CN110129779A - A kind of method of the electroless plated iron of aluminum alloy surface - Google Patents
A kind of method of the electroless plated iron of aluminum alloy surface Download PDFInfo
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- CN110129779A CN110129779A CN201910507574.0A CN201910507574A CN110129779A CN 110129779 A CN110129779 A CN 110129779A CN 201910507574 A CN201910507574 A CN 201910507574A CN 110129779 A CN110129779 A CN 110129779A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/54—Contact plating, i.e. electroless electrochemical plating
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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
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/42—Pretreatment of metallic surfaces to be electroplated of light metals
- C25D5/44—Aluminium
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Abstract
The invention discloses a kind of methods of the electroless plated iron of aluminum alloy surface, comprising the following steps: aluminum alloy material surface polishing pretreatment；Pretreated aluminum alloy materials are immersed in aqueous slkali to remove oxide film dissolving and field trash, aluminum alloy materials after alkaline etching are immersed in acid solution to remove the black erosion generated during alkaline etching, aluminium alloy is immersed in chemical plating iron solution to the deposition for carrying out iron layer, chemistry leaching ferrous solution includes molysite, stripper and promotor.The present invention passes through electroless plated method, the iron layer that a layer thickness is 2-15 μm can be deposited within the aluminum alloy surface short period, and it is plated layer compact, smooth, the oxidation film of aluminum alloy surface is effectively removed after handling simultaneously, and the electrode potential on surface is greatly improved, and can be effectively improved the quality of coating in following electroplating process.Meanwhile the technical process is simple, can handle the aluminum alloy part of complicated shape, and cost is relatively low, high production efficiency, is suitble to large-scale production.
Description
Technical field
The invention belongs to aluminum alloy surface process fields, and in particular to a kind of to prepare plating iron layer in aluminum alloy surface
Solution formula and method.
Background technique
Aluminium and aluminium alloy are widely used in power electronics, boat since its specific strength is high, ductility is excellent, good conductivity
In many industrial departments such as sky, chemical industry, building and traffic and daily life, becomes current usage amount and be only second to the second largest of steel
Metalloid material.However, the surface hardness of aluminium and aluminium alloy is low, wears no resistance, limits it and further apply.Currently,
Develop a variety of process for treating surface to improve the surface abrasion resistance of aluminium alloy, as glow discharge nitriding, ion implanting, physical vapor are heavy
Product, differential arc oxidation and Laser Surface Treatment etc..These methods can effectively improve the surface property of aluminium and aluminium alloy, but there is also
Some drawbacks are carried out as glow discharge nitriding processing at 500 DEG C, and such high temperature will damage the mechanical property of aluminum substrate；Physics gas
Mutually deposition, differential arc oxidation and Laser Surface Treatment etc. require the technique of expensive equipment and complexity, this, which will increase, is surface-treated
Cost.Therefore, developing a kind of low temperature, simple process and lower-cost process for treating surface is aluminum alloy surface engineering neck
The important research direction in domain.
Plating is the modified important means of aluminum alloy surface.By electroplating technology, can aluminium surface deposit Fe, Ni,
The scuff-resistant coatings such as Cr, substantially increase the surface abrasion resistance of aluminum material, at the same be electroplated it is low for equipment requirements, and to the tissue of matrix
With performance without influence, thus obtain large-scale application.However, there are the dense oxides of one layer of self-assembling formation for aluminum alloy surface
Film, this layer of oxidation film seriously reduce the binding force of aluminium alloy surface electric plating layer and matrix, lead to the peeling or failure of coating.For
This, needs to carry out the pretreatment such as chemical zincation before plating on aluminium alloy, be pre-processed by chemical zincation, by strong in immersion plating zinc solution
Oxide film dissolving is removed in the effect of alkali, and is reacted by aluminum substrate with the displacement of Zn ion form zinc protective layer on surface simultaneously, and zinc is protected
The effect of sheath is to avoid electrode potential that is reoxidized and improving surface, then carries out electricity to aluminium alloy pretreated in this way
Plating, can obtain the extraordinary electroplated layer of binding force.But in the treatment process of this method, due to the Zn layer that is deposited
Also table is lower for current potential, is easy to occur to replace with plating solution during subsequent electroplated Ni, Cu etc. to react, and then influence electroplated layer
Deposition.Therefore, it is necessary to develop a kind of suitable immersion plating pretreating process to improve aluminium alloy electric coating quality.According to various metals
Electrode potential table can be used as suitable pre-plating layer it is found that the electrode potential of Fe is higher, but there is presently no mature aluminium alloys
Immersion plating iron process.
