CN102439201A - Power supply for anodizing, anodizing method, and anodized film - Google Patents

Power supply for anodizing, anodizing method, and anodized film Download PDF

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CN102439201A
CN102439201A CN2010800203468A CN201080020346A CN102439201A CN 102439201 A CN102439201 A CN 102439201A CN 2010800203468 A CN2010800203468 A CN 2010800203468A CN 201080020346 A CN201080020346 A CN 201080020346A CN 102439201 A CN102439201 A CN 102439201A
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pulse wave
pulse
unit
voltage
modulation
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辛容奉
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KOST CORP
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KOST CORP
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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
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/005—Apparatus specially adapted for electrolytic conversion coating
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/024—Anodisation under pulsed or modulated current or potential

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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Chemical Vapour Deposition (AREA)
  • Plasma Technology (AREA)
  • Formation Of Insulating Films (AREA)

Abstract

An anodizing method for growing an anodized layer on a surface of aluminum in electrolyte is disclosed. The method comprises applying a DC/AC-combined pulse wave between an anode and a cathode. The DC/AC-combined pulse wave is provided by combining a DC pulse wave with an AC wave, and has a peak voltage at a start point of each pulse. The grown anodized layer may be equal to or less than 300[mu]m in thickness, and the diameter of a cell in the anodized layer may range between 50nm and 100nm. The power supply used for anodizing may comprise a rectifying modulator unit, an AC modulating unit, a pulse wave synthesizing unit, and a control unit.

Description

Anodic oxidation power supply, anode oxidation method and anode oxide film
Technical field
Embodiment relates to a kind of anode oxidation method, is used for through the electrochemical process zone of oxidation of on nonferrous metal surface, growing, thereby improves the corrosion resistant performance or the wear resisting property of non-ferrous metal.Particularly, present embodiment relates to a kind of power supply, and it is applicable to provide to have the electrolyzer that comprises direct current (DC) component and the realization anode oxidation process of the pulse wave that exchanges (AC) component.In addition, present embodiment relates to a kind of anode oxidation method of this power supply and anodic oxide coating of growing through this anode oxidation method of using.
Background technology
Such as the non-ferrous metal of aluminium (Al), magnesium (Mg) and titanium (Ti) usually be included in airborne moisture and react with overactivity property, thereby be formed naturally thin oxide layer above that.Yet this natural oxidizing layer is too thin or have too sparse structure, to such an extent as to can not protect the influence of not frayed annular of non-ferrous metal or corrosive environment.Therefore,, preferably make the zone of oxidation of on the surface of non-ferrous metal, growing that ins all sorts of ways, thereby improve the surface property of non-ferrous metal in order to protect non-ferrous metal.The method of zone of oxidation of being used to grow can be divided into chemical process and electrochemical method.Can use chromic salt technology or thin water aluminium technology, with the aluminium surface of chemical treatment as one of non-ferrous metal.This technology can need not electric current is applied to aluminium through chemical technology, comes to form zone of oxidation on the aluminium surface.Yet, when forming zone of oxidation through this chemical surface technology, very thin or the wear resisting property of zone of oxidation with lower-level, and therefore this chemical surface technology is not all suitable for various application.Simultaneously, as the anode oxidation method of one of electrochemical method with sulphuric acid soln as electrolytic solution, and on the aluminium surface, electrochemically form zone of oxidation through electric current being applied to the aluminium surface.Zone of oxidation through the anode oxidation method growth has electricity and chemical property than good quality, and can be used for such as building, machinery, automobile, aircraft and mobile various industry of using.
In traditional anode oxidation method, dc voltage is applied between the electrode, with the surface of oxidation base material electrochemically.That is, oxidized base material is used as pair of electrodes, and dc voltage is applied to the electrode in comprising the electrolyzer of electrolytic solution, thus oxidation substrate surface electrochemically.
Yet according to traditional anode oxidation method, because the reaction between metal and the electrolytic solution, along with the formation of zone of oxidation, metal is simultaneously dissolved, makes that the density of zone of oxidation reduces and the mechanical characteristics deterioration along with the increase of oxidated layer thickness.Therefore, be difficult to grow zone of oxidation above specific thicknesses.In addition, if specific zone of oxidation sticks at the oxidized layer that generates through anode oxidation process with before anode oxidation process between the metal as base material, then the bonding rate between base material and oxidized layer has reduced, and makes zone of oxidation separate from base material easily.
