CN101705509A - Low-stress nickel plating technology - Google Patents
Low-stress nickel plating technology Download PDFInfo
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Abstract
The invention provides a low-stress nickel plating technology which takes nickel salt as main salt and obtains a protective layer with low internal stress, high hardness, strong binding force and very superior ductility by checking a plating solution, removing the stress of a material to be plated, anode electrolytic oil removing, etching, nickel preplating, nickel plating and heat treatment. The technology is simple to operate and easy to maintain, has high work efficiency, less pollution to environment and simple sewage treatment, can be widely applied in the protective treatment of low alloy and high strength steel parts of aviation engines, and can be popularized and applied to the protective aspects of the low alloy and high strength steel parts of aviation and aerospace engines, civilian use products and the like and other parts.
Description
Technical field
The invention belongs to technology corrosion and protection technical field, particularly a kind of protection processing method of Hi-Stren steel part.
Background technology
Low alloy steel belongs to high-quality steel series, and it is the various alloying elements that add trace in common steel grade.
The Hi-Stren steel part that is used for aircraft industry need carry out protective treatment, and according to the difference of its Working environment, also different for the protective layer performance demands.Provide certain anti-oxidant and resistance to corrosion to the Hi-Stren steel part of under medium high temperature, working, require to have in the coating lower tension stress to avoid obviously reducing fatigue strength.The protective layer of low-stress is adopted in requirement as fastening piece, and simultaneously, the pre-treatment of part and the whole process of plating also must be controlled the generation of hydrogen embrittlement.
Nickel is the metal of white light yellow complexion, has ferromegnetism.Usually, there is one deck passive film, thereby has higher chemical stability on its surface.At normal temperatures, all be stable to water and air.The nickel electrode current potential than ferroelectric electrode potential just, after the nickel surface passivation, electropotential corrigendum, thereby the nickel coating on the iron-based body is a cathodic electrodeposition coating.Nickel coating now has been widely used for all respects such as the decoration of many conductors such as steel, copper, aluminium, plastics or non-metallic material and protection.The performance of nickel coating and the nickel plating technology of employing have substantial connection, and technology difference, the performance of the nickel coating of acquisition are also different.As functional coating, can be as repair electroplating, be worn, be corroded, or the plating coating thicker than actual needs on the processing over-drastic part passes through mechanical workout then, makes it reach the size of regulation.In addition, select suitable plating bath, can at full speed plate good toughness, nickel coating that internal stress is low.
Coating stress can pass through the nickel plating of red copper test piece single face, and the crooked situation of test piece judges, coating towards on curve concave surface, show the state of tension of coating, the concave curvature of coating face represents that the pulling force of coating, test piece do not have tensile stress and show; Carry out the hydrogen embrittlement test inspection in addition: adopt the stable dress sample that carries of axially parallel rounded groove steel with grain flow, nickel layer thickness is not less than 0.13mm, the 8h that eliminates stress changes in the mechanical property that loads under the endurance testing machine of 3-5 ton after certain static loads (stress) is evaluated the material electroplating processes.75% of loading stress notch strength σ bH continues 200 hours on the static load of regulation, coupon is not disrumpent feelings or do not crack.
Traditional nickel plating technology, hydrogen embrittlement test will rupture in 2 hours even shorter time.
Summary of the invention
The object of the present invention is to provide a kind of low-stress nickel plating technology, be specially adapted to the protective treatment of Hi-Stren steel part, the internal stress of the settled layer that this technology obtained is low, hardness is high, and bonding force is strong, and has very superior ductility.
The present invention specifically provides a kind of low-stress nickel plating technology; this technology is main salt with nickel salt; by check plating bath, remove the material stress that plates, anode electrolysis oil removing, burn into nickel preplating, nickel plating and thermal treatment acquisition internal stress be low; the hardness height; bonding force is strong, and has the protective layer of very superior ductility.
A kind of low-stress nickel plating technology provided by the present invention is characterized in that these technology concrete steps are:
(a), check plating bath: the steel wire of use ¢ 0.8 is converted into the circle of ¢ 75, dips in the transparence film 20S that produces along circumference behind the plating bath and does not break for qualified; The purpose of checking: whether the addition of checking sodium lauryl sulphate in the plating bath is enough.
(b), destressing: institute's plating part is placed 3~4h under 246 ℃ ± 14 ℃ temperature.