Summary of the invention
For the shortcoming of pre- immersion plating technology before current plating on aluminium alloy, the present invention provides a kind of simple process, at
This is cheap, and can prepare the electroless plated method for the iron plating being well combined with matrix, and in particular to its solution formula and
Immersion plating processes.
To achieve the above object, the invention provides the following technical scheme:
A kind of method of the electroless plated iron of aluminum alloy surface, comprising the following steps:
(1) aluminum alloy material surface pre-process: with sand paper to aluminum alloy material surface polish, then by aluminum alloy materials according to
Secondary be placed in acetone and dehydrated alcohol is cleaned by ultrasonic 5-10min, and drying obtains pretreated aluminum alloy materials；
(2) aluminum alloy surface alkaline etching and activation: pretreated aluminum alloy materials are immersed in aqueous slkali to remove oxidation
Film and field trash, alkaline etching technique are as follows: solution temperature is 40-60 DEG C, and the alkaline etching time is 20-50s；
Aluminum alloy materials after alkaline etching are immersed in acid solution to remove the black erosion generated during alkaline etching, pickling
Technique are as follows: acid solution temperature is room temperature, pickling time 30-60s；
(3) aluminum alloy surface immersion plating iron: step (2) treated aluminium alloy is immersed in chemical plating iron solution and carries out iron layer
Deposition；Immersion plating technology are as follows: chemical plating iron solution temperature is 25-100 DEG C, sedimentation time 1-20min；
Chemistry leaching ferrous solution includes molysite, stripper and promotor.
In step (2), the aqueous slkali is mixed by 50g/L sodium hydroxide and 2g/L neopelex.
In step (2), alkaline etching technique are as follows: solution temperature is 50 DEG C, and the alkaline etching time is 30s.
In step (2), the acid solution is that the water of concentrated nitric acid same volume dilutes, acid cleaning process are as follows: acid solution temperature
Degree is room temperature, pickling time 50s
In step (3), the molysite in the chemistry leaching ferrous solution is one in frerrous chloride, ferrous sulfate and ferric nitrate
Kind or several mixtures, the mass concentration of the molysite are 20-100g/L.
In step (3), the promotor in the chemistry leaching ferrous solution is made of thiocarbamide and fluoride, and the thiocarbamide quality is dense
Degree is 5-20g/L, and the mass concentration of the fluoride is 0.01-1g/L.
In step (3), the stripper in the chemistry leaching ferrous solution is in hydrofluoric acid, boric acid, citric acid and tartaric acid
One or two kinds of mixtures, the stripper mass concentration be 5-30g/L.
In step (3), the preparation method of the electroless plated ferrous solution, comprising the following steps:
By stripper deionized water dissolving, promotor and stirring and dissolving is then added, is eventually adding molysite and stirs molten
Solution, then required volume is settled to get the electroless plated ferrous solution.
The beneficial effects of the present invention are:
The present invention develops suitable electroless plated ferrous solution formula and immersion plating processes by electroless plated method, can
It is 2-15 μm of iron layer that a layer thickness is deposited within the aluminum alloy surface short period, and plated layer compact, smooth, while after handling
The oxidation film of aluminum alloy surface is effectively removed, and the electrode potential on surface is greatly improved, and can be effectively improved
The quality of coating in following electroplating process.Meanwhile the technical process is simple, can handle the aluminum alloy part of complicated shape, and at
This lower, high production efficiency is suitble to large-scale production.
