CN102690975B - Ternary tin-zinc alloy and electroplating method thereof - Google Patents
Ternary tin-zinc alloy and electroplating method thereof Download PDFInfo
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- CN102690975B CN102690975B CN201210191702.3A CN201210191702A CN102690975B CN 102690975 B CN102690975 B CN 102690975B CN 201210191702 A CN201210191702 A CN 201210191702A CN 102690975 B CN102690975 B CN 102690975B
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Abstract
The invention relates to a ternary tin-zinc alloy which comprises the following components in percentage by mass: 35-60 percent of tin, 35-60 percent of zinc and 1-10 percent of manganese. The invention also provides an electroplating method of the ternary tin-zinc alloy. The method is carried out under the following conditions of an alloy plating solution temperature of 16-24 DEG C, a plating solution stirring speed of 80-180m/min and a cathode current density of 15-90A/dm<2>. The ternary tin-zinc alloy obtained by electroplating has strong corrosion resistance, can reduce pollution, and is especially suitable for being used as a corrosion preventing layer of an iron material.
Description
Technical field
The present invention relates to have the novel tertiary tin zinc alloy of specific composition composition, it contains a kind of manganese metal as the 3rd alloy compositions.In addition, the invention still further relates to a kind of electro-plating method that is used for generating this type of ternary tin zinc alloy layer, and this alloy layer is as the purposes of preservative coat or ornament layer.
Background technology
Known, iron material can be anticorrosion by coming with zinc coating passivation immediately, and passivation is such as chromic acid passivation is (based on Cr
6+) or chromous acid passivation (based on Cr
3+), its surface becomes yellow, basket look, black or olive-green and can identify.Take this measure, test in (DIN50021-ss) until start to occur that the guard time of red corrosion can reach 200-600 hour at salt spray.
For higher requirement, in salt spray test until reach and within 1000 hours, just approximately start to occur that the erosion resistance of red corrosion can contain nickel, cobalt or iron as also chromic acid passivation immediately of the zinc alloy of alloy compositions by platings.The share of alloying element can be less than 1 % by weight until 15 % by weight, the for example Fe of 0.4-0.6 % by weight in ZnFe system, the for example Ni of 12-15 % by weight (zinc alloy method: the performance in technology and application (Zinklegierungsverfahren:Eigenschaften und Anwendungen inder Technik) in ZnNi system, Dr.A.Jim é nez, B.Kerle and H.Schmidt, electroplating technology 89 (1998) 4).
Tin zinc alloy layer also can be used as the preservative coat of iron.In salt spray test, for the SnZn-coating through chromic acid passivation until start to occur that red corrosion is 1000 hours.The Sn that optimum alloy composition composition is 70 % by weight and the Zn of 30 % by weight.Its shortcoming is only the have an appointment less hardness (tin-zinc-plating, E.Budmann and D.Stevens, Trans IMF 76 (1998) 3) of 50HV of SnZn-coating.
Can recognize as the observation of the development in automotive industry for the corrosion-resistant field at iron material, will propose protective system with the unappeasable requirements at the higher level of known method future.This can be to exceed the erosion resistance of 3000 hours in salt spray test by the requirement of raising to erosion resistance.In addition, such preservative coat should have high as far as possible hardness, is wear-resisting, and also may weld especially.
So task of the present invention is, finds the new alloy system with extra high erosion resistance, and the plating bath for depositing this alloy is provided, it can meet the requirement for preservative activity in the future.
CN1239751C discloses a kind of ternary tin zinc alloy, and its moiety is that the zinc of tin, 30-65 % by weight of 30-65 % by weight and 0.1-15 % by weight are as the metal in a kind of chosen from Fe of the 3rd alloy compositions, brill, nickel group.The electrolytic deposition that corresponding alloy layer can be bathed by moisture plating bath generates, and this plating bath is bathed the alloy compositions containing with lysed form.Alloy layer shows extra high erosion resistance, is therefore particularly suitable as the preservative coat of iron material.
