CN1271249C - Supersonic-electrochemical deposition method for nano metal ceramics - Google Patents
Supersonic-electrochemical deposition method for nano metal ceramics Download PDFInfo
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- CN1271249C CN1271249C CN 200410003068 CN200410003068A CN1271249C CN 1271249 C CN1271249 C CN 1271249C CN 200410003068 CN200410003068 CN 200410003068 CN 200410003068 A CN200410003068 A CN 200410003068A CN 1271249 C CN1271249 C CN 1271249C
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Abstract
The present invention belongs to an electrochemical treatment method and application thereof, particularly relates to an ultrasonic electrodeposition method for nanometer level metal ceramics. The present invention is characterized in that the ultrasonic electrodeposition processes is composed of the following technologic procedures: (1) pretreatment of nanometer level metal compounds; (2) electroplating solution preparation; (3)preparation of nanometer metal mixed solutions and electroplating solutions; (4)an ultrasonic electrodeposition technologic process; (5)pretreatment and aftertreatment of electroplating pieces. Nanometer granular material applied by the present invention is one of TiN, TiC, SiN, SiC and Al2O3, or a composition composed of more than one of TiN, TiC, SiN, SiC and Al2O3. An auxiliary electrode used in the ultrasonic electrodeposition process is a Ni plate electrode or a ni profile modeling electrode, and the interelectrode distance is from 20 to 100mm. The nanometer level functional film layer formed in the ultrasonic electrodeposition process has tight structure, good intensity, good toughness and firm combination with basal body. The rockwell hardness can reach more than HRC60, so the film layer is suitable for the surface peening of industrial part and subassembly or repair operation of wear part.
Description
Technical field
The invention belongs to electrochemical process for treating and application thereof, relate in particular to the ultrasonic-electro-deposition method of nano level metal pottery.
Background technology
At present, the main method that is used to prepare the nanometer metal ceramic matrix material is a high-energy ball milling method, i.e. MA method and direct precipitation method.MA method technology is fairly simple, and the preparation efficiency height is easily introduced impurity but exist in the preparation, and purity is not high, the unequal shortcoming of size distribution.Electrodip process is one of high efficiency method of the generation nano level rete that occurs in recent years, compares with additive method, possesses to be widely used, and equipment is simple, and cost is low, the efficient height, and technology is flexible, is easy to control, is convenient to by testing laboratory to advantages such as the on-the-spot transfers of technology.But the nano material that generates with electrodip process mainly is nano metal (alloy) crystal and amorphous film, the thickness＜300nm of settled layer.Its achievement still is in the laboratory study stage, does not see the reported in literature of relevant galvanic deposit and ultrasonic-galvanic deposit nano level metal Ceramic Composite rete.Ultrasonic technology is the utilisation technology of a comparative maturity, just begins in recent years to be applied in the preparation of nano material and nanometer film.Giving full play to the characteristics of ultrasonic wave and two kinds of technology of galvanic deposit, and the two is organically combined, be applied in the new technology that steel metal parts surface generates the nanometer metal ceramic functional film layer, then is the target that the contriver pursued.
Summary of the invention
The objective of the invention is to propose a kind of employing pulsed current and ultrasonic wave turbulent compound action, form the processing method of nanometer metal ceramic functional film layer on the surface of steel metal parts.The used major equipment of ultrasonic-electro-deposition method that the present invention proposes is suitable coating bath, the pulse power and supply line thereof, ultrasonic wave generation systems and transmission channel thereof and the weak corrosion and the vapour hot water cleaning system that carry out the steel components surface.The technological process of galvanic deposit is at first tackled the nano level metal compound and is anticipated.The nano level metal compound that the present invention uses mainly comprises titanium nitride TiN, titanium carbide TiC, silicon nitride SiN, silicon carbide SiC and aluminium sesquioxide Al
2O
3Deng nano particle.Can select wherein one or more arbitrary composition according to the needs of composite film.Before the electroplate liquid preparation, nano particle is bought from market, should at first clean and dispersion treatment, disperses intact nanoparticle directly to add in the electroplate liquid.