Detailed description of the invention
Fig. 1 is the surface macro morphology of sample prepared by the embodiment of the present invention 3.
Fig. 2 is the cross section SEM photograph of sample prepared by the embodiment of the present invention 3.
Fig. 3 is the surface microscopic topographic and EDS power spectrum of sample prepared by the embodiment of the present invention 3.
Specific embodiment
Embodiment 1
A kind of method of the electroless plated iron of aluminum alloy surface, comprising the following steps:
(1) aluminum alloy material surface pre-process: with sand paper to aluminum alloy material surface polish, then by aluminum alloy materials according to
Secondary be placed in acetone and dehydrated alcohol is cleaned by ultrasonic 5-10min, and drying obtains pretreated aluminum alloy materials；
(2) aluminum alloy surface alkaline etching and activation: pretreated aluminum alloy materials are immersed in aqueous slkali to remove oxidation
Film and field trash, the aqueous slkali are mixed by 50g/L sodium hydroxide and 2g/L neopelex, alkaline etching technique
Are as follows: solution temperature is 50 DEG C, and the alkaline etching time is 30s；
Aluminum alloy materials after alkaline etching are immersed to remove the black erosion generated during alkaline etching in acid solution, it is described
Acid solution is that the water of concentrated nitric acid same volume dilutes, acid cleaning process are as follows: acid solution temperature is room temperature, pickling time 50s；
(3) aluminum alloy surface immersion plating iron: step (2) treated aluminium alloy is immersed in chemical plating iron solution and carries out iron layer
Deposition；Immersion plating technology are as follows: chemical plating iron solution temperature is 25 DEG C, sedimentation time 1min；
Chemistry leaching ferrous solution includes 20g/L molysite, 5g/L stripper and 5.1g/L promotor, and wherein molysite is protochloride
Iron, stripper are hydrofluoric acid, and promotor is made of 5g/L thiocarbamide and 0.1g/L ammonium fluoride.
Chemistry leaching ferrous solution preparation steps are as follows:
(1) thiocarbamide and ammonium fluoride of the above-mentioned concentration of deionized water dissolving of 500mL are used, and is stirred well to and is completely dissolved；
(2) hydrofluoric acid of normal concentration is added in Xiang Shangshu solution, and is sufficiently stirred；
(3) 200ml deionized water dissolving 20g frerrous chloride is used, after stirring to clarify, (1) (2) step is added thereto
Mixed liquor obtained, stirs evenly, and then uses deionized water constant volume to 1L to get the electroless plated ferrous solution.
For XRD diffraction analysis overlay coating mainly by α-Fe phase composition, the cross section of scanning electron microscopic observation sample shows coating
With a thickness of 0.9-1.1 μm, the surface of scanning electron microscopic observation sample shows that the crystallite dimension of coating is 490-510nm.
The difference of following embodiment and embodiment 1 is only that,
Embodiment 2
Chemistry leaching ferrous solution in the implementation case includes 45g/L molysite, 10g/L stripper and 8.5g/L promotor,
Middle molysite is frerrous chloride, and stripper is hydrofluoric acid, and promotor is made of 8g/L thiocarbamide and 0.5g/L ammonium fluoride.
Chemistry leaching ferrous solution preparation steps are as follows:
(1) thiocarbamide and ammonium fluoride of the above-mentioned concentration of deionized water dissolving of 500mL are used, and is stirred well to and is completely dissolved；
(2) hydrofluoric acid of normal concentration is added in Xiang Shangshu solution, and is sufficiently stirred；
(3) 200ml deionized water dissolving 45g ferrous sulfide is used, after stirring to clarify, (1) (2) step is added thereto
Mixed liquor obtained, stirs evenly, and then uses deionized water constant volume to 1L up to the electroless plated ferrous solution.
Operating temperature is 50 DEG C when immersion plating, time 5min.
It is black, plated layer compact, without appearance the problems such as blistering, fall off that sample surfaces are observed after plating.
