CN105970260B - A method of improving uniformity in jet-electrodeposited method process - Google Patents
A method of improving uniformity in jet-electrodeposited method process Download PDFInfo
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- CN105970260B CN105970260B CN201610260762.4A CN201610260762A CN105970260B CN 105970260 B CN105970260 B CN 105970260B CN 201610260762 A CN201610260762 A CN 201610260762A CN 105970260 B CN105970260 B CN 105970260B
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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
- C25D5/08—Electroplating with moving electrolyte e.g. jet electroplating
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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
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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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
- C25D5/20—Electroplating using ultrasonics, vibrations
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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
- C25D5/22—Electroplating combined with mechanical treatment during the deposition
Abstract
The present invention discloses a kind of method for improving uniformity in jet-electrodeposited method process.The following steps are included: matrix surface pre-processes；Polishing treatment, surface clean, sheet erosion is handled, distilled water cleans up, it is spare to dry；Configure electrolyte；Particle pretreatment；First the particles such as micron order aluminum oxide or silicon carbide and electrolyte are mixed and stirred for 2 hours before electro-deposition, then are stirred by ultrasonic 30 minutes, so that particle is obtained sufficiently wetting, evenly dispersed, micron order aluminum oxide particle additive amount is 10-30 grams per liter；Carry out numerical control program setting；When processing operation, ultrasound wave vibrating bar is directly contacted with electrolyte.It is influenced by particle and changes electrolyte in the electric field redistribution of cathode surface.Crystal grain refinement is promoted by the growth course that particle changes sedimentary crystal grain.Particle generates vibration, rubbing action in electro-deposition.This method can make the leveling performance of deposition surface be improved.
Description
Technical field
The present invention discloses a kind of method for improving uniformity in jet-electrodeposited method process；Belong to advanced Surface Engineering
Technical field.
Background technique
Advanced field of surface engineering technique, electro-deposition techniques be most have application prospect low cost apply layer manufacturing method thereof it
One, have many advantages, such as that simple process, easy to operate, coating type is more, the reparation for thin-walled parts and amount of damage smaller parts
With the incomparable advantage of other technologies (such as built-up welding, laser, spraying).But due to itself there is some inadequate natural endowments
It affects and further uses, Dendritic TiC caused by edge effect is wherein one outstanding.
Edge effect refers to that, in complexity, abnormity shape electro-deposition, field distribution is uneven, the edges such as type face or type hole
The electric field strength that will appear concentration causes deposit local superiority to grow, and coarse grains form dendroid deposit-Dendritic TiC
Even dross etc.；And electric field strength is smaller at center, deposition velocity slows down, and generates even without deposition.Above situation causes
The inhomogeneities of deposition, causes the deposition quality to deteriorate.This is a great problem of electro-deposition processing method encountered.
In order to obtain the sedimentary of crystal grain refinement and surface finishing, existing the relevant technologies include: that (such as machine adds with secondary operation
Work) leveling processing (milling or grinding) is carried out to depositional plane after continue to deposit.The method can guarantee size requirement, the disadvantage is that extending
Production cycle easily causes sedimentary to be layered, and there are hidden danger of quality, and is not suitable for small size or complex parts processing；Using improvement
In electro-deposition concentration polarization and activation polarization and force equilibrium electric field mode (including increase solution conductivity ability, force
Stirring, configuration impressed current anode or auxiliary cathode, adjusting Anode-cathode Distance etc.), such as Nanjing Aero-Space University Zeng Yongbin, Wang Kun
Using electrical-chemistry method auxiliary cathode, anode design based on Ansys；Nanjing Aero-Space University Zhu Zengwei, Wang Guifeng etc. are adopted
Free microballon auxiliary mill technology, grinding jet stream electro-deposition techniques also contribute to improving this problem.The method has become mature at present,
But it is chiefly used in the outer wall processing of revolving body, is related to plane, inner wall, inner hole or irregular type face and is not seen in report then.
