CN109735891A - A method for improving mechanical properties of particle jet electrodeposition composite coating - Google Patents
A method for improving mechanical properties of particle jet electrodeposition composite coating Download PDFInfo
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- CN109735891A CN109735891A CN201811522330.1A CN201811522330A CN109735891A CN 109735891 A CN109735891 A CN 109735891A CN 201811522330 A CN201811522330 A CN 201811522330A CN 109735891 A CN109735891 A CN 109735891A
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- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000002131 composite material Substances 0.000 title claims abstract description 25
- 238000000576 coating method Methods 0.000 title claims abstract description 24
- 238000004070 electrodeposition Methods 0.000 title claims description 25
- 239000011248 coating agent Substances 0.000 title claims description 20
- 239000002245 particle Substances 0.000 title claims description 16
- 239000002105 nanoparticle Substances 0.000 claims abstract description 54
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000004202 carbamide Substances 0.000 claims abstract description 36
- 230000000694 effects Effects 0.000 claims abstract description 34
- 239000003792 electrolyte Substances 0.000 claims description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 9
- 238000000151 deposition Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000005238 degreasing Methods 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 5
- 238000010907 mechanical stirring Methods 0.000 claims description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 238000005137 deposition process Methods 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- 238000005054 agglomeration Methods 0.000 claims description 2
- 230000002776 aggregation Effects 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims 2
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims 2
- 238000013386 optimize process Methods 0.000 claims 1
- 238000002203 pretreatment Methods 0.000 claims 1
- 239000000654 additive Substances 0.000 abstract description 11
- 230000000996 additive effect Effects 0.000 abstract description 10
- 239000008151 electrolyte solution Substances 0.000 abstract description 7
- 239000011859 microparticle Substances 0.000 abstract description 5
- 230000005012 migration Effects 0.000 abstract description 4
- 238000013508 migration Methods 0.000 abstract description 4
- 230000002787 reinforcement Effects 0.000 abstract description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 22
- 235000013339 cereals Nutrition 0.000 description 11
- 230000009471 action Effects 0.000 description 9
- 239000002114 nanocomposite Substances 0.000 description 7
- 238000005498 polishing Methods 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 6
- 239000004615 ingredient Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000013019 agitation Methods 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 3
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 230000002708 enhancing effect Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 229910017767 Cu—Al Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- -1 aluminium oxide compound Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052927 chalcanthite Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
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- 239000007791 liquid phase Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
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- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
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- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
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Abstract
The present invention discloses a kind of method for improving microparticle jetting electrodeposited composite coatings mechanical property, urea additive is added in the electrolytic solution, by being acted on the nano particle of co-deposition, improve the polarity of nanoparticle surface charge, nanoparticle is set self-dispersing tendency occur, weaken reuniting effect, be conducive to cathodic migration, transmitting and be easy to be captured by cathode surface, to improve nano-particles reinforcement amount and uniformity.
Description
Technical field
The present invention relates to a kind of methods for improving microparticle jetting electrodeposited composite coatings mechanical property.
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 substantially such as the single-element of deposition
The metals such as copper, nickel, hardness, tensile strength, creep strength are low, poor for being repaired object performance recovery effects.In order to obtain
High performance reparation is obtained, the mode of composite electrodeposition can be usually taken, i.e., add nanometer reinforcing phase particle in the electrolytic solution,
Such as nano aluminium oxide and silicon-carbide particle, it is co-deposited with metal ion and is being repaired material surface, form nano-composite plate.By
In nano-composite plate include the nano particle haveing excellent performance, therefore generate reparation have good comprehensive performance,
It is remarkably improved the uniformity etc. of coating hardness, wearability, corrosion resistance and deposition.
But, the agglomeration traits of nano particle become current nano-composite plate preparation process problem urgently to be resolved.