Summary of the invention
Technical problem
Specific embodiment of the present invention provides a kind of power supply of anode oxidation process; And provide and have the anodic oxide coating that increases thickness; It has than the better machinery of other anodic oxide coatings that form through traditional method, electricity and chemical property, and a kind of anode oxidation method and a kind of through using the anodic oxide coating of this anode oxidation method growth is provided.
Technical scheme
In order to address the above problem, a kind of anodic oxidation device has according to an aspect of the present invention been proposed.This device comprises rectification modulation device unit, is configured to through to carrying out from the unitary AC voltage wave of AC power supplies that rectification produces the DC pulse wave and period 1 of DC pulse wave or first amplitude being modulated synthetic DC pulse wave being provided; The AC modulating unit, being configured to provides AC ripple through the second cycle or second amplitude modulated from the unitary AC voltage wave of AC power supplies; The pulse wave synthesis unit is configured to DC/DC assembled pulse ripple or DC/AC assembled pulse ripple are applied between anode and the negative electrode; And control unit, be configured to control the operation of rectification modulation device unit and AC modulating unit.Through making up at least one in synthetic DC pulse wave and the AC ripple, generate DC/DC assembled pulse ripple or DC/AC assembled pulse ripple.
Anodic oxidation device can also be included between rectification modulation device unit and the AC power supplies unit or the switch between AC modulating unit and AC power supplies unit.This switch can be through control unit control.
Anodic oxidation device can also be included between rectification modulation device unit and the pulse wave synthesis unit or the switch between AC modulating unit and pulse wave synthesis unit.This switch can be through control unit control.
The electrical condenser of voltage rating that rectification modulation device unit can comprise 600KHz FET (field-effect transistor) and have electrostatic capacitance and the 400V of 1500uF.
Rectification modulation device unit can comprise two or more rectification units.These two or more rectification units can be operated independently.
According to a further aspect in the invention, a kind of anode oxidation method that is used for growth anodic oxide coating on surface of aluminum plate is provided.This method is included in anode and negative electrode is set in the electrolytic solution, and anode comprises aluminium sheet; And between anode and negative electrode, apply DC/AC assembled pulse ripple.Through combination DC pulse wave and AC ripple DC/AC assembled pulse ripple is provided, and this DC/AC assembled pulse ripple has PV at the starting point place of each pulse.
Each pulse waveform of DC/AC assembled pulse ripple can be protruding upward, and voltage level is along with the time descends from voltage peak.
During from the end point of pulse to the timed interval the starting point of next pulse, negative voltage can be applied between anode and the negative electrode.
The DC pulse wave can be through making up a DC pulse wave and at least one the 2nd DC pulse wave forms, and a DC pulse wave has and at least one second pulse wave different phase.
The maximal voltage level or the average voltage level of each pulse of DC/AC assembled pulse ripple can change along with the time.
The maximal voltage level of each pulse of DC/AC assembled pulse ripple or the track of average voltage level can meet sinusoidal waveform.
At least one that has in cycle and cycle of positive voltage with DC/AC assembled pulse ripple of negative voltage of DC/AC assembled pulse ripple can change along with the time.
According to a further aspect in the invention, the anodic oxide coating that the DC/AC assembled pulse ripple that provides use to form through synthetic at least one DC pulse wave and at least one AC ripple forms on the surface of aluminium sheet or aluminium alloy plate.The thickness of anodic oxide coating can be smaller or equal to 300 μ m, and in the anodic oxide coating diameter range of lattice from 50nm to 100nm.
DC/AC assembled pulse ripple can be through making up the assembled pulse ripple of at least two formation in the first modulation DC pulse wave, the second modulation DC pulse wave and the AC ripple.
According to a further aspect in the invention, a kind of device that anode oxidation process provides the assembled pulse ripple that is used to is provided.This device comprises the first pulse wave generation unit, is configured to provide first pulse wave; The second pulse wave generation unit is configured to provide second pulse wave, and the pulse wave synthesis unit, is configured to make up first pulse wave and second pulse wave, so that the assembled pulse ripple to be provided.