XRD diffraction analysis overlay coating is mainly by α-Fe phase composition.
The cross section of scanning electron microscopic observation sample show coating with a thickness of 3.9-4.1 μm, scanning electron microscopic observation sample
Surface shows that the crystallite dimension of coating is 280-310nm.
Embodiment 3
Chemistry leaching ferrous solution in the implementation case includes 50g/L molysite, 15g/L stripper and 6g/L promotor, wherein
Molysite is frerrous chloride, and stripper is made of 14g/L hydrofluoric acid and 1g/L boric acid, and promotor is by 5g/L thiocarbamide and 1g/L ammonium fluoride
Composition.
Chemistry leaching ferrous solution preparation steps are as follows:
(1) thiocarbamide and ammonium fluoride of the above-mentioned concentration of deionized water dissolving of 500mL are used, and is stirred well to and is completely dissolved；
(2) hydrofluoric acid and boric acid of normal concentration are added in Xiang Shangshu solution, and is sufficiently stirred；
(3) 200ml deionized water dissolving 50g frerrous chloride is used, after stirring to clarify, (1) (2) step is added thereto
Mixed liquor obtained, stirs evenly, and then uses deionized water constant volume to 1L up to the electroless plated ferrous solution.
Operating temperature is 65 DEG C when immersion plating, time 10min.
It is black, plated layer compact, without appearance the problems such as blistering, fall off that sample surfaces are observed after plating.
For XRD diffraction analysis overlay coating mainly by α-Fe phase composition, the cross section of scanning electron microscopic observation sample shows coating
With a thickness of 4.8-5.1 μm, the surface of scanning electron microscopic observation sample shows that the crystallite dimension of coating is 76-83nm.
Embodiment 4
Chemistry leaching ferrous solution in the implementation case includes 60g/L molysite, 15g/L stripper and 6g/L promotor, wherein
Molysite is ferrous sulfide, and stripper is made of 14g/L hydrofluoric acid and 1g/L boric acid, and promotor is by 5g/L thiocarbamide and 1g/L ammonium fluoride
Composition.
Chemistry leaching ferrous solution preparation steps are as follows:
(1) thiocarbamide and ammonium fluoride of the above-mentioned concentration of deionized water dissolving of 500mL are used, and is stirred well to and is completely dissolved；
(2) hydrofluoric acid and boric acid of normal concentration are added in Xiang Shangshu solution, and is sufficiently stirred；
(3) 200ml deionized water dissolving 60g ferrous sulfide is used, after stirring to clarify, (1) (2) step is added thereto
Mixed liquor obtained, stirs evenly, and then uses deionized water constant volume to 1L up to the electroless plated ferrous solution.
Operating temperature is 65 DEG C when immersion plating, time 10min.
It is black, plated layer compact, without appearance the problems such as blistering, fall off that sample surfaces are observed after plating.
XRD diffraction analysis overlay coating is mainly by α-Fe phase composition.
The cross section of scanning electron microscopic observation sample show coating with a thickness of 2.9-3.1 μm, scanning electron microscopic observation sample
Surface shows that the crystallite dimension of coating is 180-210nm.
Embodiment 5
Chemistry leaching ferrous solution in the implementation case includes 80g/L molysite, 15g/L stripper and 6g/L promotor, wherein
Molysite is frerrous chloride, and stripper is made of 10g/L hydrofluoric acid and 5g/L boric acid, and promotor is by 5g/L thiocarbamide and 1g/L ammonium fluoride
Composition.
Chemistry leaching ferrous solution preparation steps are as follows:
(1) thiocarbamide and ammonium fluoride of the above-mentioned concentration of deionized water dissolving of 500mL are used, and is stirred well to and is completely dissolved；
(2) hydrofluoric acid and boric acid of normal concentration are added in Xiang Shangshu solution, and is sufficiently stirred；
(3) 200ml deionized water dissolving 80g frerrous chloride is used, after stirring to clarify, (1) (2) step is added thereto
Mixed liquor obtained, stirs evenly, and then uses deionized water constant volume to 1L up to the electroless plated ferrous solution.
