added is preferably as aluminum ions per plating solution.
0.05 to 5 g, especially 0.1 to 2 g can be added. In addition, in the plating bath, if necessary, conductivity salts such as ammonium sulfate and ammonium chloride may be added in an amount of 0 to 200 g, particularly 20 to 150 g, and boric acid, etc. may be added as a PH buffer to 0 to 60 g, particularly 20 to 150 g. 50g/
, 0 to 20 g/, especially 1 to 10 g/of acidic ammonium fluoride etc. as a complexing agent for trivalent iron ions.
Can be added. In addition, the plating bath of the present invention
The pH is preferably 0.5 to 3.5. When plating a desired object using the iron/phosphorous electroplating bath mentioned above, the bath temperature is room temperature to 80°C.
℃, in particular 30 to 70 ℃, and the cathode current density can be 0.5 to 30 A/ dm2 , in particular 2 to 20 A/dm2. Further, although stirring is not necessarily required, bath stirring using a cathode rocker or stirrer may also be employed. Note that an iron plate is generally used for the anode. [Effects of the Invention] The appearance of the iron/phosphorus plating film obtained using the iron/phosphorus electroplating bath of the present invention is generally a semi-glossy, uniform surface, and the resulting matte film has no cracks. However, since it has excellent mechanical properties, it is suitably used for plating sliding members such as piston skirts and other parts. EXAMPLES Hereinafter, the present invention will be specifically explained by showing examples and comparative examples, but the present invention is not limited to the following examples. [Example] FeCl 2・4H 2 O 220g/ NH 4 F・HF 10 〃 Al 2 (SO 4 ) 3・14−18H 2 O 5 〃 H 3 PO 3 1.5 〃 PH 1.2 Next, the above plating bath was Used, bath temperature 60℃, Dk
20 μm iron/phosphorus electroplating was applied to an AC8A/T6 aluminum alloy that had been pretreated by a known method under conditions of 4 A/dm 2 . For comparison, using the plating bath of the comparative example below, AC8A・
20μ iron/phosphorus electroplating applied to T6 aluminum alloy. [Comparative example] FeCl 2・4H 2 O 80g/ FeSO 4・7H 2 O 100 〃 NaH 2 PO 2・H 2 O 10 〃 PH 1.4 The appearance, hardness, and phosphorus content of the obtained iron/phosphorus plating film were It is shown in Table 1. In addition, the plating film was cut and the cut surface was
After etching with nital for 2 seconds, the presence or absence of cracks was examined using a metallurgical microscope (400x magnification).
The results are also listed in Table 1.
【表】
更に、上記めつき浴を用して公知の方法により
前処理した素材（AC8A・T6のアルミニウム合
金）に20μの鉄・リン電気めつき浴を施したもの
を試料として使用し、JIS Ｚ 2274に基いて金属
材料の回転曲げ疲れ試験を行つた。その結果を第
２表に示す。[Table] Furthermore, a material (AC8A/T6 aluminum alloy) pretreated using the above plating bath by a known method was subjected to a 20μ iron/phosphorus electroplating bath, and the JIS A rotating bending fatigue test of metal materials was conducted based on Z 2274. The results are shown in Table 2.
【表】
第２表の結果より、本発明浴から得られた鉄・
リンめつき被膜が良好な機械的特性を有している
ことが認められる。[Table] From the results in Table 2, the iron and
It is observed that the phosphorized coating has good mechanical properties.
Claims (1)
ン酸塩とを主成分とし、かつアルミニウム化合物
を添加してなることを特徴とする鉄・リン電気め
つき浴。 ２ 亜リン酸及び／又は亜リン酸塩の含有量がめ
つき浴１当りNaH2PO3・2H2Oとして0.01〜20
ｇであり、アルミニウム化合物の含有量がアルミ
ニウムイオンとしてめつき液１当り0.05〜５ｇ
である特許請求の範囲第１項記載のめつき浴。[Claims] 1. An iron/phosphorus electroplating bath characterized by containing divalent iron ions, phosphorous acid and/or phosphite as main components, and adding an aluminum compound. . 2. The content of phosphorous acid and/or phosphite is 0.01 to 20 as NaH 2 PO 3 2H 2 O per plating bath.
g, and the aluminum compound content is 0.05 to 5 g per plating solution as aluminum ions.
A plating bath according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11963789A JPH0248635B2 (en) | 1989-05-12 | 1989-05-12 | TETSU * RINDENKIMETSUKYOKU |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11963789A JPH0248635B2 (en) | 1989-05-12 | 1989-05-12 | TETSU * RINDENKIMETSUKYOKU |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP24168183A Division JPS60131994A (en) | 1983-12-21 | 1983-12-21 | Iron-phosphorus electroplating bath |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0270068A JPH0270068A (en) | 1990-03-08 |
| JPH0248635B2 true JPH0248635B2 (en) | 1990-10-25 |
Family
ID=14766381
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11963789A Expired - Lifetime JPH0248635B2 (en) | 1989-05-12 | 1989-05-12 | TETSU * RINDENKIMETSUKYOKU |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0248635B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5089857A (en) * | 1990-10-15 | 1992-02-18 | Eastman Kodak Company | Electrostatographic apparatus having sheet cooling and turnover devices |
| JP3700312B2 (en) * | 1996-04-19 | 2005-09-28 | 住友電気工業株式会社 | Method for producing Fe metal porous body |
| DE10013298C2 (en) | 2000-03-09 | 2003-10-30 | Atotech Deutschland Gmbh | Method for applying a metal layer on light metal surfaces and application of the method |
-
1989
- 1989-05-12 JP JP11963789A patent/JPH0248635B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0270068A (en) | 1990-03-08 |
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