In conclusion the method for solving edge effect at present is divided into two kinds, one kind stresses to flatten that (machine adds using mechanical force
Work, abrasive grain grinding aid), another to be improved by changing the method for field distribution, homogenize deposition rate, this needs a large amount of
Empirical data and analog simulation lack versatility.If the damage location structure of part to be repaired is complex, using existing
Electro-deposition method carry out Repair gene have biggish difficulty.Have if energy work in-process facilitates to alleviate the problem online
There is preferable practical value.
Summary of the invention
The present invention provides one kind by adding particle suppression Dendritic TiC undue growth in the electrolytic solution, improves deposition quality
Experimental method.The core of this method is that following effect is played by particle: 1. are influenced by particle and change electrolyte in yin
The electric field of pole surface redistributes；2. promoting 3. particle of crystal grain refinement by the growth course that particle changes sedimentary crystal grain to exist
Vibration, rubbing action are generated in electro-deposition.By making particle play three kinds of effects, the leveling of deposition surface can be made under combined influence
Performance is improved.
The invention is realized by the following technical scheme, specific steps are as follows:
Step 1: matrix surface pretreatment；To obtain preferable binding force and smooth careful coating.
Polishing treatment；
Surface clean: distilled water clean matrix surface, after with acetone soak scouring make oil removal treatment；
Sheet erosion processing；
Distilled water cleans up, it is spare to dry；
Step 2: configuration electrolyte；
Step 3: particle pretreatment；First by the particles such as micron order aluminum oxide or silicon carbide and electrolyte before electro-deposition
Be mixed and stirred for 2 hours, then be stirred by ultrasonic 30 minutes, make particle obtain sufficiently wetting, it is evenly dispersed；
Step 4: setting numerical control program；
Step 5: when processing operation, ultrasound wave vibrating bar directly being contacted with electrolyte.
Rectangular nozzle 10 × 1mm of bore of surface clean in the step 1, nozzle and matrix distance are 2-10mm.
Polishing treatment described in step 1 be first remove its oxide layer with 400 mesh abrasive paper for metallograph polishing matrix surface, then with
800, the grinding of 1000 mesh abrasive paper for metallograph, polishing, it is ensured that matrix surface reaches certain roughness.
The processing of sheet erosion described in step 1 is to place the substrate at 10% dilution heat of sulfuric acid etch passivation in 5 minutes
Reason.
The ingredient of electrolyte and it is respectively as follows: cupric sulfate pentahydrate 250-300g/L, the concentrated sulfuric acid with technological parameter in the step 2
50g/L, 25 DEG C of electrolyte temperature.
Micron order aluminum oxide particle additive amount in the step 3 is 10-30 grams per liter.
The pretreated current density of particle is in 200-500A/dm in the step 32Between, electrolyte flow rate 200-300L/
h。
Particle and dendrite rubbing action a part in electrolyte realize the impact of cathode plate by electrolysis liquid stream.Cathode plate
It can generally place, can also be adjusted according to certain rotation angle, range is between 0-90 degree by natural level.This allows for cathode
When rotation angle adjusts, certain variation can also occur for relative motion situation, the effect of friction between particle and dendrite, therefore need
Find preferable relative position.
The setting numerical control program of the step 4 includes scanning times, scanning distance, Z axis following position (adjusting nozzle to base
The distance of body), injection shuttle-scanning when returning control pump whether stop hydrojet information.
When processing operation in the step 5, ultrasound wave vibrating bar is to be placed in electricity with the contact position that electrolyte directly contacts
It solves in flow container.
When processing operation in the step 5, ultrasound wave vibrating bar is to be fixed on the contact position that electrolyte directly contacts
In the spray chamber of jet stream electrodeposition apparatus.