Summary of the invention
One of object of the present invention is to provide a kind of ternary tin zinc alloy, and the alloy layer erosion resistance of described alloy is strong, can be used as the preservative coat of iron material, and can reduce pollution.
In order to achieve the above object, the present invention has adopted following technical scheme:
Described ternary tin zinc alloy, it comprises by mass percentage:
Tin 35 ~ 60%
Zinc 35 ~ 60%
Manganese 1 ~ 10%.
As optimal technical scheme, described ternary tin zinc alloy, comprises by mass percentage:
Tin 40 ~ 60%
Zinc 40 ~ 60%
Manganese 2 ~ 8%.
As optimal technical scheme, described ternary tin zinc alloy, comprises by mass percentage:
Tin 45 ~ 60%
Zinc 45 ~ 60%
Manganese 3 ~ 8%.
As optimal technical scheme, described ternary tin zinc alloy, it comprises by mass percentage:
Tin 50 ~ 60%
Zinc 50 ~ 60%
Nickel 3 ~ 6%.
In described ternary tin zinc alloy, the mass percent that tin accounts for alloy is 35 ~ 60%, for example 36%, 37%, 38%, 39%, 40%, 41%, 42%, 43%, 44%, 45%, 46%, 47%, 48%, 49%, 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, preferably 40 ~ 60%, further preferably 45 ~ 60%, more preferably 50 ~ 60%.
In described ternary tin zinc alloy, the mass percent that zinc accounts for alloy is 35 ~ 60%, for example 36%, 37%, 38%, 39%, 40%, 41%, 42%, 43%, 44%, 45%, 46%, 47%, 48%, 49%, 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, preferably 40 ~ 60%, further preferably 45 ~ 60%, more preferably 50 ~ 60%.
In described ternary tin zinc alloy, the mass percent that manganese accounts for alloy is 1 ~ 10%, for example 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9%, 9.5%, preferably 2 ~ 8%, further preferably 3 ~ 8%, more preferably 3 ~ 6%.
" comprising " of the present invention, mean it except described component, can also comprise other components, these other components give described alloy different characteristics.In addition, " comprising " of the present invention, can also replace with enclosed " being " or " by ... composition ".No matter which kind of composition alloy of the present invention comprises, the mass percent sum of described alloy is 100%.
Ternary tin zinc alloy of the present invention, can only be made up of tin, zinc and manganese, and meanwhile, alloy of the present invention also can contain other composition.
For example, alloy of the present invention can also include Fe, the mass percent that described Fe accounts for alloy is 0.1 ~ 15%, for example 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 1.2%, 1.5%, 1.8%, 2.1%, 2.4%, 2.7%, 3.0%, 3.3%, 3.6%, 3.9%, 4.5%, 5.0%, 5.5%, 6.0%, 6.5%, 7.0%, 7.5%, 8.0%, 8.5%, 9.0%, 9.5%, 9.8%, 9.9%.
For example, alloy of the present invention can also include Co, the mass percent that described Co accounts for alloy is 0.1 ~ 15%, for example 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 1.2%, 1.5%, 1.8%, 2.1%, 2.4%, 2.7%, 3.0%, 3.3%, 3.6%, 3.9%, 4.5%, 5.0%, 5.5%, 6.0%, 6.5%, 7.0%, 7.5%, 8.0%, 8.5%, 9.0%, 9.5%, 9.8%, 9.9%.
For example, alloy of the present invention can also include Ni, the mass percent that described Ni accounts for alloy is 0.1 ~ 15%, for example 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 1.2%, 1.5%, 1.8%, 2.1%, 2.4%, 2.7%, 3.0%, 3.3%, 3.6%, 3.9%, 4.5%, 5.0%, 5.5%, 6.0%, 6.5%, 7.0%, 7.5%, 8.0%, 8.5%, 9.0%, 9.5%, 9.8%, 9.9%.