This device can also comprise control unit, and this control unit is configured to the operation of the control first pulse wave generation unit, the second pulse wave generation unit and pulse wave synthesis unit.First pulse wave can be first rectification unit for the first modulation DC pulse wave, the first pulse wave generation unit; This first rectification unit is configured to first and/or first amplitude that produces a DC pulse wave and modulate a DC pulse wave the first modulation DC pulse wave is provided from the AC voltage wave of AC power supplies through rectification, and second pulse wave can be the second modulation DC pulse wave; And second the pulse wave generation unit can be second rectification unit, this second rectification unit is configured to through second and/or second amplitude that rectification produces the 2nd DC pulse wave from the AC voltage wave of AC power supplies and modulates the 2nd DC pulse wave the second modulation DC pulse wave is provided.The first pulse wave generation unit can be independent of the operation of the second pulse wave generation unit.
This device can also comprise the AC modulating unit, and this AC modulating unit is configured to from the period 3 or the 3rd amplitude of the AC voltage wave of AC power supplies AC is provided pulse wave through modulation.The pulse wave synthesis unit can be configured to make up the first modulation DC pulse wave, second modulation DC pulse wave and the AC pulse wave.
The electrical condenser of voltage rating that in the first pulse wave generation unit, the second pulse wave generation unit and the AC modulating unit at least one can comprise 600KHz FET (field-effect transistor) and have electrostatic capacitance and the 400V of 1500uF.
This device can also be included in first switch on and off between in first rectification unit and AC power supplies and the pulse wave synthesis unit; Second switch on and off between second rectification unit and AC power supplies and pulse wave synthesis unit one, and the pass is broken off in the threeway between AC modulating unit and AC power supplies and pulse wave synthesis unit one.
First pulse wave can be the first modulation DC pulse wave; The first pulse wave generation unit can be first rectification unit; This first rectification unit is configured to first and/or first amplitude that produces a DC pulse wave and modulate a DC pulse wave the first modulation DC pulse wave is provided from the AC voltage wave of AC power supplies through rectification, and second pulse wave can be the AC pulse wave; And second the pulse wave generation unit can be the AC modulating unit, this AC modulating unit is configured to from the period 3 or the 3rd amplitude of the AC voltage wave of AC power supplies AC is provided pulse wave through modulation.
According to a further aspect in the invention, a kind of anode oxidation method that is used for growth anodic oxide coating on surface of aluminum plate is provided.This method is included in anode and negative electrode is set in the electrolytic solution, and between anode and negative electrode, applies pulse wave.In this case, anode comprises aluminium sheet.
Pulse wave can have PV at the starting point place of each pulse.Pulse wave can comprise at least two in the first modulation DC pulse wave component, the second modulation DC pulse wave component and the AC wave component.Each pulse waveform of pulse wave can be protruding upward, and voltage level is along with the time descends from voltage peak.
During the timed interval of the starting point of next pulse, negative voltage can be applied between anode and the negative electrode in the end point of pulse.The first modulation DC pulse wave component can have and the second modulation DC pulse wave component different phase.The maximal voltage level of each pulse of pulse wave or average voltage level can change in time.The maximal voltage level of each pulse of pulse wave or the track of average voltage level can meet sinusoidal waveform.Can be at least through voltage level be increased to predetermined first level from the beginning level; To keep at the voltage level at the first level place for first scheduled time; Voltage is increased to second level that is higher than first level from first level, and will keep for second scheduled time formed track at the voltage level at the second level place.
At least one that has in cycle and cycle of positive voltage with pulse wave of negative voltage of pulse wave can change along with the time.
According to a further aspect in the invention, provide a kind of through comprising the anodic oxide coating that pulse wave is applied to the technology formation of the step between anode and the negative electrode.On aluminium sheet or aluminium alloy plate surface, form this anodic oxide coating, and the diameter range of the lattice in anodic oxide coating at 50nm between the 100nm.
Anodic oxide coating is formed continuously, and does not have the interface therein.
The thickness of anodic oxide coating can be smaller or equal to 300 μ m.
Beneficial effect
According to embodiments of the invention, can provide to have the anodic oxide coating that improves characteristic, be used to provide the apparatus and method of same anode zone of oxidation.
Description of drawings
Being included to provides the accompanying drawing of further understanding of the present invention to show embodiments of the invention, and is used to explain principle of the present invention with specification sheets.
