CN101275263B - Voltage step micro-arc oxidation method - Google Patents
Voltage step micro-arc oxidation method Download PDFInfo
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- CN101275263B CN101275263B CN2007100326650A CN200710032665A CN101275263B CN 101275263 B CN101275263 B CN 101275263B CN 2007100326650 A CN2007100326650 A CN 2007100326650A CN 200710032665 A CN200710032665 A CN 200710032665A CN 101275263 B CN101275263 B CN 101275263B
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Abstract
The invention discloses a voltage step micro-arc oxidation method: after surface preprocessed part and a counter electrode are respectively connected with output ports of a power source and then are steeped into a micro-plasma oxidation electrolyte, a low voltage delta U<int> is used as start voltage and applied, afterward the voltage is increased in a step way, when reaching the peak value delta<p>, the voltage is maintained, until a total process time t<T> is finished. The method of the invention not only can effectively weak the impact to the power system caused by a current pulse which isproduced at the instant when the voltage-control micro-plasma oxidation is started, obviously decrease the request to the nominal parameter of the micro-arc oxidation power source, and save the manufacture/procurement cost of the micro-arc oxidation power source, but also can improve the electric efficiency and reduce the thermal losses. Moreover, when the micro-arc oxidation method provided by the invention is used, the membrane effect can be also obviously improved, and obtains a smoother, evener and more compact ceramic membrane can be obtained.
Description
Technical field
The invention belongs to field of surface engineering technique, particularly a kind of voltage step micro-arc oxidation method.
Background technology
As a kind of material surface modifying technology, differential arc oxidation has following outstanding advantage: one, organic original position that can realize metal and stupalith is compound, keep both to realize the potteryization of metallic surface separately under the prerequisite of characteristic property advantage, can effectively overcome defectives such as stupalith fragility by the conventional sintering prepared is big, easy fracture, workability difference simultaneously.Its two, film forming ability is strong, and pre-treatment is not had strict demand, can handle the workpiece of complex geometry, potteryization can both be realized in every surface that can contact with electrolytic solution.Its three, by to parameters Optimization, can realize regulation and control to ceramic membrane composition, structure and performance index, obtain that corrosion-resistant, wear-resistant, bonding force is strong, insulation, surface reforming layer attractive in appearance.Four, operation is simple, and appointed condition does not have particular requirement, easily realizes mass, uninterrupted production.Its five, by to the strictness of electrolyte component control, can realize truly " cleaner production ".
Because above-mentioned technical superiority, differential arc oxidation receives the unprecedented concern of academia and business circles as most economical, the most effective a kind of in Mg, Al, Ti etc. " valve metal (valve metals) " and the many surface strengthening technologies of alloy thereof.Under numerous at home and abroad scholars, expert's the unremitting effort, differential arc oxidation fundamental research and application and development make significant progress, and use in industrial realization mass-producing.However, existing differential arc oxidization technique still exists defective and deficiency, and outstanding behaviours is that efficient is low, energy consumption big, comprehensive cost (especially power supply cost) is high.At " electroplating and finish " 1998 the 20th volume the 3rd phase 1-4 pages or leaves, deliver the article that is entitled as " aluminium differential arc oxidation current efficiency examination " as people such as Xue Wenbin, reported that aluminium differential arc oxidation current efficiency only is the result of study of 10-30%.People such as Xue Wenbin " metal heat treatmet " calendar year 2001 the 1st phase 1-3 page or leaf deliver the article that is entitled as " non-ferrous metal surface by micro-arc oxidation technology review ", point out high-voltage and a large amount of electric energy of high current density consumption that differential arc oxidation uses, limited the working (finishing) area of single workpiece.Above-mentioned defective and deficiency have become one of main bottleneck of applying of restriction differential arc oxidization technique.
Differential arc oxidation is the surface reaction process of an electrode and electrolytic solution fellowship " stage " feature distinctness, is a strong polarization process of electrochemistry.Polarization condition must influence process of growth (comprising growth velocity and capacity usage ratio) and component, structure and the performance of ceramic membrane, and polarization condition the place one's entire reliance upon kind (comprising waveform, amplitude, frequency and dutycycle etc.) and the output control mode of power supply output electrical parameter.Therefore, under the prerequisite that other parameter remains unchanged, the control of the selection of electrical parameter kind and the way of output (counter electrode is the mode that applies of electrical parameter) becomes most important.