Ultrasonic wave plays the role of another part with friction to the particle vibration in electrolyte.When processing operation, by ultrasonic wave
Vibrating head is directly contacted with electrolyte, and there are two types of position is available:
1. being placed in electrolyte tank.After starting vibrating head, the ultrasonic wave of generation is transmitted to the electrolyte of surrounding by vibrating head,
On the one hand so that particle is made forced movement accelerates the diffusion of particle to avoid reuniting, another aspect electrolyte recycle stream in conveyance conduit
It moves continuous and is not blocked, ultrasonic wave can be transmitted to along pipeline to cathodic region surface as propagation medium.Impact yin
The electrolyte of pole surface can contain ultrasonic wave, and with Dendritic TiC microcosmic shape can occur for the particle in electrolyte under ultrasonic activation
Dendrite inhibition effect is played in friction under state；
2. being fixed in the spray chamber of jet stream electrodeposition apparatus.Flowing through electrolyte herein will receive the concussion shadow of ultrasonic wave
It rings.Compared to position 1, the distance that ultrasonic wave is transmitted to cathodic region can shorten, and impact the ultrasonic wave that the electrolyte of cathode surface contains
Also there is better vibrating effect relative to position 1.
The present invention, around particle by influencing deposition process in conjunction with multiple means, reaches inhibition branch using particle as core
The purpose of crystals growth, specifically includes:
1) particle itself has nonconducting property, has when impacting on cathode jointly with electrolyte to the distribution of power line
There is the influence of homogenization, redistributes deposition electric field, will not be excessively excessively intensive in edge, weaken edge effect
It answers.See attached drawing 1.
2) particle can change crystal growing process during the deposition process, increase nucleation rate and increase the quantity of nucleus and be unfavorable for
The increase of crystallite dimension, to play the effect of refinement crystal grain.
3) impact of the particle along with electrolyte to crystallizing field can weaken and diffusion layer is inhibited to be formed, and improve effective current
Density promotes crystal grain refinement.
4) particle has friction, removal to act on dendrite under ultrasonic wave and the dual kinetic energy of liquid stream, objectively plays whole
Flat effect.
5) particle not only can inhibit Dendritic TiC, can also be co-deposited with matrix metal in matrix surface, play reinforced phase
Effect, for sedimentary mechanical property have strengthening effect.
Detailed description of the invention
Fig. 1 particle influences the schematic diagram of cathode electric field redistribution.
Fig. 2 jet-electrodeposited method basic structure and configuration ultrasonic device schematic diagram.
The friction and impact of Fig. 3 ultrasonic wave in the electrolytic solution.
Specific embodiment
The present invention provides following specific embodiments: embodiment one: 1) matrix surface pre-processes.To obtain preferable knot
Resultant force and smooth careful coating, need to carry out following pretreatment process: 1. polishing treatment: first with 400 mesh abrasive paper for metallograph polishing base
Body such as stainless steel substrate surface removes its oxide layer, then with the grinding of 800,1000 mesh abrasive paper for metallograph, polishing, it is ensured that matrix surface reaches
To certain roughness；2. surface clean: distilled water cleans matrix surface, after cleaned with acetone soak and make oil removal treatment in about 5 minutes.
3. sheet erosion is handled: stainless steel substrate is placed in 10% 5 minutes Passivation Treatments of dilution heat of sulfuric acid etch；4. distilled water cleans
Completely, it dries spare.
2) electrolyte is configured.The ingredient of electrolyte and it is respectively as follows: cupric sulfate pentahydrate 250-300g/L, dense sulphur with technological parameter
Sour 50g/L, 25 DEG C of electrolyte temperature.
3) particle pre-processes.Because the small high surface activity of diameter of particle is easy to reunite, therefore first by micron order three before electro-deposition
The particles such as Al 2 O or silicon carbide and electrolyte are mixed and stirred for 2 hours, then are stirred by ultrasonic 30 minutes, obtain particle sufficiently
It soaks, is evenly dispersed, micron order aluminum oxide particle additive amount is 10-30 grams per liter.
4) technological parameter: rectangular nozzle 10 × 1mm of bore, nozzle and matrix distance are 2-10mm, and current density is in 200-
500A/dm2Between, electrolyte flow rate 200-300L/h.This section for reference, can incite somebody to action for empirical parameter according to actual condition
Design parameter is adjusted within this range, is selected, as shown in Fig. 2.