(c), anode electrolysis oil removing: the part after the destressing placed except that oil solution carry out the anode electrolysis oil removing, check the continuity of piece surface moisture film in 10-30 of plating, as if then qualified continuously; Purpose: remove the pollutions such as material surface greasy dirt, hand perspiration of plating, improve the bonding force of coating.
The composition and the constituent concentration that wherein remove oil solution are: NaOH 30-70g/l, Na
2CO
330-100g/l, Na
3PO
410-30g/l, Na
2SiO
33-10g/l; The oil removing current density is 3~5A/dm
2, 60~80 ℃ of temperature, time 2~3min.
(d), corrosion: at room temperature, place etchant solution to corrode 0.5-1min the material after the oil removing; Purpose: remove the slight oxidation film of the material surface that plates, make the material surface activation.
Wherein the composition of etchant solution and constituent concentration are: hydrochloric acid 150-200ml/l, if fourth 1~2g/l;
(e), nickel preplating: at room temperature, the material after the corrosion is placed pre-nickel plating solution 1~4min, galvanization 3~5min in pre-nickel plating solution again, current density is 5~8A/dm
2Purpose: improve the release that binding force of cladding material promotes hydrogen simultaneously.
Wherein the composition of pre-nickel plating solution and constituent concentration are: NiCl
2.6H
2O 200~250g/l, HCl180~220g/l.
(f), nickel plating: it is the nickel plating of switching on of the nickel plating solution of 3.5-4.2 that the material behind the nickel preplating is placed PH, and the nickel plating time is 32-210min, and the nickel plating temperature is 40-70 ℃; Cathode current density is 1~4A/dm
2
Wherein the composition of nickel plating solution and constituent concentration are: nickel sulfamic acid 270-330g/l, boric acid 40-60g/l, sodium-chlor 15-30g/l, 0.3g/l≤sodium lauryl sulphate<0.8g/l.
(g), thermal treatment: temperature is 246 ± 14 ℃, and the time is 8h ± 15min.Purpose: remove the hydrogen that electroplating process infilters.
One of obvious characteristics of the present invention is; do not use any destressing additive; and just having added the protective layer that a spot of moistened surface agent sodium lauryl sulphate obtains low-stress, this is in order to prevent owing to adding the negative impact that the destressing agent brings for the toughness of coating performance such as coating, corrosion resisting property etc.
Another obvious characteristic of the present invention is that the timed interval between above-mentioned steps (f) and the step (g) is less than 60min, preferably is controlled within the 30min.Because prolongation along with pitch time between two steps, the protium that penetrates into matrix in the electroplating process As time goes on, constantly to the matrix internal divergence, causing protium to discharge can increase according to the concentration difference principle, thereby the stress of coating is increased, rupture in the hydrogen embrittlement coupon drawing process.The contriver sums up by several thousand times test-results over 4 years, and the timed interval between step (f) and the step (g) is less than 60min, preferably is controlled within the 30min, and the coating hydrogen embrittlement of gained test percent of pass significantly improves like this.
A kind of low-stress nickel plating technology provided by the present invention is characterized in that the destressing temperature is preferably 246 ℃ in the above-mentioned steps (b), and the time is preferably 4h.The nickel plating temperature is preferably 60 ℃ in the step (f).
A kind of low-stress nickel plating technology provided by the present invention is characterized in that the bed thickness of nickel preplating in the above-mentioned steps (e) preferably is controlled at 2.5 μ m.
A kind of low-stress nickel plating technology provided by the present invention is characterized in that the PH of nickel plating solution in the above-mentioned steps (f) is preferably 4, and stirs plating bath with the filtering pressurized air of the process of cleaning when nickel plating, so that institute's nickel layer is even.The layer thickness control of nickel plating is best between 0.008mm~0.038mm.