Up to now,, realize strengthening the R﹠D work of differential arc oxidation treatment effect target, obtained a large amount of achievement/results by improving electric power outputting current/voltage, optimizing parameters such as output waveform, frequency and/or dutycycle.Yet, problem that a series of costs that directly cause for above-mentioned approach (especially improving the approach of outward current/voltage) increase and the negative impact that brings thereof, rarely seen concern.The differential arc oxidation suite of equipment is made up of power supply, electrolyzer, washing bath, whipping appts, cooling back installation and drying installation etc. usually.Power supply conduct core wherein, its cost occupies quite great proportion in the equipment total cost.Raising is to the requirement of power supply output parameter such as voltage, electric current and frequency etc., and the manufacturing cost and the procurement price of power supply are unprecedented soaring with making.On the other hand, because thermal losses and a series of side reaction, the operating method of high-voltage, strong current must be brought bigger power loss.The direct result that thermal losses brings is to cause electrolyte temperature to raise.Too high solution temperature both can have a negative impact to the process of growth of ceramic membrane, can increase the weight of the vaporization losses of electrolytic solution again, therefore, must force cooling to electrolytic solution, and this must increase the weight of the load and the corresponding cost of cooling back installation.In sum, preferred and control to the electrical parameter kind, though be the effective way that strengthens the differential arc oxidation treatment effect, can't solve problems such as exist in the differential arc oxidization technique expensive, high energy consumption and poor efficiency, even make the problems referred to above more outstanding to a certain extent.
For these reasons, electrical parameter applies mode causes the part scholar to the influence of differential arc oxidation film-formation result concern.Characteristics according to the differential arc oxidation process, carry out preferred and control to the process that applies of electrical parameter, not only can utilize existing installation and technology, when improving utilization rate of electrical, reducing thermal losses, obtain high-quality ceramic coating formed by micro-arc oxidation, and can reduce requirement to the equipment and technology parameter, save the manufacturing and/or the purchase cost of new installation.With regard to the mode that applies of electrical parameter, what research and practical application were maximum is control stream method and pressure control method.With the pressure control method is example, and existing method can be divided into two classes.The first kind is: from 0V, with certain speed booster tension to preset value.This class control method is used for determining of differential arc oxidation process U-I relation more.As people such as Dittrich K H at " Crystal Res﹠amp; Technol " in the article that is entitled as " Structure and Properties of ANOF Layers " delivered of 1984 years 19 volume the 1st phase 93-99 pages or leaves; and people such as Zhao Shuping is in the research paper that is entitled as " relation of electric current, acoustical signal and optical signal and coating formation voltage during differential arc oxidation " that " material protection " 2006 the 39th volumes the 2nd phase 70-71 page or leaf is delivered, and used voltage control method is so.These class methods help the investigator to understand the overall picture of U-I relation, have critical role in applied basic research.But these class methods also are not suitable for production practice, because there is following major defect in it: the first, in some differential arc oxidation electrolytic solution, electrode suffers corrosion failure because of forming protective membrane fast in process of anodic polarization; The second, oxidization time is long, and processing efficiency is low excessively, and this is for producing particularly streamline operration and automatic production line, significant adverse in batches.
At the major defect of first kind pressure control method, have the scholar to propose the second class pressure control method: it is rate of pressure rise that moment is pressurized to the required voltage value
Keep constant voltage then.The article of delivering at " Acta Physica Sinica " 2005 the 54th volume the 4th phase 1697-1701 page or leaf as people such as Wu Hanhua that is entitled as " characteristic research of electricity parameter in the aluminum alloy differential arc oxidation process " is wherein to being described as of used pressure method " ... just operating voltage can be added to required value when differential arc oxidation begins ".People such as Li Wei deliver the article that is entitled as " anode voltage is to the influence of medical titanium material differential arc oxidation " at " Special Processes of Metal Castings and non-ferrous alloy " 2007 the 27th volumes the 2nd phase 97-100 page or leaf, and people such as Jiang Bailing delivers the article that is entitled as " electrical parameter is to the influence of titanium alloy differential arc oxidation bioactive ceramic layer calcium phosphorus composition " at " China YouSe Acta Metallurgica Sinica " 2005 the 15th volumes the 2nd phase 264-269 page or leaf, people such as Huangping deliver the article that is entitled as " the porous titanium oxide film and the bioactivation mechanism thereof that are rich in calcium phosphorus " at " silicate journal " 2004 the 32nd volumes the 12nd phase 1449-1454 page or leaf, and wherein used step-up method is all so.
