CN101311322A - Surface treatment process for electroplating iron-nickel alloy and electroplating solution thereof - Google Patents
Surface treatment process for electroplating iron-nickel alloy and electroplating solution thereof Download PDFInfo
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- CN101311322A CN101311322A CNA2008100305837A CN200810030583A CN101311322A CN 101311322 A CN101311322 A CN 101311322A CN A2008100305837 A CNA2008100305837 A CN A2008100305837A CN 200810030583 A CN200810030583 A CN 200810030583A CN 101311322 A CN101311322 A CN 101311322A
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Abstract
The invention discloses a superficial treatment process of an electroplating iron-nickel alloy and the electroplating solution thereof. The electroplating solution is prepared by aqueous solution and the elements include: ferrous sulfate, 100 to 150 grams per liter; nickel sulfate, 120 to 200 grams per liter; boric acid, 30 to 60 grams per liter; saccharin, 0.5 to 3 grams per liter; and sodium benzene sulfinate, 0.1 to 0.4 grams per liter. A work piece is taken as a cathode in the electroplating process. The anode is a Ti-oxide inert anode. A high-frequency switch power supply is adopted. An iron-nickel film coating can be got by electroplating with the current density of 5-10A/dm<2>. After treatment by the invention, the work piece surface is plated with an iron-nickel alloy coating which contains 40 percent to 60 percent of iron. The coating structure is a structure which is amorphous but includes nano-crystalline. The surface of the coating structure is flat and uniform and has fine crystallization. The alloy plating is characterized by good anti-corrosion performance, good ductility and high hardness, etc. Compared with the nickel plating technique, the coating got by the invention is more superior in cost performance, has the same service performance and at the same time greatly reduces the production cost and has very good economical benefits.
Description
Technical field
The invention belongs to technical field of surface, relate to a kind of novel electroplating iron-nickel alloy process for treating surface to substitute nickel plating technology technology and employed electroplate liquid thereof.
Background technology
Nickel plating technology is widely used in all respects of electroplating industry, be used for to metal device carry out anticorrosion, decorate and to be the surface treatment of purpose.
But because nickel resources belongs to Nonrenewable resources,, supply with wretched insufficiency, cause substantial appreciation of prices along with the continuous increase of nickel consumption.Each electroplating enterprise nickel plating cost is high.Electroplating enterprise seeks to save nickel one after another, for the novel process of nickel.From the character of coating, iron-nickel alloy should be first-selected plating.
In the 60 to 70's, China electroplates industry and once carried out on a large scale for nickel, the motion of joint nickel.Mainly be the tin ore resource of utilizing China's abundant at that time, having carried out with cyaniding low tin bronze, the high zinc-copper of cyaniding is also using on producing rapidly for the nickel technical study of bottom.The cupric cyanide tin alloy plating solution of China was once becoming maximum, the most widely used country of quantity in the world.Most popular at that time process combination is:
Gunmetal → polishing → directly chromium plating
Full bright copper tin alloy → directly chromium plating
Gunmetal → polishing → plating approaches nickel → chromium plating
High zinc-copper alloy → polishing → flash brass → chromium plating
In today of the high enterprise of nonferrous metal price,,, make great efforts to research and develop and promote for nickel, joint nickel novel process in conjunction with the new demand of environmental protection, cost and efficient according to the invaluable experience of electroplating the older generation.At present, comparative maturity has for nickel, joint nickel electroplating technology: Rhometal technology, no cyanogen tin nickel are for nickel technology, nickel-free electroplating technology.
Wherein Rhometal once obtained the industrial application of certain scale in the U.S. as far back as the seventies.China is also rather popular in the 1970s and 1980s, is mainly used in the plating processing of art metal furniture, irony torch light.Be characterized in: the coating iron-holder is between 15%-20%, and joint nickel effect is limited; Use soluble anode to make anode, solution component is wayward, and along with the plating bath increase of duration of service, iron-holder is fewer and feweri in the coating, is lower than 10%; In addition, if handle badly, coating gets rusty easily.