Because the nano particle diameter of addition in the electrolytic solution is minimum, 30 rans are typically only, therefore living with high surface
Performance has the tendency reunited together to reduce energy nano particle usually.Therefore two negative effects are caused: first is that
A nanometer aggregate is formd, particle volume is increased, hinders nano particle in the electrolytic solution to cathodic migration, to reduce
Compound quantity of the nano particle in composite deposite in plating solution；It is being plated second is that nanoparticle agglomerates body is unfavorable for compound nano particle
Being uniformly distributed in layer.This weakens the performance that nano particle assigns composite deposite to a certain extent.It is nano combined to solve
This problem of electro-deposition, researcher attempt that many householder methods is taken to weaken nanometer reunion tendency, promote point of nano particle
It dissipates and is uniformly distributed.This mainly includes the modes such as mechanical stirring and supersonic oscillations.Chemical method is in the group for solving nano particle
The other compositions having a negative impact to coating performance have also been introduced while poly-, reduce its comprehensive performance.Physical method
Can effectively dispersing nanoparticles, but since the limitation of technique is also difficult to give full play to during prepared by entire coating
Effect.
Jet stream electro-deposition method is a kind of novel electro-deposition method occurred in recent years, it be mainly characterized by make electrolyte
Under a certain pressure, cathode surface is sprayed at a high speed, therefore there is high mass transfer in liquid phase effect, can be formed in sedimentary tiny
Nanocrystalline structure and high limiting current density.Its distinctive high speed liquid flow is also in Nano-composite Electrodeposition application simultaneously
In play certain stirring action, efficiently avoid the reunion of nano particle.In 101717977 B high rigidity of patent CN
The preparation method and its special equipment of Cu-SiC nano-composite plate propose to be mixed with using the method preparation of jet stream electro-deposition
The electrolyte of SiC nano particle sprays to cathode surface from anode cavities high speed at a high speed under certain pressure effect, accelerates electrolyte
Flowing, strong stirring action is played to the nano particle of electrolyte, efficiently avoids the reunion of nano particle.But this
A little methods only consider merely one side, without combining physics and chemical action effect, play comprehensive function, because
The effect that this is obtained is also than relatively limited.If suitable additive and nano particle are added in electrolyte simultaneously, so that adding
Add agent to act under the action of forced stirring effect of jet stream electro-deposition with nano particle, makes its self-dispersing, nano combined can be obtained
Grain effectively improves the deposition effect for repairing coating coating is higher, composite effect more evenly.Pass through newest patent and document
Retrieval, at present by adding urea additive and nano aluminium oxide in jet stream electrodeposition technology, to improve enhancing in coating
The compound content of grain, and play the role of improving the technical though and scheme appearance not yet of mechanical property.
Summary of the invention
For existing issue, the present invention provides a kind of for improving the side of microparticle jetting electrodeposited composite coatings mechanical property
Method adds urea additive in the electrolytic solution, by acting on the nano particle of co-deposition, improves nanoparticle surface charge
Polarity makes nanoparticle self-dispersing tendency occur, weakens reuniting effect, is conducive to cathodic migration, transmitting and is easy by cathode
Surface trapping, to improve nano-particles reinforcement amount and uniformity.
Step that the specific method is as follows:
1) substrate material surface pretreating process to be repaired: first with 400 mesh abrasive paper for metallograph polishing material surface to be repaired, removal
Its oxide layer, then with the gradual grinding of 800-1200 mesh abrasive paper for metallograph, polishing；By the 35g/L NaOH solution of the material after polishing
It is cleaned, surface degreasing degreasing: and then be activated with 10% concentrated sulfuric acid and 10% nitric acid mixed acid；Distilled water cleaning
Completely, it dries spare；
2) composite electrolyte configures ingredient, and the ingredient of electrolyte includes: cupric sulfate pentahydrate, and the concentrated sulfuric acid, urea, partial size is 35 nanometers
Al2O3；
3) preprocess method of composite electrolyte, first composite electrolyte is stirred by ultrasonic before electro-deposition, then with 1000 revs/min
Clock rate degree mechanical stirring, the reuniting effect for reducing nano particle keep its evenly dispersed, while aoxidize urea molecule and nanometer three
Two alumina particles come into full contact with, and promote the positive charge polarity of nano grain surface；Electrolyte temperature is controlled by water bath with thermostatic control at this time
60 DEG C, to guarantee that urea molecule has preferable activity in this temperature, play its effect；
4) Optimizing Process Parameters used when jet stream electro-deposition: rectangular nozzle 10 × 1mm of bore, nozzle and matrix distance are 5mm,
Using DC current, current density 350A/dm2, electrolyte flow rate 250L/h, 800 layers of the number of plies of scanning, scanning speed
1000mm/ minutes, sedimentation time 30 minutes；
5) in deposition process, the mechanical stirring of ultrasonic agitation and 1000 revs/min is remained, to promote urea molecule and three oxygen
Change two aluminum nanoparticles to come into full contact with, and keeps processing temperature at 55 DEG C.