A kind of low-stress nickel plating technology provided by the present invention, be specially adapted to the protective treatment of the Hi-Stren steel part in the aircraft industry, the Hi-Stren steel part that is used for aircraft industry need carry out protective treatment, and according to the difference of its Working environment, also different for the protective layer performance demands. require to adopt the protective layer of low-stress as fastening piece. therefore, the pre-treatment of part and the generation of electroplating all necessary control hydrogen embrittlement of whole process. the internal stress of the settled layer that technology obtained that we study is low, the hardness height, bonding force is strong, and having very superior ductility. hydrogen embrittlement test reaches the requirement of American army mark ASTM519. and the key problem in technology of its required breakthrough is to continue 200 hours on the static load of regulation, coupon is not disrumpent feelings or do not crack. the success of the test of nickel plating technology of the present invention, fundamentally solved the key issue that the hydrogen embrittlement coupon ruptures and cracks in drawing process. simultaneously, introduce automatic control system, production process control and real time on-line monitoring function have automatically been realized, solved the quality instability that causes because of personal errors, the problem of process monitoring ability. this technical matters is simple, easy handling and maintenance. this technology has been applied in the production process of aircraft engine Hi-Stren steel part, respond well, performance, state is highly stable, satisfy the protective treatment technical requirements of Hi-Stren steel part in the aircraft industry, this technology can also be promoted towards the same industry simultaneously, popularize.
The present invention adopts the tank liquor that meets the special process requirement, by selecting suitable tank liquor prescription and processing parameter, obtains best protective coating, has fundamentally solved the protection problem of Hi-Stren steel part.
The coating that uses low-stress nickel plating technology provided by the invention to obtain all obtains test result preferably by following test:
Solidity to corrosion test adopts ASTM B117 to carry out the continuous salt air corrosion experiment of 48 ± 1h among the present invention, the workpiece working face that the plates obvious corrosion sign that do not have.
The method of stipulating among the ASM2424D is adopted in the thermotolerance test among the present invention: be heated to 538 ℃ ± 8 ℃ in the recirculated air stove, and more than the insulation 2h, coating does not have foaming and crackle.
The method of stipulating among the ASM2424D is adopted in the sticking power test among the present invention: the test piece specification is 0.81 * 25 * 102mm, behind crooked about 180 ° of the diameter that is equivalent to its thickness twice, amplify 4 times of inspections, the coating of sample does not have and peels off, and can not cause plating exfoliation and blistered crackle to form is to allow.
Hydrogen embrittlement test adopts the method for regulation among the ASTM F 519 among the present invention: adopt the stable dress sample that carries of axially parallel with grain flow rounded groove steel, nickel layer thickness is not less than 0.13mm, the 8h that eliminates stress changes in the mechanical property that loads under the endurance testing machine of 3-5 ton after certain static loads (stress) is evaluated the material electroplating processes.75% of loading stress notch strength σ bH continues 200 hours on the static load of regulation, coupon is not disrumpent feelings or do not crack.
Stress test adopts the method for stipulating among the ASM2424D among the present invention: the nickel plating of red copper test piece single face, coating towards on curve concave surface, show the state of tension of coating, the concave curvature of coating face represents that the pulling force of coating, test piece do not have tensile stress and show.
The coating that adopts low-stress nickel plating technology provided by the invention to obtain, smooth, be attached on the matrix continuously and outward appearance even, do not have defectives such as visible pin hole, pore, foaming, plethora, hole point.Slight stain and variable color allow.If plating defect can be eliminated after mechanical workout, also can allow.
Adopt Hi-Stren steel nickel layer of the present invention to carry out Performance Detection such as sticking power, solidity to corrosion, thermotolerance and stress, meet above-mentioned standard-required fully, coating does not have foaming, peeling phenomenon, the stress test result does not have tensile stress and shows, solidity to corrosion adopts neutral salt spray test, and the white corrosion point does not all appear in the test piece surface.Disrumpent feelings and seminess does not all appear in the hydrogen embrittlement test coupon.
The key problem in technology of the required breakthrough of this technology is that coating should not have tensile stress; The coating that this technology obtained continues 200 hours according to the detection of hydrogen embrittlement test of regulation among the ASTM F 519 on the static load of regulation simultaneously, and coupon is not disrumpent feelings or do not crack.
The technology of the present invention is applied to subcontract in the production process of part, and is respond well, and performance, state are highly stable, satisfies the technical requirements of low-stress deposition nickel layer, and this technology can also be promoted towards the same industry, popularize simultaneously.
In the interior coating protection of the low-stress deposition technology of parts such as warplane and civil aircraft, is once great promotion for low-alloy high-strength piece surface guard technology with process application of the present invention, has considerable economic and good social benefit.