Undoubtedly, the above-mentioned second class pressure control method has overcome the defective of first kind pressure control method, has higher utility.But then, also there is the drawback that threatens power supply service life and stability under working conditions thereof in this class pressure control method.In the differential arc oxidation process, relative power supply, the electrode system that electrode (comprising working electrode that is made of the pre-treatment part and the counter electrode that is made of pre-treatment part or inert material) and electrolytic solution are formed constitutes variable load, the resistivity of its resistance and electrode materials, geometrical shape and size, and the parameters such as impedance of the existing rete of electrode surface are relevant.For the electrode that the surface does not form the protective membrane with higher resistance value as yet; because the solution resistance generally very little (ohm level) of differential arc oxidation electrolytic solution; therefore; if with bigger magnitude of voltage trigger voltage loading procedure; certainly will cause current break, this sudden change is particularly evident to broad-area electrode.The sudden change of electric current will cause serious impact for some components and parts such as the thyristor and the IGBT etc. of power supply, causes it to burn because of overheated or overcurrent, and finally influences the normal operation of power unit and whole differential arc oxidation system.
At the drawback of the second class pressure control method, the professional angle of different scholars from being good at separately proposed different solutions.Rolled up the 4th phase 6-10 page or leaf as people such as Chen Kexuan in 2007 the 10th in " power technology application ", deliver the article that is entitled as " the magnesium alloy differential arc oxidation process is analyzed and the primary source design ", propose: be the damage of avoiding the differential arc oxidation starting stage may cause the Primary Component of power supply because of current break, carry out surface preparation with the low pressure special power supply that can bear big electric current earlier, behind the very thin oxide film of one deck to be generated, use the differential arc oxidation primary source again instead and carry out differential arc oxidation and handle.People such as Zhang Wei mention in Chinese invention patent " a kind of method at Mg alloy surface positive and negative bipolarities micro arc electrodepositing ceramic layer " (ZL 03157173.5), the control method of used electrical parameter is " output voltage of the power supply that constantly raises is kept lasting micro-arc discharge ".People such as Gong Weiwei deliver the article that is entitled as " research of magnesium alloy plasma micro-arc oxidising process control " at " material heat treatment journal " 2005 the 26th volumes the 1st phase 77-80 page or leaf, the voltage control method that " gradual " progressively pressurizes has been proposed, promptly " adopt the initial voltage of 300V; when the sample anodes electric current drops to 3A; " with the anode voltage 20V that raises, until required voltage.Its result of study shows: compare with the mode that directly adds high pressure, novel method is little to the total thickness influence of film, but can improve the ratio of tight zone and tectorium, obtains the rete that character is even more, performance is excellent more.
The solution that people such as Chen Kexuan propose has novelty and practicality undoubtedly, but because its realization approach depends on the uses of two cover independent electric power supplies, and the current design capacity of special power supply must enough greatly just can meet the demands, and has therefore increased equipment cost.People's such as Zhang Wei invention is quite creative at aspect such as save energy and reduce the cost, raise the efficiency, but wherein the description of pressure control method is only had in a nutshell, and concrete ins and outs are unknown.The pressurization that people such as Gong Weiwei are used since with the anodic current value as the judgment criteria of whether boosting, this has bigger limitation for the changeable actual application background of electrode size.On the other hand, they do not mention selection foundation and concrete boosting mode and speed to initial voltage.
Summary of the invention
The objective of the invention is to provides a kind of voltage step micro-arc oxidation method at problems such as " expensive, high energy consumption, poor efficiency " that exist in the existing differential arc oxidization technique.
The present invention is achieved by the following technical programs: a kind of voltage step micro-arc oxidation method: will be connected the back respectively with the output port of power supply with counter electrode through the pre-treatment part of surface dressing and immerse in the differential arc oxidation electrolytic solution, with low pressure Δ U
IniTrigger voltage applies, subsequently with step mode booster tension, when voltage reaches peak delta U
PAfter keep this voltage, up to overall treatment time t
TFinish.
Described low pressure Δ U
IniValue be striking voltage Δ U
0-30 (V) are to striking voltage Δ U
0+ 100 (V).
The mean rate of described voltage step
Value is 0.5-50V/min, and identical or different in the different periods of same differential arc oxidation process.
The cycle Δ T value of described voltage step is 0.1sec-30min, and identical or different in the different periods of same differential arc oxidation process.
Described crest voltage Δ U
PValue be striking voltage Δ U
0+ 50 (V) are to striking voltage Δ U
0+ 600 (V).
Described differential arc oxidation total time t
TValue be 1min-2h.
Said among the present invention " striking voltage " is meant that the pairing bath voltage of the differential of the arc/spark appears in electrode surface, and its value is relevant with the composition of electrode system and the kind of electrical parameter etc.