The basic ingredient concentration of the electrolyte are as follows: cupric sulfate pentahydrate 250-300g/L, concentrated sulfuric acid 50g/L, urea
10g/L, the Al that partial size is 35 nanometers2O3 10g/L。
1) the present invention provides one kind by adding urea additive in the electrolytic solution, by aoxidizing two with the three of co-deposition
Aluminum nanoparticles effect, improves the polarity of nanoparticle surface charge, keeps nano grain surface positively charged, and gradually increase.
Make to form electrostatic repulsion power between nano particle, is produced from dispersion effect, while together with high speed liquid flow action of forced stirring effect
Weaken nanometer reuniting effect.In addition, the positive charge of nano grain surface is conducive to attract capture to by cathode.Therefore add in urea
Under the action of adding agent, nano-particles reinforcement amount and uniformity are greatly improved in composite deposite, and then promote the mechanics of composite deposite
Performance.
2) present invention is the urea and aluminum oxide nanoparticles that certain content is carried by jet electrolytic liquid line, because
This provides specific hydrodynamics field, ultrasonic vibration field and temperature field, makes three energy field superpositions, to promote urea molecule
Under suitable temperature and flow velocity, complex compound is formed with metal cation, is realized in nano grain surface and adheres to, surround, formd
Dispersion effect and adsorption effect to cathode to increase nano-particle content in cathode, and then improve the mechanics of composite deposite
Performance.
Detailed description of the invention
Fig. 1 be electrolyte in urea molecule, metal cation and nano particle interactively figure.
Fig. 2 is jet stream electro-deposition auxiliary device and processing site schematic diagram.
Fig. 3 is the compound content coordinate diagram of nano aluminium oxide in coating under different urea addition contents.
Fig. 4 is the coating microhardness coordinate diagram under different urea addition content.
Fig. 5 is the coating tensile strength coordinate diagram under different urea addition content.
Specific embodiment
The invention belongs to a kind of microparticle jetting electro-deposition to improve technique, i.e., add urea additive in the electrolytic solution, pass through
It is acted on the nano particle of co-deposition, improves the polarity of nanoparticle surface charge, so that nanoparticle self-dispersing tendency is occurred, cut
Weakly agglomerated effect is conducive to cathodic migration, transmitting and is easy to be captured by cathode surface, thus improve nano-particles reinforcement amount and
Uniformity.The core of this method is the urea and aluminum oxide nanoparticles by adding certain content from electrolyte, and
Guarantee specific temperature field and aerodynamic field, so that the two plays following effect: making urea molecule in suitable temperature and High Speed Flow Field
Under, complex compound is formed with metal cation, in nano grain surface attachment, surround, keeps nano grain surface positively charged, and by
It is cumulative to add.Therefore make to form electrostatic repulsion power between nano particle, be produced from dispersion effect, avoid reunion.Nanometer simultaneously
The positive surface charge that particle increases also enhances electronegative cathode to the attraction of nano particle, promotes more nano particles
It is deposited to cathode, to increase nano-particle content in cathode.Its action principle is as shown in Fig. 1.
The invention is realized by the following technical scheme, specific steps are as follows:
1) substrate material surface pretreating process to be repaired:First with 400 mesh abrasive paper for metallograph polishing material surface to be repaired, removal
Its oxide layer, then with the gradual grinding of 800-1200 mesh abrasive paper for metallograph, polishing；Material after polishing is molten with 35g/L NaOH
Liquid is cleaned, surface degreasing degreasing: and then be activated with 10% concentrated sulfuric acid and 10% nitric acid mixed acid；Distilled water
Clean up, dry it is spare.
2) composite electrolyte configures ingredient.The basic ingredient of electrolyte and it is respectively as follows: cupric sulfate pentahydrate with technological parameter
250-300g/L, concentrated sulfuric acid 50g/L, urea 10g/L, the Al that partial size is 35 nanometers2O310g/L.Urea and Al2O3Additive amount
It is the technological parameter of optimization.