This technological operation is simple, is easy to safeguard high efficiency.Environmental pollution is little, and sewage disposal is simple.Can in the protective treatment of aircraft engine Hi-Stren steel part, be used widely, and can promote the use of the protection aspect of Hi-Stren steel parts such as each Aeronautics and Astronautics engine, the product for civilian use and other part.
Description of drawings
Fig. 1 is a ni plating apparatus;
Fig. 2 is used part of embodiment and anchor clamps;
Fig. 3 is that the microcosmic surface pattern (* 1000) of part before and after the nickel preplating is after (b) is pre-activated nickel plating before handling (a).
Embodiment
The material that plates is all selected CF6-80E engine forefan shaft joint nut for use in the present embodiment, only is principle and effect thereof in order to demonstrate the invention, but not is used to limit the present invention.Any person of ordinary skill in the field all can be in the scope of inventive concept and spirit, and the foregoing description is made amendment and changed.Therefore, the scope of the present invention should be as the criterion so that claim is listed.
Embodiment 1
The circle of the ¢ 75 that the steel wire of use ¢ 0.8 is converted into dips in plating bath and checks that tank liquor transparence film 30S does not break.CF6-80E engine forefan shaft joint nut is placed 246 ℃ of following 190min, to remove stress.
In degreasing tank the part after the destressing is carried out the anode oil removing, current density is 3.5A/dm
2, electrolysis time 2min, 60 ℃ of temperature, check to plate piece surface moisture film 20S continuous.Afterwards the part after the oil removing is placed hydrochloric acid 160ml/l, if corrode 0.6min in the etchant solution of fourth 1.5g/l.
Adopt the nickel preplating groove that the part through pre-treatment is carried out nickel preplating, under 24 ℃ (room temperatures), part is placed NiCl
2.6H
23min in the pre-nickel plating solution of O 246.3g/l, HCl 190.7g/l, the 4min of energising plating afterwards, current density is 6.5A/dm
2, part area (containing the anchor clamps area) is 5dm
2
Part after nickel bath is to preplating carries out nickel plating, the composition of nickel plating solution and constituent concentration are: nickel sulfamic acid 286.4g/l, boric acid 45g/l, sodium-chlor 21.61g/l, sodium lauryl sulphate 0.4g/l, adopt the filtering pressurized air of process of cleaning to stir plating bath during nickel plating, pH value is 3.92, and current density is 3A/dm
2, temperature is 60 ℃, time 60min, size of sample: ¢ 13mm * 102mm, sample thickness of coating 1#0.015mm~0.020mm, 2#0.020mm~0.025mm, 3#0.015mm~0.025mm.The temperature of dehydrogenation stove is raised to thermal treatment temp, goes into the dehydrogenation stove immediately after the part after the nickel plating dries up, the dehydrogenation temperature is 246 ℃, time 8h.
Plating back part loads 8843 POUNDS under the endurance testing machine of 3-5 ton load continues 200 hours, does not occur disrumpent feelings or crackle.Adopt hydrogen embrittlement sample 30min fracture under same load of common nickel plating technology processing by this flow process.
Embodiment 2
The circle of the ¢ 75 that the steel wire of use ¢ 0.8 is converted into dips in plating bath and checks that tank liquor transparence film 20S does not break.CF6-80E engine forefan shaft joint nut is placed 246 ℃ of following 180min, to remove stress.
In degreasing tank the part after the destressing is carried out the anode oil removing, current density is 4A/dm
2, electrolysis time 2min, 60 ℃ of temperature, it is continuous to check that material surface moisture film 20S plates in institute. and afterwards the part after the oil removing is placed hydrochloric acid 190ml/l, corrode 0.8min. as if in the etchant solution of fourth 1.0g/l
Adopt the nickel preplating groove that the part through pre-treatment is carried out nickel preplating, under 24 ℃ (room temperatures), part is placed NiCl
2.6H
23.5min in the pre-nickel plating solution of O 242.9g/l, HCl 190.1g/l, the 4.5min of energising plating afterwards, current density is 6A/dm
2, part area (containing the anchor clamps area) is 5dm
2
Part after nickel bath is to preplating carries out nickel plating, and the composition of nickel plating solution and constituent concentration are:
Nickel sulfamic acid 305.3g/l, boric acid 50g/l, sodium-chlor 22.68g/l, sodium lauryl sulphate 0.5g/l adopt the filtering pressurized air of process of cleaning to stir plating bath during nickel plating, pH value is 3.6, and current density is 3A/dm
2, temperature is 60 ℃, time 60min, size of sample: ¢ 13mm * 102mm, sample thickness of coating 1#0.025mm~0.038mm, 2#0.025mm~0.038mm, 3#0.020mm~0.025mm.The temperature of dehydrogenation stove is raised to thermal treatment temp, goes into the dehydrogenation stove immediately after the part after the nickel plating dries up, the dehydrogenation temperature is 246 ℃, time 8h.