In the accompanying drawings:
Fig. 1 shows the anodic oxidation device according to first embodiment of the invention.
Fig. 2 shows the anodised power supply that is used for according to an embodiment of the invention.
Fig. 3 (a), Fig. 3 (b) and Fig. 3 (c) show the instance of single order recurrent pulse ripple according to an embodiment of the invention, single order constant time length pulse wave non-periodic and single order variable-duration impulse non-periodic ripple respectively.
Fig. 4 shows the instance of second order recurrent pulse ripple according to an embodiment of the invention.
Fig. 5 (a) and Fig. 5 (b) show the instance of single order cycle DC/AC assembled pulse ripple according to an embodiment of the invention and second order cycle DC/AC assembled pulse ripple respectively.
Fig. 6 (a) and Fig. 6 (b) show the instance of single order variable duration non-periodic DC/AC assembled pulse ripple according to an embodiment of the invention and second order variable duration non-periodic DC/AC assembled pulse ripple respectively.
Fig. 7 shows the instance of DC/AC assembled pulse ripple according to an embodiment of the invention, and wherein, the track of the maximal voltage level of each pulse is similar to sinusoidal waveform.
Fig. 8 shows the sectional view that passes through the exemplary anode zone of oxidation of anode oxidation method growth according to of the present invention, and it passes through electron microscope observation.
The structure according to the microscopic examination of the exemplary anode zone of oxidation through anode oxidation method growth of the present invention of Fig. 9 instance, it passes through electron microscope observation.
< explanation of reference number >
210:AC power supply 220: rectification modulation device unit
224: the second rectification units of 222: the first rectification units
230:AC modulating unit 240: pulse wave synthesis unit
250: control unit 260a, 260b, 260c: switch
Embodiment
In the back literary composition, will illustrate and describe exemplary embodiment of the present invention.In this manual, for the present invention's purpose clearly, there be not to describe structure or the function of having understood.Referring now to describing exemplary embodiment of the present invention in detail, the example is shown specifically in the accompanying drawings.Below will provide detailed description with reference to accompanying drawing, it is intended to explain exemplary embodiment of the present invention, rather than an embodiment that can realize according to the present invention only is shown.Below describe in detail to be included as the specific detail of understanding fully of the present invention is provided.Yet it will be appreciated by those skilled in the art that does not have this specific details can realize the present invention yet.For example, provide following description to particular term, but the invention is not restricted to this, and any other term also can be used to represent the identical meaning.
Fig. 1 is the schematic representation of apparatus that is used for growth anodic oxide coating on surface of aluminum plate according to an embodiment of the invention.Anodic oxidation device can comprise electrolyzer 100, is applicable to comprise electrolytic solution 102; Anode 104 and negative electrode 106 are applicable in the value of the being filled electrolytic solution 102; And power supply 108, being configured to provides electric power or electric current between anode 104 and negative electrode 106.
Here, the aluminum or aluminum alloy plate can be used as anode 104, and alumina layer can be grown above that.In the back literary composition, for simply, term " duraluminum " can be known as " aluminium ".
Power supply 108 can provide dc voltage between anode 104 and negative electrode 106.Power supply 108 can be configured between anode 104 and negative electrode 106, typical dc voltage is provided.In addition, power supply 108 can provide DC pulse wave between anode 104 and negative electrode 106, and it is the form of pulse sequence; And/or DC/AC assembled pulse ripple can be provided between anode 104 and negative electrode 106, it can generate through combination DC pulse wave and AC ripple.Can be through supplying with dc voltage and/or DC pulse wave and/or the DC/AC mixed pulses ripple anodic oxide coating of growing.
In presents, DC/AC assembled pulse ripple and DC/DC assembled pulse ripple can be known as " assembled pulse ripple ".
Among this paper, above-mentioned " AC ripple " can be the AC pulse wave.
Fig. 2 is the skeleton diagram of the exemplary configuration of the power supply that is used for anode oxidation process according to an embodiment of the invention.
As shown in Figure 2, power supply 108 according to an embodiment of the invention can comprise rectification modulation device unit 220, AC modulator unit 230, pulse wave synthesis unit 240 and control unit 250.
In presents, term " pulse wave generation RF " is meant the combination of rectification modulation device unit 220, AC modulator unit 230 and pulse wave synthesis unit 240.