Summary of the invention
The object of the present invention is to provide a kind of with low cost, excellent property for nickel plating technology, be surface treatment process for electroplating iron-nickel alloy and employed electroplate liquid, can save the use of nickel widely, improve the content of iron, the content that overcomes iron in the electroplating technology technology in the past is low, can't improve and make the stable deficiency of coating performance.
For achieving the above object, the present invention proposes a kind of novel electroplating iron-nickel alloy process for treating surface to substitute nickel plating technology.
Described electroplate liquid adopts aqueous solution preparation, composition comprises ferrous sulfate 100-150 grams per liter, single nickel salt 120-200 grams per liter, boric acid 30-60 grams per liter, asccharin 0.5-3 grams per liter, benzene sulfinic acid sodium salt 0.1-0.4 grams per liter, workpiece is as negative electrode in the electroplating process, adopt high frequency switch power, with 5-10A/dm
2Current density electroplate and obtain iron nickel plated film, adopt Ti-oxide compound inert anode.
The iron-nickel alloy of gained, iron level are 40-60%, and surplus is a nickel.
Automatic supplementing device is taked in adding of main salt of the present invention, and meter is added automatically on time, reduces personal errors.
Ti-oxide compound inert anode is by Ti matrix and lining iridium and the oxide compound inert anode formed of the oxide electrochemical active coating of tantalum on it.
Being prepared as of the oxide compound inert anode of Ti-iridium and tantalum: the alcoholic solution of preparation chloro-iridic acid, tantalum chloride, it is coated in the surface of pure metallic titanium, through promptly obtaining behind the high bake (80-500 ℃) by Ti matrix and lining iridium and the oxide compound inert anode formed of the oxide electrochemical active coating of tantalum on it.
The electroplate liquid that technology of the present invention is used, for described electroplate liquid adopts aqueous solution preparation, composition comprises ferrous sulfate 100-150 grams per liter, single nickel salt 120-200 grams per liter, boric acid 30-60 grams per liter, asccharin 0.5-3 grams per liter, benzene sulfinic acid sodium salt 0.1-0.4 grams per liter.
Technology of the present invention has following characteristics:
1) adopts aqueous solution preparation treatment soln
2) main salt adopts ferrous sulfate and single nickel salt preparation, not chloride ion-containing
3) formula range ferrous sulfate 100-150 grams per liter single nickel salt 120-200 grams per liter
The electroplating technology of described electroplating iron-nickel alloy is:
Anode adopts Ti-oxide compound inert anode, and automatic supplementing device is taked in adding of main salt, and meter is added automatically on time, reduces personal errors.Workpiece adopts high frequency switch power, with 5-10A/dm as negative electrode
2Current density electroplate and obtain iron nickel plated film
The characteristics of this technology are: chloride ion-containing not in the plating bath can not produce deleterious chlorine in the electroplating process; Anode has adopted Ti-oxide compound inert anode, adds and adopts automatic supplementing device, and solution component is stable, and coating compactness is good, and corrosion resisting property is stronger. coating iron-holder height, can effectively save nickel resources.
The advantage of the iron-nickel alloy coating that the present invention obtains:
1) iron-holder height, coating iron-holder scope can require to carry out the adjustment of component according to reality between 40%-60%.The iron-holder height, joint nickel effect is remarkable.
2) the coating microstructure is that amorphous is mingled with nanocrystalline structure.Corrosion resistance nature is good, and independent coating can anti-8 hours neutral salt spray.
3) as prime coat, with other coating compound after, to the protective value of body material fine (seeing the following form 1).
The coating microstructure is that amorphous is mingled with nanostructure
| The coating combination | Respective thickness (micron) | The CASS test-results |
| Iron nickel dam of the present invention/ |
20/0.3 | 15h |
| Iron nickel dam of the present invention/sour copper layer/iron nickel dam of the present invention/chromium layer | 5/10/10/0.3 | 24h |
| Iron nickel dam of the present invention/sour copper/iron nickel dam of the present invention/iron nickel dam of the present invention/chromium layer | 5/10/10/10/0.3 | 36h |
4) as prime coat, and the bonding force between other metals is good, sees Fig. 1.
