CN104451616A - Chemical nickel plating method for 4Cr13 stainless steel - Google Patents

Chemical nickel plating method for 4Cr13 stainless steel Download PDF

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Publication number
CN104451616A
CN104451616A CN201410721016.1A CN201410721016A CN104451616A CN 104451616 A CN104451616 A CN 104451616A CN 201410721016 A CN201410721016 A CN 201410721016A CN 104451616 A CN104451616 A CN 104451616A
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CN
China
Prior art keywords
nickel
nickel plating
chemical nickel
plating
stainless steel
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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.)
Pending
Application number
CN201410721016.1A
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Chinese (zh)
Inventor
陈祝桥
徐涛涛
王道军
徐超
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Tianjin Aviation Mechanical and Electrical Co Ltd
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Tianjin Aviation Mechanical and Electrical Co Ltd
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Application filed by Tianjin Aviation Mechanical and Electrical Co Ltd filed Critical Tianjin Aviation Mechanical and Electrical Co Ltd
Priority to CN201410721016.1A priority Critical patent/CN104451616A/en
Publication of CN104451616A publication Critical patent/CN104451616A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/16Chemical 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 by reduction or substitution, e.g. electroless plating
    • C23C18/31Coating with metals
    • C23C18/32Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/16Chemical 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 by reduction or substitution, e.g. electroless plating
    • C23C18/18Pretreatment of the material to be coated

Abstract

The invention provides a chemical nickel plating method for 4Cr13 stainless steel. With 4Cr13 stainless steel as a difficult-to-plate material, a qualified coating cannot be obtained by using an existing chemical nickel plating method; and the coating peels and falls off during binding force detection after chemical nickel plating is carried out. According to the chemical nickel plating method, through adopting nickel plating processes of pretreatment, tri-acid corrosion, surface dusting removal, nickel preplating and chemical nickel plating, and selecting a proper solution formula and process parameters, the binding force of the coating is increased, and the qualified coating is obtained. The method is stable in pretreatment process, is suitable for chemical nickel plating treatment of a 4Cr13 stainless steel material, and is also suitable for pretreatment of other electroplating and chemical plating of the 4Cr13 stainless steel material.