Rectification modulation device unit 220 can be configured to the AC ripple that rectification is provided by AC power cell 210, with the production burst ripple.In addition, DC pulse wave amplitude or cycle can be modulated in rectification modulation device unit 220, to produce amplitude or periodic modulation ripple.Here, DC pulse wave amplitude is represented the magnitude of voltage of DC pulse wave.In this case, rectification modulation device unit 220 can only comprise a rectification unit, can comprise the rectification unit of two or more independent operations in addition.The rectification modulation device unit 220 that in Fig. 2, schematically shows comprises two modulating units, that is, and and first modulating unit 222 and second modulating unit 224.
AC modulating unit 230 can be configured to generate and export the AC ripple through AC voltage wave period or amplitude that modulation is provided by AC power cell 210.
Pulse wave synthesis unit 240 can be configured to generate and export DC/DC assembled pulse ripple through making up its each DC pulse wave that one or more modulating unit provided by composition modulationmodulator unit 220.In addition, pulse wave synthesis unit 240 can be configured to generate and export DC/AC assembled pulse ripple through AC ripple and DC pulse wave that combination is provided by AC modulating unit 230.For example; As shown in Figure 2; Comprise in rectification modulation device unit 220 under the situation of first rectification unit 222 and second rectification unit 224; First rectification unit 222 and second rectification unit 224 are configured to independent rectification AC voltage wave, can have different cycles and amplitude to generate a DC pulse wave and the 2nd DC pulse wave, to make the DC pulse wave of winning with the 2nd DC pulse wave.The one DC pulse wave, the 2nd DC pulse wave and can be imported into pulse wave synthesis unit 240 by the AC ripple that AC modulating unit 230 provides make up then.
Control unit 250 can be connected to rectification modulation device unit 220 and AC modulating unit 230.In addition, control unit 250 can be configured to control the operation of rectification modulation device unit 220 and AC modulating unit 230, with the pulse wave characteristic of adjustment by rectification modulation device unit 220 and 230 generations of AC modulating unit.
Power supply 108 can also be included between rectification modulation device unit 220 and the AC power cell 210 or at least one switch between AC modulating unit 230 or AC power cell 210.This switch can be the switch on and off of any kind of, and it connects two electric units that connect through this switch or breaks off.Control unit 250 can further be configured to be switched on or switched off switch.Through trip switch, can determine whether provides DC pulse wave and/or AC ripple to pulse wave synthesis unit 240.For example; As shown in Figure 2, the first switch 260a, second switch 260b and the 3rd switch 260c can be arranged between the AC power cell 210 and first rectification unit 222, between AC power cell 210 and second rectification unit 224 and between AC power cell 210 and the AC rectification unit 230.Can control the waveform of the pulse wave that offers pulse wave synthesis unit 240 through trip switch 260a, 260b and 260c.Second switch 260b and the 3rd switch 260c break off if the first switch 260a connects, and then only will provide to anode and negative electrode through pulse wave synthesis unit 240 from the DC pulse wave of first modulating unit 222.But; For example; If the first switch 260a and second switch 260b connect and the 3rd switch 260c breaks off, then pulse wave synthesis unit 240 can be through the DC pulse wave output DC/DC assembled pulse ripple of combination from first rectification unit 222 and second rectification unit 224.In addition; If at least one connection among the first switch 260a and the second switch 260b and the 3rd switch 260c connect, then pulse wave synthesis unit 240 can be exported DC/AC assembled pulse ripple after receiving from the DC pulse wave of the first switch 260a and/or second switch 260b and the AC ripple from AC modulating unit 230.
In addition, above-mentioned switch can be set between rectification modulation device unit 220 and the pulse wave synthesis unit 240 or between AC modulating unit 230 and the pulse wave synthesis unit 240.In this case, the action of switch is identical with the above with effect.
Depend on from the DC pulse wave of rectification modulation device unit 220 and/or from the waveform of the AC ripple of AC modulating unit 230 such as the waveform of the assembled pulse ripple of DC/AC assembled pulse ripple and/or DC/DC assembled pulse ripple.Therefore, control unit 250 can be confirmed the waveform from the assembled pulse ripple of pulse wave synthesis unit 240 through the waveform of adjustment and control DC pulse wave and AC ripple.