Particle and dendrite rubbing action a part in electrolyte realize the impact of cathode plate by electrolysis liquid stream.Cathode plate
It can generally place, can also be adjusted according to certain rotation angle, range is between 0-90 degree by natural level.This allows for cathode
When rotation angle adjusts, certain variation can also occur for relative motion situation, the effect of friction between particle and dendrite, therefore need
Find preferable relative position.
5) numerical control program is set: starting numerical control program, should be servo-actuated position comprising scanning times, scanning distance, Z axis in the program
Whether control pump stops the information such as hydrojet when returning when setting (distance of adjusting nozzle to matrix), injection shuttle-scanning.These letters
Breath is also required to be adjusted acquirement optimal effectiveness according to the actual situation.
6) ultrasonic wave plays the role of another part with friction to the particle vibration in electrolyte.It, will be ultrasonic when processing operation
Wave vibrating head is directly contacted with electrolyte, and there are two types of position is available:
1. being placed in electrolyte tank.After starting vibrating head, the ultrasonic wave of generation is transmitted to the electrolyte of surrounding by vibrating head,
On the one hand so that particle is made forced movement accelerates the diffusion of particle to avoid reuniting, another aspect electrolyte recycle stream in conveyance conduit
It moves continuous and is not blocked, ultrasonic wave can be transmitted to along pipeline to cathodic region surface as propagation medium.Impact yin
The electrolyte of pole surface can contain ultrasonic wave, and with Dendritic TiC microcosmic shape can occur for the particle in electrolyte under ultrasonic activation
Dendrite inhibition effect is played in friction under state；
2. being fixed in the spray chamber of jet stream electrodeposition apparatus.Flowing through electrolyte herein will receive the concussion shadow of ultrasonic wave
It rings.1. compared to position, the distance that ultrasonic wave is transmitted to cathodic region can shorten, and impact the ultrasonic wave that the electrolyte of cathode surface contains
Relative to position 1. also there is better vibrating effect.
It is influenced by particle and changes electrolyte in the electric field redistribution of cathode surface；Deposition layer crystal is changed by particle
The growth course of grain promotes 3. particle of crystal grain refinement and generates vibration, rubbing action in electro-deposition.By making particle play three
Kind acts on, and the leveling performance of deposition surface can be made to be improved under combined influence.
Embodiment two: in test specimen stainless steel plate 1Cr18Ni9Ti having a size of 100mm × 10mm × 1mm, electricity is used on surface
Depositing device processing method prepares copper deposits, and operating procedure is as follows:
1) stainless steel 1Cr18Ni9Ti is surface-treated, successively polishing, oil removing, passivation, washing, drying.
2) electrolyte is configured.The constituent of electrolyte and it is respectively as follows: with technological parameter in present embodiment
CuSO4·5H2O 250g/L, 98% concentrated sulfuric acid 50g/L, electrolyte temperature is 25 DEG C.Electrolyte with analyze it is pure or
Chemically pure reagent adds distilled water to be formulated.
3) the mixed particle of electrolyte is micron aluminum oxide particle, and 10 microns of granularity, purity is greater than 99.99%.Add
Particle pretreatment is done before work.
4) electro-deposition parameter selection is current density 300A/dm2, electrolyte flow rate 300L/h, it is 0 that cathode plate, which rotates angle,
Degree, i.e., it is horizontal positioned.Ultrasound wave vibrating bar is placed in electrolyte tank.Sedimentation time is 120 minutes.Unevenness σ is quoted to retouch
The inhomogeneities of sedimentary is stated,
In formula: hmaxIndicate the maximum value of sedimentary, hminIndicate the minimum value of sedimentary, havIndicate being averaged for sedimentary
Value.
The statistics of sedimentary height value under the different processing conditions of table 1
As seen from the above table, after electrolyte is mixed into particle and ultrasonic vibration is added, unevenness reduces, and has to deposition quality
There is improvement result.
Compared with being currently known method, have the advantage that
1) particle realizes that dendrite inhibition improves by the redistribution of influence electric field and electrocrystallization process in jet stream electro-deposition and sinks
The effect of product Surface flat, this is a kind of mode of " soft " property, does not need complicated equipment and additional process, process costs are low, tool
Have the characteristics that simple and easy to do.