The electroplate liquid that this law adopts needs prepared beforehand, and the composition of electroplate liquid is as follows:
Single nickel salt NiSO
45～12g/L
Sulfuric acid H
2SO
410～50ml/L
Additive PPM 0.5～5g/L
Nano metal particles 0.2～10g/L
20～40 ℃ of temperature
PH value 1～6
Supporting electrode Ni plate or Ni profiling electrode
Interpole gap 20～100mm
The electroplate liquid that finishes of preparation preferably carries out electrolysis treatment, handles after 8 hours, leaves standstill 12 hours, and filtering again adds the nanoparticle of specified amount then, becomes muddy liquid, adds water to specified amount subsequently.Secondly, get the part of desiring to cover and plate pre-treatment, inorganic solvent or chemical solution are removed greasy dirt, carry out the weak corrosion of hydrochloric acid soln and clean completely.Under the charged situation of tank liquor, get plating piece and put into coating bath, configure supporting electrode, import pulsed current and ultrasonic wave, begin ultrasonic-electrodeposition process.The parameter of the pulse power is:
Pulse voltage amplitude 3～15V
Current density amplitude 5～60A/dm
2
Pulse width 1～200ms
Pulse interval 1～1000ms
Pulse duty factor 1～1/10
Pulse-repetition 100～2000Hz
The pulse waveform rectangle
Power up time 10～60min
Hyperacoustic parameter is:
Wave direction X, Y, X+Y
Power 0～300W
Frequency 18～50KHz
Time 10～100min
The aftertreatment of plating piece mainly comprises operations such as hot water cleaning, flowing water cleaning.
Provided by the invention ultrasonic-electro-deposition method is simple, cost is low, the thickness of complex function rete 10～100 μ m, wear resistance is good, the repair that is particularly useful for the surface strengthening of mechanical component or takes place because of wearing and tearing.
[case study on implementation]
Ultrasonic-the galvanic deposit of the composite film of embodiment 1 Compressor Rotor axle journal.
Compressor Rotor shaft neck Ф 100 * 200mm because of wearing and tearing are keeped in repair, needs plating nanometer metal ceramic (TiC+TiN) 0.08mm, the technological specification that proposes by this law deposits 8 hours in corresponding coating bath after, has obtained good result.After testing, the size of this axle journal has reached Ф 100.11mm, and the surface is visual smooth, the end little rough, and Rockwell hardness is more than HRC60.
The surface Hardening Treatment of embodiment 2 piston compressor valve blocks
Piston gas compressor valve block (external diameter Ф 100mm, internal diameter Ф 80mm, thickness 0.8mm), material is 35CrMo.Need plating nanometer metal ceramic (SiC+SiN) functional film layer thickness to reach 0.02mm, the technological specification that proposes by this law carried out ultrasonic-electrodeposition process after 2 hours in corresponding coating bath, obtain result preferably, after testing, valve block surface hardness HRC65～70, one-sided sintering metal thicknesses of layers 0.02mm, smooth surface, compare with conventional valve block, improve 1.5～2 times work-ing life.
Claims (4)
1, a kind of nanometer metal ceramic ultrasonic-electrochemical deposition method, is that coating bath powers up and introduce ultrasonic wave with the metal parts of desiring plating through inserting after the pre-treatment in the conventional plating tank by the pulse power and ultrasonic generator, between plating piece and anode, form current path, it is characterized in that this ultrasonic-electrodeposition process is made of following steps:
(1) pre-treatment of nano level metal compound
(2) preparation of electroplate liquid
(3) preparation of nano metal mixed solution and electroplate liquid
(4) ultrasonic-electrodeposition technology process
(5) aftertreatment of plating piece.