Operating temperature is 80 DEG C when immersion plating, time 10min.
It is black, plated layer compact, without appearance the problems such as blistering, fall off that sample surfaces are observed after plating.
XRD diffraction analysis overlay coating is mainly by α-Fe phase composition.
The cross section of scanning electron microscopic observation sample show coating with a thickness of 7.8-8.2 μm, scanning electron microscopic observation sample
Surface shows that the crystallite dimension of coating is 77-83nm.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.Any reference signs in the claims should not be construed as limiting the involved claims.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (8)
1. a kind of method of the electroless plated iron of aluminum alloy surface, which comprises the following steps:
(1) aluminum alloy material surface pre-processes: being polished with sand paper aluminum alloy material surface, then successively sets aluminum alloy materials
It is cleaned by ultrasonic 5-10min in acetone and dehydrated alcohol, dries up, obtain pretreated aluminum alloy materials；
(2) aluminum alloy surface alkaline etching and activation: by pretreated aluminum alloy materials immerse aqueous slkali in go oxide film dissolving and
Field trash, alkaline etching technique are as follows: solution temperature is 40-60 DEG C, and the alkaline etching time is 20-50s；
Aluminum alloy materials after alkaline etching are immersed in acid solution to remove the black erosion generated during alkaline etching, acid cleaning process
Are as follows: acid solution temperature is room temperature, pickling time 30-60s；
(3) aluminum alloy surface immersion plating iron: step (2) treated aluminium alloy is immersed in chemical plating iron solution and carries out the heavy of iron layer
Product；Immersion plating technology are as follows: chemical plating iron solution temperature is 25-100 DEG C, sedimentation time 1-20min；
Chemistry leaching ferrous solution includes molysite, stripper and promotor.
2. the method for the electroless plated iron of aluminum alloy surface according to claim 1, which is characterized in that described in step (2)
Aqueous slkali is mixed by 50g/L sodium hydroxide and 2g/L neopelex.
3. the method for the electroless plated iron of aluminum alloy surface according to claim 1, which is characterized in that in step (2), alkaline etching
Technique are as follows: solution temperature is 50 DEG C, and the alkaline etching time is 30s.
4. the method for the electroless plated iron of aluminum alloy surface according to claim 1, which is characterized in that described in step (2)
Acid solution is that the water of concentrated nitric acid same volume dilutes, acid cleaning process are as follows: acid solution temperature is room temperature, pickling time 50s.
5. the method for the electroless plated iron of aluminum alloy surface according to claim 1, which is characterized in that described in step (3)
Molysite in chemistry leaching ferrous solution is one or more of frerrous chloride, ferrous sulfate and ferric nitrate mixture, the iron
The mass concentration of salt is 20-100g/L.
6. the method for the electroless plated iron of aluminum alloy surface according to claim 1, which is characterized in that described in step (3)
Promotor in chemistry leaching ferrous solution is made of thiocarbamide and fluoride, and the thiocarbamide mass concentration is 5-20g/L, the fluoride
Mass concentration be 0.01-1g/L.
7. the method for the electroless plated iron of aluminum alloy surface according to claim 1, which is characterized in that described in step (3)
Stripper in chemistry leaching ferrous solution is one or both of hydrofluoric acid, boric acid, citric acid and tartaric acid mixture, described
Stripper mass concentration is 5-30g/L.
8. the method for the electroless plated iron of aluminum alloy surface according to claim 1, which is characterized in that described in step (3)
Electroless plated ferrous solution is prepared with the following method:
By stripper deionized water dissolving, promotor and stirring and dissolving is then added, is eventually adding molysite and stirring and dissolving, then
Required volume is settled to get the electroless plated ferrous solution.
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Cited By (1)
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| CN110423977A (en) * | 2019-09-05 | 2019-11-08 | 合肥工业大学 | One kind is with electroless plated iron for pretreated aluminum material gas nitriding process |
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