Fig. 3 shows the instance of the single order DC pulse wave that can pass through first rectification unit 222 or 224 generations of second rectification unit.Fig. 3 (a) shows the instance of single order recurrent pulse ripple, and Fig. 3 (b) shows single order constant time length pulse wave non-periodic, and Fig. 3 (c) shows the instance of single order variable-duration impulse non-periodic ripple.
The DC pulse wave can pass through duty characterization recently.Pass through T OnWith T OffRatio represent dutycycle.T OnBe to be applied in the time span that is used for anodised positive voltage, and T OffFor the time span of the non-positive voltage that is applied in, as shown in Figure 3.Can represent dutycycle through following formula 1.
[formula 1]
Duty?cycle(％)＝[T on/(T on+T off)]×100
Single order recurrent pulse ripple shown in Fig. 3 (a) is periodic, and it has recurrence interval T On+ T Off, recurrent interval T Off, and in cycle T OnVoltage level does not during this time change in time.
Can be through adjustment T OnWith T OffRatio, i.e. the dutycycle of single order recurrent pulse ripple changes the characteristic of pulse wave.
Be the cycle T of each pulse in the similar part of single order constant time length pulse wave non-periodic shown in Fig. 3 (b) and single order recurrent pulse ripple OnDo not change in time.Yet, for single order constant time length pulse wave non-periodic, the interval T between the adjacent pulse OffLength change in time.
For single order variable-duration impulse non-periodic ripple, cycle T OnLength and/or the interval T between the adjacent pulse OffLength change in time.Fig. 3 (c) shows single order variable-duration impulse non-periodic ripple, wherein, and cycle T OnLength and/or the interval T between the adjacent pulse OffLength change in time.
Simultaneously, can obtain DC/DC assembled pulse ripple through the DC pulse wave that makes up from first rectification unit 222 and second rectification unit 224.DC/DC assembled pulse ripple can be divided at least three types: second order recurrent pulse ripple, second order constant time length pulse wave non-periodic and second order variable-duration impulse non-periodic ripple.
For the second order recurrent pulse ripple shown in Fig. 4, the recurrence interval keeps constant, and cycle T OnComprise two different sub cycles with different electric voltage level.That is cycle T, OnComprise the first subcycle T with relative higher voltage level HWith the second subcycle T with relatively low voltage level LThe first and second subcycle T HAnd T LTime span do not change along with the time respectively.
Can be through obtaining second order recurrent pulse ripple from the DC pulse wave of first rectification unit 222 and DC pulse wave from second rectification unit 224 in pulse wave synthesis unit 240 places combinations.For example, first rectification unit 222 can generate and have relative higher voltage level and relatively than SP T On, 1A DC pulse wave, and second rectification unit 224 can generate and has relatively low voltage level and relative longer cycle T On, 2The 2nd DC pulse wave, pulse wave synthesis unit 240 can make up a DC pulse wave and the 2nd DC pulse wave then, to produce second order recurrent pulse ripple as shown in Figure 4.
Can utilize with Fig. 3 identical principle of principle that illustrates that combines and generate second order constant time length pulse wave non-periodic and second order variable-duration impulse non-periodic ripple.For example, can obtain second order constant time length pulse wave non-periodic through meeting the following conditions: (i) in time will be from the cycle T of a DC pulse wave of first rectification unit 222 On, 1With cycle T from the 2nd DC pulse wave of second rectification unit 224 On, 2Remain on steady state value, (ii) change the interval T of a DC pulse wave and the 2nd DC pulse wave in time with same ratio Off, 1And T Off, 2Can obtain second order variable-duration impulse non-periodic ripple through above condition (i) being changed into following condition: (i ') change cycle T with same ratio in time On, 1And cycle T On, 2
In addition, the power supply according to this embodiment can generate and provide DC/AC assembled pulse ripple through combination by the AC ripple of AC modulating unit 230 generations and the one or more DC pulse waves that generated by first rectification unit 222 and/or second rectification unit 224.Fig. 5 shows the instance of DC/AC assembled pulse ripple.This DC/AC assembled pulse ripple demonstrates by the AC ripple in cycle T OnThe characteristic of the voltage peak that forms during this time.In this case, the cycle T of PV in each pulse OnHas highest voltage level during this time.