Fig. 1 is the cross-section morphology of the FeNi/Cu sample on the steel substrate, does not have the gap between layer and the layer, and description taken in conjunction power is good.
5) flexility is good, and 20 microns plated film does not rupture through doubling repeatedly
6) hardness of coating is higher, Vickers' hardness 450-550Hv.
Iron-nickel alloy coating of the present invention can be used as prime coat, unites use with chromium layer, copper layer, tungstenalloy coating.As: iron nickel/copper/iron nickel/chromium composite plating, half bright iron nickel/three layers of plating of bright iron nickel/chromium, iron nickel/tungstenalloy coating etc.
Structure by the resulting iron-nickel alloy of surface treatment process for electroplating iron-nickel alloy of the present invention is that amorphous is mingled with nanocrystalline coating.Having an even surface of this coating, evenly, crystallization is careful, and granularity is tiny, belongs to nanocrystalline scope on the size and (sees Fig. 4: SEM).From XRD figure (Fig. 5: XRD) as can be known, contain amorphous component, so that structure is that amorphous is mingled with is nanocrystalline.Fig. 6 is respectively the Ni element, the Fe element distributes.Can see among the figure that there are not the poly-partially phenomenon of composition in Ni and Fe element at the coated surface uniform distribution.The iron nickel nano-alloy plating layer that obtains does not have simple metallic nickel and iron to exist, but exists with iron-nickel alloy sosoloid.
By iron-nickel alloy coating iron content 40%-60% of the present invention, be used with other plating, and have good solidity to corrosion and mechanical property, can be used as the application that prime coat replaces nickel plating technology to obtain becoming reconciled.
The plated film that the technology of the present invention obtains is compared with nickel plating technology has more superior cost performance, has equal use properties and greatly reduces production cost simultaneously, has excellent economic.
The present invention is further illustrated below in conjunction with the drawings and specific embodiments.
Description of drawings
Fig. 1 is the cross-section morphology of the FeNi/Cu sample on the steel substrate, does not have the gap between layer and the layer, and bonding force is good.
Fig. 2 plates parts drawing behind the lockset for the present invention.
Fig. 3 plates parts drawing behind the pincer pliers for the present invention
The sem photograph of Fig. 4 coating.The surface particles degree is very tiny, even does not see tangible crystal boundary, and coating crystallization crystal grain is tiny, belongs to nanocrystalline scope on the size.
Fig. 5 coating x-ray diffraction pattern.XRD, the peak of broad has illustrated that amorphous is mingled with
The distribution diagram of element of Fig. 6 coating.B figure is that Ni unit vegetarian noodles distributes, and C figure is that Fe unit vegetarian noodles distributes.Can see among the figure that there are not the poly-partially phenomenon of composition in Ni and Fe element at the film surface uniform distribution.Specifically
Embodiment
Following examples are intended to illustrate the present invention rather than limitation of the invention further.
Embodiment 1:
Lockset is electroplated, the brass substrate
Operational path: oil removing-cleaning-pickling-clean-electroplate iron-nickel alloy coating-cleaning of the present invention-cleaning-chromium plating.
In the above-mentioned route, oil removing is the alkali electroless oil removing; Pickling is a dilute sulphuric acid, and corresponding processing condition all can be handled by existing processes.
When electroplating iron-nickel alloy coating of the present invention, described electroplate liquid adopts aqueous solution preparation, composition comprises ferrous sulfate 100 grams per liters, single nickel salt 120 grams per liters, boric acid 30 grams per liters, asccharin 0.5 grams per liter, benzene sulfinic acid sodium salt 0.1 grams per liter, workpiece is as negative electrode in the electroplating process, adopt high frequency switch power, with 5-10A/dm
2Current density electroplate and obtain iron nickel plated film, adopt the oxide compound inert anode of Ti-iridium and tantalum.
Fig. 2 is the lockset part photo neutral salt spray test 120 hours rust not after above-mentioned art breading.Satisfy production requirement.
Embodiment 2:
Hardware ﹠ tools is electroplated, No. 45 steel matrix
Operational path: oil removing-cleaning-pickling-clean-electroplate iron-nickel alloy coating of the present invention-cleaning-chromium plating.