The example of described alloy has: tin, zinc, manganese and Fe; Tin, zinc, manganese and Co; Tin, zinc, manganese and and Ni; Tin, zinc, manganese, Fe and Co; Tin, zinc, manganese, Fe and Ni; Tin, zinc, manganese, Co and Ni; Tin, zinc, manganese, Fe, Co and Ni.It is as follows that the each component of described alloy accounts for the mass percent of alloy:
The mass percent that tin accounts for alloy is 35 ~ 60%, for example 36%, 37%, 38%, 39%, 40%, 41%, 42%, 43%, 44%, 45%, 46%, 47%, 48%, 49%, 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, preferably 40 ~ 60%, further preferably 45 ~ 60%, more preferably 50 ~ 60%.
The mass percent that zinc accounts for alloy is 35 ~ 60%, for example 36%, 37%, 38%, 39%, 40%, 41%, 42%, 43%, 44%, 45%, 46%, 47%, 48%, 49%, 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, preferably 40 ~ 60%, further preferably 45 ~ 60%, more preferably 50 ~ 60%.
The mass percent that manganese accounts for alloy is 1 ~ 10%, for example 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9%, 9.5%, preferably 2 ~ 8%, further preferably 3 ~ 8%, more preferably 3 ~ 6%.
The mass percent that Co accounts for alloy is 0.1 ~ 15%, for example 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 1.2%, 1.5%, 1.8%, 2.1%, 2.4%, 2.7%, 3.0%, 3.3%, 3.6%, 3.9%, 4.5%, 5.0%, 5.5%, 6.0%, 6.5%, 7.0%, 7.5%, 8.0%, 8.5%, 9.0%, 9.5%, 9.8%, 9.9%.
The mass percent that Ni accounts for alloy is 0.1 ~ 15%, for example 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 1.2%, 1.5%, 1.8%, 2.1%, 2.4%, 2.7%, 3.0%, 3.3%, 3.6%, 3.9%, 4.5%, 5.0%, 5.5%, 6.0%, 6.5%, 7.0%, 7.5%, 8.0%, 8.5%, 9.0%, 9.5%, 9.8%, 9.9%.
The mass percent that Fe accounts for alloy is 0.1 ~ 15%, for example 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 1.2%, 1.5%, 1.8%, 2.1%, 2.4%, 2.7%, 3.0%, 3.3%, 3.6%, 3.9%, 4.5%, 5.0%, 5.5%, 6.0%, 6.5%, 7.0%, 7.5%, 8.0%, 8.5%, 9.0%, 9.5%, 9.8%, 9.9%.
No matter which kind of composition alloy of the present invention comprises, the mass percent sum of described alloy is 100%.
Ternary tin zinc alloy of the present invention can be prepared by single component by melt-metallurgic method or powder metallurgic method.
In view of typical application, the preferably mode to electroplate of its preparation, by the mode of the electrolytic deposition from moisture plating bath is bathed, contains the alloy compositions of the form through dissolving in electrolysis bath of liquid especially.
Two of object of the present invention is to provide ternary tin zinc alloy electroplating method as above, described method is by selecting bath temperature and cathode current density etc., and use alloy electroplating bath as described below, thereby obtain a kind of alloy electroplating method, the tin-zinc alloy coating erosion resistance that described method obtains after electroplating is strong, hardness is large, can reduce pollution, is the desirable coating for cadmium.
The electro-plating method of described ternary tin zinc alloy carries out under following condition:
Alloy electroplating bath temperature: 16～24 DEG C,
The stirring velocity of plating solution: 80 ~ 180m/min, and
Cathode current density: 15～90A/dm
2.
Preferably, described method is carried out in following condition:
Alloy electroplating bath temperature: 16～24 DEG C,
The stirring velocity of plating solution: 90 ~ 170m/min, and
Cathode current density: 25～82A/dm
2.