Fig. 5 (a) shows the instance of the single order DC/AC assembled pulse ripple that the AC ripple that changes in time through combination single order recurrent pulse ripple and its voltage level generates.In single order DC/AC assembled pulse ripple, the cycle T in each pulse OnForm voltage level during this time.In this case, preferably form single order DC/AC assembled pulse ripple, make voltage peak be in cycle T OnThe starting point place.In this case, each pulse waveform can be for protruding upward, and voltage level begins to descend from voltage peak.In addition, as shown in Figure 5, DC/AC assembled pulse ripple is in the interval T from the end point of a pulse to the starting point of next pulse OffCan have negative voltage level during this time.
Fig. 5 (b) shows the instance of the second order DC/AC assembled pulse ripple that generates through combination second order recurrent pulse ripple and AC ripple; Wherein second order recurrent pulse ripple generates through combination first rectification unit 222 and second rectification unit 224, and the AC ripple is provided by AC modulating unit 230.This second order DC/AC assembled pulse ripple can utilize with the above-mentioned identical principle of principle about single order DC/AC assembled pulse ripple and generate.
In addition, can utilize the principle identical with above-mentioned principle through the combination AC ripple and non-periodic constant time length pulse wave provide non-periodic constant time length DC/AC assembled pulse ripple.Similarly, can utilize the principle identical with above-mentioned principle through the combination AC ripple and non-periodic the variable-duration impulse ripple provide non-periodic variable duration DC/AC assembled pulse ripple.In Fig. 6 (a) and Fig. 6 (b), show exemplary single order variable duration non-periodic DC/AC assembled pulse ripple and second order variable duration non-periodic DC/AC assembled pulse ripple respectively.
For above-mentioned DC/AC assembled pulse ripple, maximal voltage level is perhaps as each recurrence interval T of each pulse OnIn the average voltage level of MV of maximal voltage level and minimum voltage level remain on the steady state value place in time.Yet, can form pulse wave, make the maximal voltage level of each pulse or average voltage level change in time.Fig. 7 shows the instance of second order variable duration non-periodic DC/AC assembled pulse ripple, and wherein the maximal voltage level of each pulse changes in time.For the graphic representation among Fig. 7, the track and the sinusoidal waveform of the maximal voltage level of each pulse are similar.
In addition, during anode oxidation process, maximal voltage level or average voltage level can change along with stepped track.Promptly; When the pulse mode voltage wave is applied between anode and the negative electrode; Can implement anode oxidation process through repeating following steps: (i), (ii) voltage level is remained on the predetermined level place scheduled time increasing between original levels and the predetermined level or reducing the voltage level between anode and negative electrode.
Can generate the pulse wave that has such as the various characteristics of DC pulse wave, DC/DC assembled pulse ripple and DC/AC assembled pulse ripple as described above.Can utilize above-mentioned various pulse wave that anodic oxide coating is formed and have various characteristics.The anodic oxide coating that becomes through different pulse shape can have different characteristic.Compare with using the DC pulse wave that generates through traditional DC power supply, the anodic oxide coating that the DC/AC assembled pulse ripple that use according to an embodiment of the invention generates through power supply is grown on surface of aluminum plate has significantly improved machinery and chemical property.Particularly, be positioned at the anodic oxide coating that anode oxidation process produced that the DC/AC assembled pulse ripple at the starting point place of each pulse carries out through its PV separately and can have structure very uniformly, its thickness is so thin like 300 μ m.In addition, this anodic oxide coating shows improved erosion resistance and mechanical characteristics, for example, and wear resistance or hardness.
In the back literary composition, with describing according to embodiments of the invention and using the result of DC/AC assembled pulse ripple according to an embodiment of the invention through the various characteristics test of the anodic oxide coating of anode oxidation method formation.
Experiment embodiment
In this embodiment, the anode oxidation process that the DC/AC assembled pulse ripple that use produces through power supply shown in Figure 2 carries out, and this power supply is realized with the compact form of drawer type.First rectification unit 222 of power supply and each in second rectification unit 224 all can comprise 600kHz FET (FET) and have the electrical condenser of voltage rating of electrostatic capacitance and the 400V of 1500uF.In this case, consider rate of heat dissipation, each in first rectification unit 222 and second rectification unit 224 all can comprise one group of two same unit.Be used for anodised DC/AC assembled pulse ripple and be the second order variable duration non-periodic DC/AC assembled pulse ripple shown in Fig. 6 (b); Wherein, Each pulse waveform is protruding upward; And voltage level reduces from the voltage peak of the starting point that is positioned at each pulse, and from the end point of a pulse to the interval T the starting point of next pulse OffApply negative voltage during this time.