Description

A kind of for the stainless chemical nickel plating method of 4Cr13
Technical field
The invention belongs to chemical plating nickel technology, particularly a kind of stainless steel chemical nickel plating method.
Background technology
By electrolysis or the chemical process method at metal or some nonmetal plating last layer nickel, be called nickel plating.Nickel plating divides electronickelling and chemical nickel plating.Electroless plating is also called electroless plating (Electroless plating), also can be called autocatalysis plating (Autocatalytic plating).Detailed process refers to: under certain condition, and the metal ion in the aqueous solution is reduced agent reduction, and is deposited to the process on solid matrix surface.Autocatalytic plating is " depositionof a metallic coating by a controlled chemical reduction that is catalyzed by the metalor alloy being deposited " is defined as in ASTMB374 (ASTM, American Society Testing and Materials).This process is plated different from displacement, and its coating can constantly thicken, and plating metal itself also has catalytic capability.
The difficult plating material of 4Cr13 stainless steel, uses existing chemical plating nickel technology cannot obtain qualified coating, carries out peeling and coming off (as shown in Figure 1) when bonding force detects after chemical nickel plating.In fields such as part plating and electroless platings, the accordance of binding force of cladding material is particularly important.
Summary of the invention
For the problem of prior art, the object of the present invention is to provide a kind of for the stainless chemical nickel plating method of 4Cr13, described method is by rational technical process, solution formula and processing parameter, the coating that bonding force is qualified can be obtained, non-scale and coming off, may be used in the plating of large quantities of part, chemical plating technology.
To achieve these goals, present invention employs following technical scheme:
The stainless chemical nickel plating method of a kind of 4Cr13, said method comprising the steps of:
(1) acid corrosion: at room temperature immersed in acid corrosion solution by the part that 4Cr13 stainless material is processed and carry out etch process, until there is yellow gas evolution only;
(2) dust is gone: be after the part clear water flushing of grey black by the surface that step (1) obtains, at room temperature immerse and go, in dust solution, to remove completely, till exposing metalluster to black dust;
(3) nickel preplating: the part that step (2) obtains is proceeded in nickel preplating groove, at room temperature carries out nickel preplating process;
(4) chemical nickel plating: proceeding in the chemical nickel-plating solution configured by completing the part after nickel preplating, carrying out chemical nickel plating process to desired thickness.
In the present invention, the stainless chemical nickel plating method of 4Cr13 comprises three step pretreatment activating techniques, the zone of oxidation of acid corrosion stainless steel surface, dust technique is gone effectively to be removed by surface corrosion product, the transition layer that nickel preplating provides bonding force good for chemical nickel plating, the binding force of cladding material that this stainless steel chemical nickel plating method obtains is good; The stainless steel pre-treating technology that the method provides is stablized, and treating processes is easy to control, and coating qualification rate is high, is applied to the chemical nickel plating process of the 4Cr13 stainless steel components of all states.
In the present invention, acid corrosion, for dissolving the oxide skin of the fine and close indissoluble of stainless steel surface and natural passive film, comprises the dissolving of the insoluble metal oxide compound such as chromic oxide, oxidation siderochrome; Go dust, for purifying the etch product of stainless steel surface, adopting the solution removal dust containing strong oxidizer, making it expose unoxidized matrix surface; Nickel preplating, for the nickel dam in the densification of stainless steel surface flash last layer, prevent stainless steel base passivation again, for the bottom as chemical nickel plating, pre-nickel plating is combined with stainless steel surface firmly, for subsequent chemistry nickel plating technology provides the intermediate metal that bonding force is good.
In the present invention, the part of step (1) described 4Cr13 stainless material processing is through following pre-treatment:
The part that 4Cr13 stainless material is processed is carried out electrochemical deoiling process, cleans out the greasy dirt on surface.
In the present invention, described acid corrosion solution composition is: hydrofluoric acid (80-100) ml/L, such as 82ml/L, 84ml/L, 86ml/L, 88ml/L, 90ml/L, 92ml/L, 94ml/L, 96ml/L or 98ml/L, hydrochloric acid (50-80) ml/L, such as 53ml/L, 56ml/L, 59ml/L, 62ml/L, 65ml/L, 68ml/L, 71ml/L, 74ml/L or 77ml/L, nitric acid (200-250) ml/L, such as 205ml/L, 210ml/L, 215ml/L, 220ml/L, 225ml/L, 230ml/L, 235ml/L, 240ml/L or 245ml/L.。
The concentration of exemplary hydrofluoric acid is such as 40%, and the density of hydrochloric acid is 1.19g/cm 3, the density of nitric acid is 1.42g/cm 3.
In the present invention, describedly dust solution composition is gone to be: nitric acid (30-50) ml/L, such as 32ml/L, 34ml/L, 36ml/L, 38ml/L, 40ml/L, 42ml/L, 44ml/L, 46ml/L or 48ml/L, hydrogen peroxide (15-25) ml/L, such as 16ml/L, 17ml/L, 18ml/L, 19ml/L, 20ml/L, 21ml/L, 22ml/L, 23ml/L or 24ml/L.
The density of exemplary nitric acid is 1.42g/cm 3, the concentration of hydrogen peroxide is 30%.