Compared with prior art, owing to utilize the control skill of " low voltage starting " and " step is boosted ", the present invention has following advantage:
One, saves equipment cost.Utilize method provided by the invention, can significantly reduce requirement, save the manufacturing/purchase cost of mao power source the mao power source nominal parameter.
Two, energy-saving and cost-reducing.Utilize method provided by the invention to carry out differential arc oxidation and handle, can improve utilization rate of electrical, reduce thermal losses, alleviate the load of cooling system simultaneously.This is significant for control industrial production cost.
Three, improve the processing quality.Utilize method provided by the invention to carry out differential arc oxidation and handle, can significantly improve film-formation result, obtain more smooth, more even, finer and close ceramic membrane.
The present invention has important guiding value for the foundation and the operation of valve metal especially magnesium, aluminium, titanium and test of alloy product differential arc oxidation and production line.
Description of drawings
Fig. 1 is a differential arc oxidation voltage step process synoptic diagram of the present invention.
Wherein: t
N0It is the initial moment of the step platform of the n time voltage step correspondence.
t
N1It is the termination moment of the step platform of the n time voltage step correspondence.
t
N2It is the termination moment of the n time voltage step.
t
StepBe the total time of voltage step.
t
TFor applying voltage from startup to the total time that finishes to apply voltage.
Δ U
IniBe trigger voltage.
Δ U
N0It is the step platform voltage of the n time voltage step correspondence.
Δ U
N2It is the final voltage of the n time voltage step correspondence.
Δ U
PBe crest voltage.
Δ t
n=t
N1-t
N0Be the voltage step berm width.
Δ T
n=t
N2-t
N0Be the voltage step cycle.
υ=(Δ U
N2-Δ U
N0)/(t
N2-t
N1) be the voltage step absolute speed.
Embodiment
Below in conjunction with drawings and Examples the specific embodiment of the present invention is described in detail.
As shown in Figure 1, be differential arc oxidation voltage step process synoptic diagram of the present invention.Principal feature of the present invention is " low voltage starting " and " step is boosted ", and its process is as follows: to the pre-treatment part polish, surface dressing such as polishing, degreasing; The pre-treatment part is connected with the output port of power supply respectively with counter electrode, immerses in the differential arc oxidation electrolytic solution; Opening power is with Δ U
IniTrigger voltage applies, and applies voltage to electrolyzer, subsequently, and according to voltage step parameter such as voltage step berm width Δ t
n, step cycle Δ T
nAnd average step speed
Value condition, the control process of boosting is until total step time t
StepFinish; Afterwards, keep the differential arc oxidation voltage levvl at crest voltage Δ U
PAs total treatment time t
TDuring end, end voltage applies, and takes out workpiece, washes, aftertreatment such as drying.
With working area respectively is 10cm
2Two AZ91D magnesium alloy samples from coarse to finely polish to 1000 successively
#Silicon carbide paper is successively used hot blast drying after tap water, distilled water and the dehydrated alcohol rinsing.Be connected the back respectively with lead and immerse in the 10g/L sodium metaaluminate group water solution of 1000ml, it is that the AC power supplies of 600V, rated output 6kW carries out differential arc oxidation according to following parameter request and handles under frequency 50Hz condition that room temperature (30 ± 2 ℃) adopts voltage rating down: with Δ U
Ini=200V startup applies voltage, with
Δ T
n≈ Δ t
n=4min, Δ U
P=300V carries out step respectively and boosts overall treatment time t
T=60min.Differential arc oxidation finishes the back deenergization, takes out sample, respectively with tap water and distilled water rinsing, hot blast drying.
Find to start the up-to-date style table and promptly produce the differential of the arc, rise with voltage step, differential of the arc severe degree increases.The differential of the arc is in small, broken bits all the time, even, intensive in whole process.The gained ceramic membrane is silver gray, and is very even, very smooth.
Embodiment 2
Remove Δ U
Ini=80V,
Δ T
n≈ Δ t
n=1min, Δ U
P=200V, t
TOutside=the 15min, other is with embodiment 1.
Finding to start the up-to-date style table does not have obvious spark, rises with voltage step, and spark produces gradually, begins to be cool colour, and severe degree is cumulative subsequently, and the differential of the arc is in small, broken bits, even, intensive during end.The colourless near-transparent of gained ceramic membrane, very even, very smooth.
Embodiment 3
Remove Δ U
Ini=200V,
Δ T
n≈ Δ t
n=10min, Δ U
P=250V, t
TOutside=the 120min, other is with embodiment 1.
Gained phenomenon and result and embodiment 1 are described similar.