Described alloy electroplating bath temperature: 16～24 DEG C, for example 16.5 DEG C, 17 DEG C, 17.5 DEG C, 18 DEG C, 18.5 DEG C, 19 DEG C, 19.5 DEG C, 20 DEG C, 20.5 DEG C, 21 DEG C, 21.5 DEG C, 22 DEG C, 22.5 DEG C, 23 DEG C, 23.5 DEG C, 24 DEG C, 24.5 DEG C.
The stirring velocity of plating solution: 80 ~ 180m/min, for example 85m/min, 90m/min, 95m/min, 100m/min, 105m/min, 110m/min, 115m/min, 120m/min, 125m/min, 130m/min, 135m/min, 140m/min, 145m/min, 150m/min, 155m/min, 160m/min, 165m/min, 170m/min, 180m/min, preferably 90 ~ 170m/min.
The stirring of plating solution specifically can be suitable for the electroplanting device, the electroplanting device of steel plate etc. that are carried out the jet flow of liquid circulation by pump.Electroplanting device is as long as the device of the material of heat-resisting, chemical proofing, arbitrarily all can, can use the metal such as stainless steel, titanium; Vinylchlorid, teflon (registered trademark), ABS resin etc.In addition can obtain the plated body entirety device of plating solution stirring velocity uniformly in order to improve the homogeneity of coating film thickness and alloy plating composition, to be preferably.
Described alloy electroplating bath contains citric acid or/and Citrate trianion, and optimization citric acid is or/and citric acid organic ammonium salt, and further optimization citric acid is or/and dibasic ammonium citrate.
As the concrete example of Citrate trianion, for example, there is an alkali metal salt (sodium, potassium, lithium salts), alkali earth metal salt (magnesium, calcium, barium salt etc.), stannous salt, zinc salt, ammonium salt and the organic amine salt (MMA, dimethylamine, Trimethylamine 99, ethamine, Isopropylamine, quadrol, Diethylenetriamine etc.) of citric acid.Citric acid and salt thereof can be used alone, but also also mix together.
In described alloy electroplating bath, the concentration of citrate ion is 105 ~ 155g/L, for example 110g/L, 115g/L, 120g/L, 125g/L, 130g/L, 135g/L, 140g/L, 145g/L, 150g/L, 154g/L, 153g/L, 152g/L, 151g/L, preferably 112 ~ 152g/L, further preferred 121 ~ 148g/L.
Described alloy electroplating bath contains amphoterics, the concentration of described amphoterics is 0.006 ~ 18g/L, for example 0.01g/L, 0.02g/L, 0.05g/L, 0.10g/L, 0.20g/L, 17g/L, 16g/L, preferably 0.02 ~ 14g/L, further preferred 1 ~ 8g/L.
Described alloy electroplating bath also contains additive, and described additive comprises formaldehyde and/or ammonium compounds, preferably formaldehyde and/or quaternary ammonium compound, further particular methanol and/or alkalization four isopropyl ammoniums.As quaternary ammonium compound, for example, can also enumerate the reaction product of tertiary amine compound and haloalkane.As concrete tertiary amine compound, for example, can enumerate imidazoles, 1-Methylimidazole, 1-ethyl imidazol(e), glyoxal ethyline, 1-Ethyl-2-Methyl imidazoles, 1-hydroxy methylimidazole, 1-vinyl imidazole and 1,5-methylimidazole as glyoxaline compound; As fatty amine, can enumerate monoethanolamine, diethanolamine, trolamine, dimethylamine, quadrol, Diethylenetriamine, the two propylamine of imino-, three second tetramines, tetraethylene-pentamine, N, N-pair-(3-aminopropyl) quadrol etc.It has stronger reductive action, stops consumingly the oxidation of tin, is conducive to the absorption of organism on electrode surface simultaneously, further improves stannous deposition potential, improves cathodic polarization, and coating is had to obvious refinement and light effect.