In the present invention, the pre-plating solution that nickel preplating adopts consists of: single nickel salt (240-260) g/L, such as 242g/L, 244g/L, 246g/L, 248g/L, 250g/L, 252g/L, 254g/L, 256g/L or 258g/L, magnesium sulfate (30-50) g/L, such as 32g/L, 34g/L, 36g/L, 38g/L, 40g/L, 42g/L, 44g/L, 46g/L or 48g/L, hydrochloric acid (20-40) ml/L.
The density of exemplary hydrochloric acid is 1.19g/cm 3.
In the present invention, the current density of nickel preplating is (5-10) A/dm 2, the current efficiency of the more conventional electronickelling of this current density is higher, is unlikely to occur that coated metal is mingled with too much, such as 6A/dm while guaranteeing coating production rate 2, 7A/dm 2, 8A/dm 2or 9A/dm 2, the time is 10 ~ 20min.
Compared with the prior art, the present invention has following beneficial effect:
(1) by semiquantitative bonding force testing method-square method, binding force of cladding material is tested, the coating area ratio that comes off reduces greatly, about 0.1% is dropped to by 5%, bonding force significantly improves, can be applicable to the stainless steel bearing pin plating of Φ <1mm, and guarantee that bending there will not be coating obscission.
(2) acid corrosion of the present invention does not corrode on the basis of stainless steel base in guarantee, dissolve surface scale and passive film thoroughly, and etch end point has advantage easy to observe the control, can obtain totally after going dust process, non-passivation, be easy to electroplate stainless steel-based surface.
(3) in order to reach good preplating effect, acid corrosion operation with go dust operation after carry out surperficial nickel preplating process immediately, the nickel preplating formula of high nickel sulfate content can form rapidly fine and close nickel dam in stainless steel-based surface, play an important role to the bonding force improving coating and matrix.
(4) the method pre-treating technology is stablized, and is not only applicable to the chemical nickel plating process of 4Cr13 stainless material, is also applicable to other plating of 4Cr13 stainless material, the pre-treatment of electroless plating.
Accompanying drawing explanation
Fig. 1 is the photo of defective coating;
Fig. 2 is the photo of qualified coating.
Embodiment
Technical scheme of the present invention is further illustrated below by embodiment.
A kind of for the stainless chemical nickel plating method of 4Cr13, its technical process, solution formula and processing parameter are as follows:
Process structure comprises, pre-treatment-acid corrosion-remove dust-nickel preplating-chemical nickel plating
Acid corrosion solution composition and relevant processing parameter
Solution composition and working conditions Processing parameter
Hydrofluoric acid HF (40%) ml/L 80-100
Hydrochloric acid HCl (density 1.19g/cm 3)ml/L 50-80
Nitric acid HNO 3(density 1.42g/cm 3)ml/L 200-250
Temperature (DEG C) Room temperature
Time (min) To only separating out yellow gas
Remove dust solution composition and relevant processing parameter
Solution composition and working conditions Processing parameter
Oxydol H 2O 2(30%)ml/L 15-25
Nitric acid HNO 3(density 1.42g/cm 3)ml/L 30-50
Temperature (DEG C) Room temperature
Time (min) Remove to black dust
Pre-nickel plating solution composition and relevant processing parameter
Solution composition and working conditions Processing parameter
Single nickel salt (NiSO 4)g/L 240-260
Magnesium sulfate (MgSO 4)g/L 30-50
Hydrochloric acid HCl (density 1.19g/cm 3)ml/L 20-40
Temperature (DEG C) Room temperature
Current density (A/dm 2) 5-10
The cathode treatment time (min) 15min
Anode material Nickel plate
A kind of as follows for 4Cr13 stainless chemical nickel plating method flow process:
The part that 4Cr13 stainless material is processed is carried out electrochemical deoiling process, cleans out the greasy dirt etc. on surface; Part after oil removing is immersed in acid corrosion solution and carries out etch process, until there is yellow gas evolution only; Be after the part clear water flushing of grey black by surface, immerse and go, in dust solution, to remove completely, till exposing metalluster to black dust; At once the part completing above-mentioned operation is proceeded in nickel preplating groove, carry out nickel preplating process; Proceeding in the chemical nickel-plating solution configured by completing the part after nickel preplating, carrying out chemical nickel plating process to desired thickness.
Should note the changing conditions of observing piece surface in pretreatment process during operation, nickel preplating process performs in strict accordance with pre-nickel plating solution composition and relevant processing parameter, and the technology stability as far as possible avoiding human factor to cause is poor.
Specific embodiment 1 ~ 3
Adopt foregoing method to carry out chemical nickel plating, acid corrosion solution composition and relevant processing parameter as follows:
Remove dust solution composition and relevant processing parameter
Pre-nickel plating solution composition and relevant processing parameter
Adopt the method for above-mentioned specific embodiment 1 ~ 3, the nickel layer outward appearance obtained at 4Cr13 stainless steel surface is homogeneous, adopts " square method " bonding force to coating to test, and the come off ratio of area of the coating obtained is less than 0.1%; Adopt bending method to carry out binding force of cladding material test, all without coating obscission simultaneously.
Applicant states, 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 namely 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, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.