Embodiment 4
Remove Δ U
Ini=200V,
Δ T
n≈ Δ t
n=0.1sec, Δ U
P=300V, t
TOutside=the 3min, other is with embodiment 1.
Gained phenomenon and result and embodiment 1 are described similar.
Embodiment 5
Remove Δ U
Ini=100V,
Δ T
n≈ Δ t
n=4min, Δ U
P=500V, t
TOutside=the 110min, other is with embodiment 1.
Gained phenomenon and result and embodiment 1 are described similar, but the rete roughness has increase slightly.
Embodiment 6
At first with Δ U
Ini=200V,
Δ T
n≈ Δ t
n=5min differential arc oxidation is handled 27min, and ordering parameter is subsequently
Δ T
n≈ Δ t
n=1min, Δ U
P=300V handles 13min.Other is with embodiment 1.
Gained phenomenon and result and embodiment 1 are described similar.
Comparative Examples 1
Remove Δ U
Ini=200V,
Δ T
n≈ Δ t
n→ 0, Δ U
P=300V boosts to outside the 300V after promptly starting with 200V immediately fast, and other is with embodiment 1.
The result shows that though it is in small, broken bits, even, intensive to start the differential of the arc of moment generation, with the voltage fast rise, the micro-arc discharge degree sharply increases, and the situation of differential of the arc unstability (sample integral body is by violent fireball parcel), solution boiling, electric current upper punch occurs.Be forced to after 1 minute 30 seconds stop.The gained ceramic membrane is canescence, and is inhomogeneous, coarse, and big area sintering trace is arranged.
Comparative Examples 2
Removing the differential arc oxidation parameter adjustment is Δ U
IniOutside 〉=the 350V, other is with embodiment 1.
The result shows, as Δ U
IniValue 350V and above when respectively being worth, apply voltage after because the immediate current pulse that produces surpasses the power supply nominal parameter, the power protection module is cut off voltage output automatically, the differential arc oxidation process does not begin promptly to be forced to stop as yet.
Claims (8)
1. a voltage step micro-arc oxidation method is characterized in that: will be connected the back respectively with the output port of power supply with counter electrode through the pre-treatment part of surface dressing and immerse in the differential arc oxidation electrolytic solution, with low pressure Δ U
IniTrigger voltage applies, subsequently with voltage step mode booster tension, when voltage reaches peak delta U
PAfter keep this voltage, up to overall treatment time t
TFinish.
2. voltage step micro-arc oxidation method according to claim 1 is characterized in that: described low pressure Δ U
IniValue be striking voltage Δ U
0-30V is to striking voltage Δ U
0+ 100V.
3. voltage step micro-arc oxidation method according to claim 1 is characterized in that: the mean rate υ value of described voltage step is 0.5-50V/min.
4. voltage step micro-arc oxidation method according to claim 3 is characterized in that: the mean rate υ value of described voltage step is identical or different in the different periods of same differential arc oxidation process.
5. voltage step micro-arc oxidation method according to claim 1 is characterized in that: the cycle Δ T value of described voltage step is 0.1sec-10min.
6. voltage step micro-arc oxidation method according to claim 5 is characterized in that: the cycle Δ T value of described voltage step is identical or different in the different periods of same differential arc oxidation process.
7. voltage step micro-arc oxidation method according to claim 1 is characterized in that: described crest voltage Δ U
PValue be striking voltage Δ U
0+ 50V is to striking voltage Δ U
0+ 600V.
8. voltage step micro-arc oxidation method according to claim 1 is characterized in that: described differential arc oxidation overall treatment time t
TValue be 3min-2h.
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| CN102212857A (en) * | 2010-04-01 | 2011-10-12 | 上海禹锦半导体科技有限公司 | Anodic oxidation process for semiconductor device |
| CN102061501B (en) * | 2010-12-31 | 2014-03-05 | 中国船舶重工集团公司第七0七研究所 | Inductosyn hard oxidation technology and power supply device |
| CN102212860B (en) * | 2011-05-18 | 2013-02-13 | 西安理工大学 | Method for controlling micro-arc oxidation electricity parameters under peak current output mode |
| EP3719181A3 (en) | 2019-04-05 | 2020-11-18 | Eloxalwerk Ludwigsburg Helmut Zerrer GmbH | Oxide layer and method of forming a thermally relaxed oxide layer |
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| US6027629A (en) * | 1994-11-16 | 2000-02-22 | Kabushiki Kaisha Kobe Seiko Sho | Vacuum chamber made of aluminum or its alloys, and surface treatment and material for the vacuum chamber |
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