3) preprocess method of composite electrolyte.First by composite electrolyte ultrasonic agitation 30 minutes before electro-deposition, then
It is stirred 60 minutes with 1000 revs/min of speed mechanicals, the reuniting effect for reducing nano particle keeps its evenly dispersed, while making urea
Molecule comes into full contact with nano-aluminium oxide particle, promotes the positive charge polarity of nano grain surface.Electrolyte temperature at this time
It is controlled by water bath with thermostatic control at 60 DEG C, to guarantee that urea molecule has preferable activity in this temperature, plays its effect.Itself and nanometer
The mode of action of particle is as shown in Fig. 1.
4) Optimizing Process Parameters used when jet stream electro-deposition: rectangular nozzle 10 × 1mm of bore, nozzle are with matrix distance
5mm, using DC current, current density 350A/dm2, electrolyte flow rate 250L/h, 800 layers of the number of plies of scanning, scanning speed
1000mm/ minutes, sedimentation time 30 minutes.Processing site is as shown in Fig. 2.
5) in deposition process, ultrasonic agitation and 1000 revs/min of mechanical stirring are remained, with promote urea molecule and
Aluminum oxide nanoparticles come into full contact with, and keep processing temperature at 55 DEG C.
Concrete case is as follows:
In test specimen stainless steel plate 1Cr18Ni9Ti having a size of 100mm × 10mm × 1mm, 2 electrodeposition apparatus of attached drawing is used on surface
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 is pure or chemical with analyzing
Pure reagent adds distilled water to be formulated.
3) the mixed urea molecule concentration of electrolyte is 0-20 grams/L.Mixed enhancing particle is nano-aluminium oxide
Grain, 35 nanometers of granularity, purity is greater than 99.99 %.Particle pretreatment is done before processing.First by composite electrolyte ultrasound before electro-deposition
Then stirring 30 minutes is stirred 60 minutes with 1000 revs/min of speed mechanicals.
4) electro-deposition parameter selection is current density 200-500A/dm2, electrolyte flow rate 300L/h.Scan the number of plies 800
Layer, scanning speed 1000mm/ minutes, sedimentation time 30 minutes.
5) XRD diffraction analysis is carried out to post-depositional coating, calculates coating crystallite dimension, compares statistics.It is right simultaneously
Coating carries out Mechanics Performance Testing, including hardness test and draws high strength test.
Test result is as in Figure 3-5:
A certain amount of urea additive and nano aluminium oxide is added in electrolyte, has improvement result to deposition quality, urea is optimal
Addition concentration be 10 grams/L.Specific manifestation after 10 grams/L urea is added, is received according to as can be seen in composite deposite
Rice aluminium oxide compound content highest, formed coating mechanical property it is best, show as hardness and tensile strength relative to
Other addition concentration highests.It is also possible to find 300-400A/dm2Under current density effect, mechanical property is the most prominent.
Therefore, 10 grams/L urea additive amount and 350 A/dm are taken2Strengthen the optimal procedure parameters of scheme for coating performance.
Compared with being currently known method, have the advantage that
1) nano-composite plate that the present invention is prepared has nano-particle content height, nano particle is evenly distributed, hardness is high,
The advantages that crystalline structure is fine and close, surface quality is good.
2) quantitative urea additive is added in jet stream electro-deposition electrolyte, nano particle can be improved significantly multiple
The content and uniformity in coating are closed, action mode is dexterously to reach to subtract by the distribution of charges of influence nano grain surface
The effect of small reunion and cathode adsorption effect is a kind of inherent " soft " property means, and function and effect are more obvious, easy to be easy
Row.
3) urea additive can sufficiently be made under jet stream electro-deposition high speed spray regime with nano alumina particles
With the function and effect for making its reduction nanoparticle agglomerates and enhancing cathode absorption are more significant, to more efficiently improve again
Close the mechanical property of coating.
4) realization high-hardness Cu-Al provided by the invention2O3The special equipment of process for producing nano-composite plate, structure are set
Meter is reasonable, strong operability, high production efficiency.
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