Claims (6)

1., for the stainless chemical nickel plating method of 4Cr13, it is characterized in that, said method comprising the steps of:
(1) acid corrosion: at room temperature immersed in acid corrosion solution by the part that 4Cr13 stainless material is processed and carry out etch process, until there is yellow gas evolution only;
(2) dust is gone: be after the part clear water flushing of grey black by the surface that step (1) obtains, at room temperature immerse and go, in dust solution, to remove completely, till exposing metalluster to black dust;
(3) nickel preplating: the part that step (2) obtains is proceeded in nickel preplating groove, at room temperature carries out nickel preplating process;
(4) chemical nickel plating: proceeding in the chemical nickel-plating solution configured by completing the part after nickel preplating, carrying out chemical nickel plating process to desired thickness.
2. the method for claim 1, is characterized in that, the part of step (1) described 4Cr13 stainless material processing is through following pre-treatment:
The part that 4Cr13 stainless material is processed is carried out electrochemical deoiling process, cleans out the greasy dirt on surface.
3. method as claimed in claim 1 or 2, it is characterized in that, described acid corrosion solution composition is: hydrofluoric acid (80-100) ml/L, hydrochloric acid (50-80) ml/L, nitric acid (200-250) ml/L.
4. the method as described in one of claim 1-3, is characterized in that, described in go dust solution composition to be: nitric acid (30-50) ml/L, hydrogen peroxide (15-25) ml/L.
5. the method as described in one of claim 1-4, is characterized in that, the pre-plating solution that nickel preplating adopts consists of: single nickel salt (240-260) g/L, magnesium sulfate (30-50) g/L, hydrochloric acid (20-40) ml/L.
6. the method as described in one of claim 1-5, is characterized in that, the current density of nickel preplating is (5-10) A/dm 2, the time is 10 ~ 20min.
CN201410721016.1A 2014-12-02 2014-12-02 Chemical nickel plating method for 4Cr13 stainless steel Pending CN104451616A (en)

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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN105483784A (en) * 2015-12-30 2016-04-13 无锡透平叶片有限公司 Turbine blade and surface pretreatment method thereof
CN107876702A (en) * 2017-11-14 2018-04-06 南昌航空大学 A kind of method for strengthening sprue cup mould
CN110760860A (en) * 2019-10-30 2020-02-07 湖南金裕环保科技有限公司 Stainless steel surface dedusting agent, preparation method and application
CN111740300A (en) * 2020-05-22 2020-10-02 合肥圣达电子科技实业有限公司 Manufacturing process of packaging shell for high-power laser
WO2022088216A1 (en) * 2020-10-28 2022-05-05 瑞声声学科技(深圳)有限公司 Chemical nickel-plating process for steel sheet, phosphorus-nickel-plated steel sheet and vapor chamber

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105483784A (en) * 2015-12-30 2016-04-13 无锡透平叶片有限公司 Turbine blade and surface pretreatment method thereof
CN107876702A (en) * 2017-11-14 2018-04-06 南昌航空大学 A kind of method for strengthening sprue cup mould
CN107876702B (en) * 2017-11-14 2020-07-24 南昌航空大学 Method for reinforcing pouring cup mold
CN110760860A (en) * 2019-10-30 2020-02-07 湖南金裕环保科技有限公司 Stainless steel surface dedusting agent, preparation method and application
CN111740300A (en) * 2020-05-22 2020-10-02 合肥圣达电子科技实业有限公司 Manufacturing process of packaging shell for high-power laser
WO2022088216A1 (en) * 2020-10-28 2022-05-05 瑞声声学科技(深圳)有限公司 Chemical nickel-plating process for steel sheet, phosphorus-nickel-plated steel sheet and vapor chamber

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Application publication date: 20150325