Ternary tin zinc alloy according to the present invention has very superior material property, and based on this, they not only can be used as independently material, and can be used on base material with the form of coating by different modes especially.
Ternary tin zinc alloy of the present invention has extra high erosion resistance, so this alloy is particularly suitable as the preservative coat of iron material.After the passivation of passing through chromic acid passivation or chromous acid passivation of commonly using in combination through the iron plate of this ternary alloy coating like this, do not reach the erosion resistance of the red corrosion appearance of inhibition that exceedes 3500 hours not difficultly.
Except these produce the use field of functional impact, also can be used as decorative skin according to ternary tin zinc alloy of the present invention.So, there is interesting and the noticeable color in blue wave band according to three of selected the 3rd alloying element kinds of alloy systems.
Embodiment
For the present invention is described better, be convenient to understand technical scheme of the present invention, typical but non-limiting embodiment of the present invention is as follows:
Described in embodiment 1-4 and comparative example 1-2, ternary tin zinc alloy composition is as shown in table 1.
Alloy composition described in table 1 embodiment 1-4 and comparative example 1-2
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 | Comparative example 2 | |
| Tin % | 35 | 60 | 45 | 50 | 45 | 45 |
| Zinc % | 60 | 35 | 45 | 49 | 50 | 52 |
| Manganese % | 5 | 5 | 10 | 1 | 5 | |
| Cobalt % | 3 |
Wherein, comparative example 2 is CN1239751C the disclosed embodiments 1 ternary tin zinc alloy compositions.
Embodiment 1
After iron plate is carried out to pre-treatment, using following plating solution, is that 16 DEG C, the stirring velocity of plating solution are that 80m/min, cathode current density are 15/dm at bath temperature
2condition under implement electroplating processes.
Citric acid 105g/L
Alkyl dimethyl sulfoethyl trimethyl-glycine 0.006g/L
Trolamine 0.002g/L
Embodiment 2
After iron plate is carried out to pre-treatment, using following plating solution, is that 24 DEG C, the stirring velocity of plating solution are that 180m/min, cathode current density are 90/dm at bath temperature
2condition under implement electroplating processes.
Citric acid 155g/L
Octadecyl dihydroxy ethyl amine oxide 18g/L
Trolamine 0.2g/L
Embodiment 3
After iron plate is carried out to pre-treatment, using following plating solution, is that 20 DEG C, the stirring velocity of plating solution are that 100m/min, cathode current density are 45/dm at bath temperature
2condition under implement electroplating processes.
Citric acid 125g/L
Octadecyl dihydroxy ethyl amine oxide 10g/L
Formaldehyde and diethanolamine 2g/L
Embodiment 4
After iron plate is carried out to pre-treatment, using following plating solution, is that 22 DEG C, the stirring velocity of plating solution are that 110m/min, cathode current density are 40/dm at bath temperature
2condition under implement electroplating processes.
Citric acid 135g/L
Octadecyl dihydroxy ethyl amine oxide 8g/L
Formaldehyde and diethanolamine 3g/L
Comparative example 1
The applicant's earlier application but undocumented CN201210139655.8 discloses a kind of electro-plating method of tin-zinc alloy, described comparative example 1 adopts the disclosed electro-plating method of earlier application, and described method is as follows:
After iron plate is carried out to pre-treatment, using following plating solution, is that 25 DEG C, the stirring velocity of plating solution are that 50m/min, cathode current density are 5A/dm at bath temperature
2condition under implement electroplating processes.
Comparative example 2
Comparative example 2 is CN1239751C the disclosed embodiments 1 ternary tin zinc alloy compositions, adopts electro-plating method of the present invention to electroplate it, and described method is as follows:
After iron plate is carried out to pre-treatment, using following plating solution, is that 22 DEG C, the stirring velocity of plating solution are that 110m/min, cathode current density are 40/dm at bath temperature
2condition under implement electroplating processes.