2) particle is combined with jet-electrodeposited method, is had for the surface quality that on-line machining improves sedimentary preferable real
With value.
3) vibration and the friction mode to particle are realized, tentatively to answer from now in the correlation of jet-electrodeposited method manufacture field
With providing related reference.
Claims (7)
1. a kind of method for improving uniformity in jet-electrodeposited method process, which comprises the following steps:
Step 1: matrix surface pretreatment；
Polishing treatment；
Surface clean: distilled water clean matrix surface, after with acetone soak scouring make oil removal treatment；
Sheet erosion processing；
Distilled water cleans up, it is spare to dry；
Step 2: configuration electrolyte；
Step 3: particle pretreatment；First the aluminum oxide particle of 10 micron granularities is mixed and stirred with electrolyte before electro-deposition
Mix 2 hours, then be stirred by ultrasonic 30 minutes, make particle obtain sufficiently wetting, it is evenly dispersed；
Step 4: setting numerical control program；
Step 5: cathode plate can rotation angle adjustment, when cathode rotation angle adjusts, relative motion situation between particle and dendrite,
Certain variation can also occur for the effect of friction, find preferable relative position, when processing is run, by ultrasound wave vibrating bar and electricity
Solution liquid directly contacts, and ultrasound wave vibrating bar is the spray for being fixed on jet stream electrodeposition apparatus with the contact position that electrolyte directly contacts
It is intracavitary；The contact position that ultrasound wave vibrating bar is directly contacted with electrolyte can also be in electrolyte tank.
2. a kind of method for improving uniformity in jet-electrodeposited method process according to claim 1, feature exist
In rectangular nozzle 10 × 1mm of bore of surface clean in the step 1, nozzle and matrix distance are 2-10mm.
3. a kind of method for improving uniformity in jet-electrodeposited method process according to claim 1, feature exist
Be in, polishing treatment described in step 1 first remove its oxide layer with 400 mesh abrasive paper for metallograph polishing matrix surface, then with 800,
The grinding of 1000 mesh abrasive paper for metallograph, polishing.
4. a kind of method for improving uniformity in jet-electrodeposited method process according to claim 1, feature exist
In the processing of sheet erosion described in step 1 is the 5 minutes Passivation Treatments of dilution heat of sulfuric acid etch for placing the substrate in 10%；Distillation
Water cleans up, it is spare to dry.
5. a kind of method for improving uniformity in jet-electrodeposited method process according to claim 1, feature exist
In the ingredient of electrolyte and being respectively as follows: cupric sulfate pentahydrate 250-300g/L, concentrated sulfuric acid 50g/ with technological parameter in the step 2
L, 25 DEG C of electrolyte temperature.
6. a kind of method for improving uniformity in jet-electrodeposited method process according to claim 1, feature exist
In the aluminum oxide particle additive amount in the step 3 is 10-30 grams per liter.
7. a kind of method for improving uniformity in jet-electrodeposited method process according to claim 1, feature exist
In the setting numerical control program of the step 4 returns when including scanning times, scanning distance, Z axis following position, injection shuttle-scanning
Whether control pump stops hydrojet information when returning.
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| DE102005033857A1 (en) * | 2005-07-12 | 2007-01-18 | Siemens Ag | Electrode assembly and method for electroplating a workpiece surface |
| CN101717977B (en) * | 2009-12-08 | 2011-09-14 | 淮海工学院 | Preparation method of high-hardness Cu-SiC nanometer compound plating layer and special device thereof |
| CN103255452B (en) * | 2013-05-03 | 2016-02-24 | 中国人民解放军装甲兵工程学院 | A kind of selective metal electric deposition device and application thereof |
| CN103395008A (en) * | 2013-08-20 | 2013-11-20 | 哈尔滨工业大学 | Abrasive jet machining method under effect of composite energy field |
| PL2871002T3 (en) * | 2013-11-08 | 2016-08-31 | Vln Advanced Tech Inc | Integrated fluidjet system for stripping, prepping and coating a part |
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