The chemical oil removing of alkalescence point is taked in oil removing in the above-mentioned technology; Pickling is that dilute sulphuric acid cleans, and corresponding processing condition all can be handled by existing processes.
Described electroplate liquid adopts aqueous solution preparation, composition comprises ferrous sulfate 150 grams per liters, single nickel salt 200 grams per liters, boric acid 60 grams per liters, asccharin 3 grams per liters, benzene sulfinic acid sodium salt 0.4 grams per liter, workpiece adopts high frequency switch power, with 5-10A/dm as negative electrode in the electroplating process
2Current density electroplate and obtain iron nickel plated film, adopt the oxide compound inert anode of Ti-iridium and tantalum.
Fig. 3 is the pincer pliers photo after above-mentioned art breading.
Embodiment 3: self-rescuer, No. 20 steel matrix
Operational path: oil removing-cleaning-pickling-clean-electroplate iron-nickel alloy coating-cleaning of the present invention-plating tungstenalloy.
The chemical oil removing of alkalescence point is taked in oil removing in the above-mentioned technology; Pickling is that dilute sulphuric acid cleans, and corresponding processing condition all can be handled by existing processes.
Described electroplate liquid adopts aqueous solution preparation, composition comprises ferrous sulfate 120 grams per liters, single nickel salt 150 grams per liters, boric acid 40 grams per liters, asccharin 2 grams per liters, benzene sulfinic acid sodium salt 0.3 grams per liter, workpiece adopts high frequency switch power, with 5-10A/dm as negative electrode in the electroplating process
2Current density electroplate and obtain iron nickel plated film, adopt the oxide compound inert anode of Ti-iridium and tantalum.
Embodiment 4: aluminium wheel hub, alloy matrix aluminum
Operational path: oil removing-cleaning-pickling-clean-electroplate iron-nickel alloy coating-copper facing of the present invention-electroplate iron-nickel alloy coating of the present invention-cleaning-chromium plating.
In the above-mentioned route, oil removing is the alkali electroless oil removing; Pickling is the mixed acid solution of nitric acid, phosphoric acid, hydrofluoric acid, and corresponding processing condition all can be handled by existing processes.
When electroplating iron-nickel alloy coating of the present invention, described electroplate liquid adopts aqueous solution preparation, composition comprises ferrous sulfate 110 grams per liters, single nickel salt 140 grams per liters, boric acid 50 grams per liters, asccharin 0.5 grams per liter, benzene sulfinic acid sodium salt 0.1 grams per liter, workpiece is as negative electrode in the electroplating process, adopt high frequency switch power, with 5-10A/dm
2Current density electroplate and obtain iron nickel plated film, adopt the oxide compound inert anode of Ti-iridium and tantalum.
Claims (5)
1, a kind of surface treatment process for electroplating iron-nickel alloy, it is characterized in that, described electroplate liquid adopts aqueous solution preparation, and composition comprises ferrous sulfate 100-150 grams per liter, single nickel salt 120-200 grams per liter, boric acid 30-60 grams per liter, asccharin 0.5-3 grams per liter, benzene sulfinic acid sodium salt 0.1-0.4 grams per liter.Workpiece is as negative electrode in the electroplating process, and anode adopts Ti-oxide compound inert anode, adopts high frequency switch power, with 5-10A/dm
2Current density electroplate and obtain iron nickel plated film.
2, a kind of surface treatment process for electroplating iron-nickel alloy according to claim 1 is characterized in that, the iron-nickel alloy of gained, iron level are 40-60%, and surplus is a nickel.
3, a kind of surface treatment process for electroplating iron-nickel alloy according to claim 1 is characterized in that, Ti-oxide compound inert anode is by Ti matrix and lining iridium and the oxide compound inert anode formed of the oxide electrochemical active coating of tantalum on it.
4, a kind of surface treatment process for electroplating iron-nickel alloy according to claim 3, it is characterized in that, being prepared as of the oxide compound inert anode of Ti-iridium and tantalum: the alcoholic solution of preparation chloro-iridic acid, tantalum chloride, it is coated in the surface of pure metallic titanium, through promptly obtaining behind the high bake by Ti matrix and lining iridium and the oxide compound inert anode formed of the oxide electrochemical active coating of tantalum on it.