2, a kind of nanometer metal ceramic according to claim 1 ultrasonic-electrochemical deposition method is characterized in that described nano level metal compound is titanium nitride TiN, titanium carbide TiC, silicon carbide SiC, silicon nitride SiN, aluminium sesquioxide Al
2O
3In a kind of or its composition, commercially available compound should be inserted and be cleaned in the container and dispersion treatment, amount adds in the electroplate liquid of preparation in accordance with regulations then.
3, a kind of nanometer metal ceramic according to claim 1 ultrasonic-electrochemical deposition method is characterized in that described electroplating bath components is:
Single nickel salt NiSO
45～12g/L
Sulfuric acid H
2SO
410～50ml/L
Additive PPM 0.5～5g/L
Nano metal particles 0.2～10g/L
PH value 1～6
20～40 ℃ of temperature
After the electroplate liquid preparation is finished, all should carry out electrolysis treatment usually, handle according to a conventional method and leave standstill filtering after 12 hours after 8 hours, add the nano metal particles mixed solution of specified amount then, add water to specified volume.
4, a kind of nanometer metal ceramic according to claim 3 ultrasonic-electrochemical deposition method, it is characterized in that described ultrasonic-processing parameter of electrochemical deposition process is:
(1) pulsed current:
Pulse voltage amplitude 3～15V
Current density amplitude 5～60A/dm
2
Pulse width 1～200ms
Pulse interval 1～1000ms
Pulse duty factor 1～1/10
Pulse-repetition 100～2000Hz
The pulse waveform rectangle
Power up time 10～60min
(2) ultrasonic wave
Wave direction X, Y, X+Y
Power 0～300W
(3) supporting electrode Ni plate and Ni profiling electrode
(4) interpole gap 20～100mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410003068 CN1271249C (en) | 2004-01-17 | 2004-01-17 | Supersonic-electrochemical deposition method for nano metal ceramics |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410003068 CN1271249C (en) | 2004-01-17 | 2004-01-17 | Supersonic-electrochemical deposition method for nano metal ceramics |
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| CN1557997A CN1557997A (en) | 2004-12-29 |
| CN1271249C true CN1271249C (en) | 2006-08-23 |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100348780C (en) * | 2004-03-16 | 2007-11-14 | 天津大学 | Method of pulse plating nickel based nano composite plating layer and equipment |
| CN1807702B (en) * | 2005-12-19 | 2010-07-21 | 吉林大学 | Process for preparing gradient nano compound coating on powder metallurgy part surface |
| CN102277604B (en) * | 2010-06-10 | 2013-11-27 | 中国科学院金属研究所 | Electroplated Ni stacking membrane and its preparation method |
| CN102002748A (en) * | 2010-12-09 | 2011-04-06 | 大连大学 | Method for preparing ferromagnetic nano composite material with pulse-ultrasound electrodeposition |
| CN102051644B (en) * | 2010-12-27 | 2012-12-19 | 嘉兴市天器新材料科技有限公司 | Nano-structure Ni-base composite electroplating solution containing nano Si3N4 particles and preparation method thereof |
| CN103184457B (en) * | 2011-12-28 | 2015-06-10 | 北京有色金属研究总院 | Surface alloying strengthening method |
| CN104928729A (en) * | 2015-05-14 | 2015-09-23 | 大连大学 | Electrodeposition-laser remelting strengthening process of Ni-nanometer TiN composite layer on surface of nickel base superalloy |
| CN111607816A (en) * | 2020-06-03 | 2020-09-01 | 暨南大学 | Method for pulse electrodeposition of Ni-SiC composite coating on surface of aluminum alloy |
| CN113328111B (en) * | 2021-05-25 | 2023-04-21 | 上海电力大学 | Stainless steel bipolar plate with chromium-based nitride composite coating and preparation method thereof |
| CN114182311B (en) * | 2021-12-17 | 2024-04-12 | 大连大学 | Preparation method of nano nickel-based composite layer added with graphene oxide |
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2004
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