Plating back part loads 8843POUNDS under the endurance testing machine of 3-5 ton load continues 200 hours, does not occur disrumpent feelings or crackle.Adopt hydrogen embrittlement sample 50min fracture under same load of common nickel plating technology processing by this flow process.
Embodiment 3
The circle of the ¢ 75 that the steel wire of use ¢ 0.8 is converted into dips in plating bath and checks that tank liquor transparence film 20S does not break.CF6-80E engine forefan shaft joint nut is placed 246 ℃ of following 180min, to remove stress.
In degreasing tank the part after the destressing is carried out the anode oil removing, current density is 4A/dm
2, electrolysis time 2min, 60 ℃ of temperature, check to plate material surface moisture film 20S continuous.Afterwards the part after the oil removing is placed hydrochloric acid 160ml/l, if corrode 0.6min in the etchant solution of fourth 1.8g/l.
Adopt the nickel preplating groove that the part through pre-treatment is carried out nickel preplating, under 24 ℃ (room temperatures), part is placed NiCl
2.6H
23min in the pre-nickel plating solution of O 242.3g/l, HCl 194.9g/l, the 4min of energising plating afterwards, current density is 6.5A/dm
2, part area (containing the anchor clamps area) is 5dm
2
Part after nickel bath is to preplating carries out nickel plating, the composition of nickel plating solution and constituent concentration are: nickel sulfamic acid 285.0g/l, boric acid 43g/l, sodium-chlor 21.44g/l, sodium lauryl sulphate 0.3g/l, adopt the filtering pressurized air of process of cleaning to stir plating bath during nickel plating, pH value is 4, and current density is 3A/dm
2, temperature is 60 ℃, time 60min, size of sample: ¢ 13mm * 102mm, sample thickness of coating 1#0.025mm~0.038mm, 2#0.025mm~0.038mm, 3#0.020mm~0.025mm.The temperature of dehydrogenation stove is raised to thermal treatment temp, goes into the dehydrogenation stove immediately after the part after the nickel plating dries up, the dehydrogenation temperature is 246 ℃, time 8h.
Plating back part loads 8843POUNDS under the endurance testing machine of 3-5 ton load continues 200 hours, does not occur disrumpent feelings or crackle.Adopt hydrogen embrittlement sample 2h fracture under same load of common nickel plating technology processing by this flow process.
Embodiment 4
The circle of the ¢ 75 that the steel wire of use ¢ 0.8 is converted into dips in plating bath and checks that tank liquor transparence film 20S does not break.CF6-80E engine forefan shaft joint nut is placed 246 ℃ of following 190min, to remove stress.
In degreasing tank the part after the destressing is carried out the anode oil removing, current density is 3.5A/dm
2, electrolysis time 2min, 60 ℃ of temperature, check to plate material surface moisture film 20S continuous.Afterwards the part after the oil removing is placed hydrochloric acid 180ml/l, if corrode 0.5min in the etchant solution of fourth 1.6g/l.
Adopt the nickel preplating groove that the part through pre-treatment is carried out nickel preplating, under 24 ℃ (room temperatures), part is placed NiCl
2.6H
23min in the pre-nickel plating solution of O 241.3g/l, HCl 192.4g/l, the 4min of energising plating afterwards, current density is 6.5A/dm
2, part area (containing the anchor clamps area) is 5dm
2
Part after nickel bath is to preplating carries out nickel plating, the composition of nickel plating solution and constituent concentration are: nickel sulfamic acid 284.3g/l, boric acid 40g/l, sodium-chlor 21.32g/l, sodium lauryl sulphate 0.4g/l, adopt the filtering pressurized air of process of cleaning to stir plating bath during nickel plating, pH value is 3.89, and current density is 3.5A/dm
2, temperature is 60 ℃, time 60min, size of sample: ¢ 13mm * 102mm, sample thickness of coating 1#0.015mm~0.020mm, 2#0.020mm~0.025mm, 3#0.015mm~0.025mm.The temperature of dehydrogenation stove is raised to thermal treatment temp, goes into the dehydrogenation stove immediately after the part after the nickel plating dries up, the dehydrogenation temperature is 248 ℃, time 8h.