5, the electroplate liquid of the used not chloride ion-containing of a kind of surface treatment process for electroplating iron-nickel alloy, it is characterized in that, described electroplate liquid adopts aqueous solution preparation, and composition comprises ferrous sulfate 100-150 grams per liter, single nickel salt 120-200 grams per liter, boric acid 30-60 grams per liter, asccharin 0.5-3 grams per liter, benzene sulfinic acid sodium salt 0.1-0.4 grams per liter.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105908223A (en) * | 2016-06-14 | 2016-08-31 | 浙江工业大学义乌科学技术研究院有限公司 | Alkaline electrolyte and method for preparing bright nickel by means of electrolysis in alkaline electrolyte |
| CN105951133A (en) * | 2016-06-14 | 2016-09-21 | 浙江工业大学义乌科学技术研究院有限公司 | Alkaline electrolyte and nickel electroplating method in alkaline system |
| CN106086963A (en) * | 2016-06-13 | 2016-11-09 | 西安交通大学 | A kind of double flute electrolytic preparation is nanocrystalline/method of amorphous metal plural layers plasticising |
| CN106498451A (en) * | 2016-10-31 | 2017-03-15 | 华北理工大学 | A kind of iron-nickel alloy low-carbon (LC) steel composite material and preparation method thereof |
| CN106862580A (en) * | 2017-03-06 | 2017-06-20 | 河北工业大学 | A kind of boron nitride coats the preparation method of Fe-Ni nano-alloy |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4231847A (en) * | 1978-06-21 | 1980-11-04 | Trw Inc. | Electrodeposition of nickel-iron alloys having a low temperature coefficient and articles made therefrom |
| CN1051060A (en) * | 1990-11-10 | 1991-05-01 | 机械电子工业部武汉材料保护研究所 | Electric depositing solution of antiwear non-crystal alloy of iron, nickel, phosphorus and technology thereof |
| CN1313647C (en) * | 2003-09-04 | 2007-05-02 | 长沙高新技术产业开发区英才科技有限公司 | Electroplating liquid and technology used in electrodeposition of trngsten series noncrystalline alloy cladding material or nanometer alloy cladding material |
| CN100383288C (en) * | 2004-01-15 | 2008-04-23 | 中南大学 | Method for preparing Fe-Ni, Fi-Ni-Cr alloy foil |
| CN101042044B (en) * | 2007-01-16 | 2011-01-05 | 湖南纳菲尔新材料科技股份有限公司 | Pumping rod or oil sucking pipe electroplating iron-nickel/tungsten alloy double-layer coating and surface processing technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106086963A (en) * | 2016-06-13 | 2016-11-09 | 西安交通大学 | A kind of double flute electrolytic preparation is nanocrystalline/method of amorphous metal plural layers plasticising |
| CN105908223A (en) * | 2016-06-14 | 2016-08-31 | 浙江工业大学义乌科学技术研究院有限公司 | Alkaline electrolyte and method for preparing bright nickel by means of electrolysis in alkaline electrolyte |
| CN105951133A (en) * | 2016-06-14 | 2016-09-21 | 浙江工业大学义乌科学技术研究院有限公司 | Alkaline electrolyte and nickel electroplating method in alkaline system |
| CN106498451A (en) * | 2016-10-31 | 2017-03-15 | 华北理工大学 | A kind of iron-nickel alloy low-carbon (LC) steel composite material and preparation method thereof |
| CN106498451B (en) * | 2016-10-31 | 2018-09-04 | 华北理工大学 | A kind of iron-nickel alloy-mild steel composite material and preparation method |
| CN106862580A (en) * | 2017-03-06 | 2017-06-20 | 河北工业大学 | A kind of boron nitride coats the preparation method of Fe-Ni nano-alloy |
| CN106862580B (en) * | 2017-03-06 | 2018-07-03 | 河北工业大学 | A kind of preparation method of boron nitride cladding Fe-Ni nano-alloy |
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