Citric acid 135g/L
Octadecyl dihydroxy ethyl amine oxide 8g/L
Formaldehyde and diethanolamine 3g/L
The iron plate chromic acid passivation that above-described embodiment 1-4 and comparative example 1-2 are coated with to ternary tin zinc alloy layer is (based on Cr6
+), described iron plate shows following erosion resistance in testing according to the spraying of DIN50021-SS:
The iron plate that is coated with ternary tin zinc alloy layer described in embodiment 1-4 starts to occur white corrosion within the period of 2000-3000 hour, until red corrosion does not still appear in 3500h.
Comparative example 1-2 all starts to occur white corrosion within the period of 1800-3000 hour, and until within 3000 hours, does not occur red corrosion.
As can be seen here, the corrosion resistance of tin-zinc alloy of the present invention is stronger.
Alloy layer described in embodiment 1-4 and comparative example 1-2 is carried out to hardness test, and result is as follows:
Described in embodiment 1-4, the hardness of coating is all more than 1400HV, and the hardness of coating is significantly less than alloy layer described in embodiment of the present invention 1-4 described in comparative example 1-2.
Should be noted that and understand, in the situation that not departing from the desired the spirit and scope of the present invention of accompanying claim, can make various amendments and improvement to the present invention of foregoing detailed description.Therefore, the scope of claimed technical scheme is not subject to the restriction of given any specific exemplary teachings.
Applicant's statement, the present invention illustrates method detailed of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned method detailed, does not mean that the present invention must rely on above-mentioned method detailed and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, and the selections of the equivalence replacement to the each raw material of product of the present invention and the interpolation of ancillary component, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
Claims (9)
1. an electro-plating method for ternary tin zinc alloy, is characterized in that, described ternary tin zinc alloy is made up of following component by mass percentage:
Tin 45%
Zinc 45%
Manganese 10%;
Described each constituent mass per-cent sum is 100%;
Described method is carried out under following condition:
Alloy electroplating bath temperature: 16～24 DEG C,
The stirring velocity of plating solution: 80～95m/min, and
Cathode current density: 15～90A/dm
2;
Described alloy electroplating bath contains citric acid or/and Citrate trianion, and in described alloy electroplating bath, the concentration of citrate ion is 105～155g/L; Alloy electroplating bath contains amphoterics; The concentration of described amphoterics is 0.20～18g/L; Alloy electroplating bath also contains additive, and described additive comprises formaldehyde and/or ammonium compounds.
2. the method for claim 1, is characterized in that, described method is carried out in following condition:
Alloy electroplating bath temperature: 16～24 DEG C,
The stirring velocity of plating solution: 90～95m/min, and
Cathode current density: 25～82A/dm
2.
3. the method for claim 1, is characterized in that, described alloy electroplating bath contains citric acid or/and citric acid organic ammonium salt.
4. method as claimed in claim 3, is characterized in that, described alloy electroplating bath contains citric acid or/and dibasic ammonium citrate.
5. the method for claim 1, is characterized in that, in described alloy electroplating bath, the concentration of citrate ion is 112～152g/L.
6. method as claimed in claim 5, is characterized in that, in described alloy electroplating bath, the concentration of citrate ion is 121～148g/L.
7. the method for claim 1, is characterized in that, the concentration of described amphoterics is 0.20～14g/L.
8. method as claimed in claim 7, is characterized in that, the concentration of described amphoterics is 1～8g/L.
9. the method for claim 1, is characterized in that, described additive is selected from formaldehyde and/or quaternary ammonium compound.
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| CN101096730A (en) * | 2006-06-26 | 2008-01-02 | 日立电线株式会社 | Pb-free sn-based material, wiring conductor, terminal connecting assembly, and pb-free solder alloy |
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| CN101096730A (en) * | 2006-06-26 | 2008-01-02 | 日立电线株式会社 | Pb-free sn-based material, wiring conductor, terminal connecting assembly, and pb-free solder alloy |
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