Plating back part loads 8843 POUNDS under the endurance testing machine of 3-5 ton load continues 200 hours, does not occur disrumpent feelings or crackle.Adopt hydrogen embrittlement sample 1.5h fracture under same load of common nickel plating technology processing by this flow process.
Claims (9)
1. low-stress nickel plating technology is characterized in that these technology concrete steps are:
(a), check plating bath: use the steel wire of ¢ 0.8 to be converted into the circle of ¢ 75, do not break for qualified more than dipping in behind the plating bath transparence film 10S that produces along circumference;
(b), remove preplating part stress: the preplating part is placed 3~4h under 246 ℃ ± 14 ℃ temperature;
(c), anode electrolysis oil removing: the part after the destressing placed except that oil solution carry out the anode electrolysis oil removing, check the continuity of piece surface moisture film in 10-30 of plating, as if then qualified continuously;
The composition and the constituent concentration that wherein remove oil solution are: NaOH 30-70g/l, Na
2CO
330-100g/l, Na
3PO
410-30g/l, Na
2SiO
33-10g/l; The oil removing current density is 3~5A/dm
2, 60~80 ℃ of temperature, time 2~3min;
(d), corrosion: at room temperature, place etchant solution to corrode 0.5-1min the material after the oil removing;
Wherein the composition of etchant solution and constituent concentration are: hydrochloric acid 150-200ml/l, if fourth 1~2g/l;
(e), nickel preplating: at room temperature, the material after the corrosion is placed pre-nickel plating solution 1~4min, galvanization 3~5min in pre-nickel plating solution again, current density is 5~8A/dm
2
Wherein the composition of pre-nickel plating solution and constituent concentration are: NiCl
2.6H
2O 200~250g/l, HCl 180~220g/l;
(f), nickel plating: it is the nickel plating of switching on of the nickel plating solution of 3.5-4.2 that the material behind the nickel preplating is placed PH, and the nickel plating time is 32-210min, and the nickel plating temperature is 40-70 ℃; Cathode current density is 1~4A/dm
2
Wherein the composition of nickel plating solution and constituent concentration are: nickel sulfamic acid 270-330g/l, boric acid 40-60g/l, sodium-chlor 15-30g/l, 0.3g/l≤sodium lauryl sulphate<0.8g/l;
(g), thermal treatment: temperature is 246 ± 14 ℃, and the time is 8h ± 15min.
2. according to the described low-stress nickel plating technology of claim, it is characterized in that the destressing temperature is 246 ℃ in the described step (b), the time is 4h.
3. according to the described low-stress nickel plating technology of claim 1, it is characterized in that the bed thickness of nickel preplating in the step (e) is 2.5 μ m.
4. according to the described low-stress nickel plating technology of claim 1, it is characterized in that the nickel plating temperature is 60 ℃ in the described step (f).
5. according to the described low-stress nickel plating technology of claim 1, it is characterized in that the PH=4 of nickel plating solution in the described step (f).
6. according to the described low-stress nickel plating technology of claim 1, stir plating bath with the filtering pressurized air of the process of cleaning when it is characterized in that in the step (f) nickel plating.
7. according to the described low-stress nickel plating technology of claim 1, it is characterized in that the bed thickness of nickel plating in the step (f) is 0.008mm~0.038mm.
8. according to the described low-stress nickel plating technology of claim 1, it is characterized in that timed interval between step (f) and the step (g) is less than 60min.
9. described according to claim 8, it is characterized in that timed interval between step (f) and the step (g) is less than 30min.
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CN101922032A (en) * | 2010-09-14 | 2010-12-22 | 常德力元新材料有限责任公司 | Method for preparing nickel-coated porous steel strip |
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CN102330133A (en) * | 2011-07-27 | 2012-01-25 | 太仓市金鹿电镀有限公司 | Technology for evenly and continuously plating nickel |
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