In this case, basic level voltage (that is, the minimum voltage level of unit pulse) is set to-0.5V, and allows PV to reach maximum 40V.In the present embodiment, first voltage level and second voltage level are set to 10V and 5V respectively.In addition, allow the cycle of unit pulse to adjust between the 10sec at 10msec.
For electrolytic solution, the density that is used for the sulphuric acid soln of accelerated reaction can be set in 3% to 10% scope.In the present embodiment, the density of sulphuric acid soln is set between 5% to 6%.In addition, 3.0% pyroligneous liquor can be added to electrolytic solution.In the present embodiment, 1.0% pyroligneous liquor can be added to electrolytic solution.In addition, during the reaction times, the temperature of electrolytic solution is maintained at-2 ℃.
The generation of DC/AC assembled pulse ripple can be described below the ground Be Controlled.Aluminium sheet as the target of anode oxidation process is set up, with as anode.Voltage between anode and negative electrode is risen to 5V (step S1) lentamente from 0V.Then, sustaining voltage 5 minutes (step S2).Then, voltage is risen to 10V (step S3) from 5V.Then, sustaining voltage grows into required thickness (step S4) until anodic oxide coating.Remain on the conventional anodization technology between the 15V to 40V than the voltage between the electrode; Use the anode oxidation process consumption power still less of above-mentioned four steps, and produce anodic oxide coating and pile up with level structures density, high-grade hardness, high-grade wear resistance and high-grade erosion resistance.
The thickness range of the anodic oxide coating that produces through above embodiment from 20 μ m to 300 μ m.In addition, anodic oxide coating comprises the lattice with even cross-sectional structure.The xsect of the anodic oxide coating of the outside surface from the aluminum oxide interface to anodic oxide coating has uniform crystalline network.According to traditional anode oxidation method, can not easily obtain to have the uniform texture of above-mentioned thickness range from 20 μ m to 300 μ m.
Fig. 8 shows the sectional view through the exemplary anode zone of oxidation with 220 μ m thickness of electron microscope observation.
Fig. 9 shows the microstructure through the anodic oxide coating of electron microscope observation.
Observe anodic oxide coating according to an embodiment of the invention and have uniform crystalline network.In this case, the scope of lattice diameter is from 50nm to 100nm.Therefore, the scope from 50/300,00 to 1/6,000 of aspect ratio (diameter/length).
Fig. 9 shows the part that the lattice diameter is approximately the anodic oxide coating of 50nm and 80nm.
According to this observation, should be understood that, can produce the anodic oxide coating with a density and even lattice diameter of continuous growth according to anode oxidation method of the present invention.Can observe above-mentioned microstructure characteristic, and irrelevant with the thickness of the anodic oxide coating that uses the embodiments of the invention growth.Can not obtain to have the even microstructural this anodic oxide coating of about 300 μ m thickness through the conventional anodization method.Because the good microstructure characteristic that obtains through the present invention has obtained good improvement machinery, electricity and chemical property according to anodic oxide coating of the present invention.
Table 1 shows according to thickness of oxide layer and is used for the result that Rockwell hardness (HRC, KS B 0806:2000) is tested and Vickers' hardness (Hv) is tested that the type that is used for anodised aluminium according to an embodiment of the invention is carried out.For comparison purposes, in table 1, also show in general factory and be used as SUS 316 stainless steels of structured material and the hardness of titanium.In table 1, the hardness that shows the aluminum of the AL 6061 with any anodic oxide coating is starkly lower than titanium and SUS 316 stainless hardness.Yet when the anodic oxide coating of growth 20 μ m-60 μ m on aluminium sheet, observing the Rockwell hardness scope and be from 57-59 and Vickers' hardness scope is from 636 to 675, and this is to improve the result significantly.These numerical value are apparently higher than titanium and SUS 316 stainless hardness.Particularly, when growth on AL 5058 aluminium sheets obtains fabulous hardness result during anodic oxide coating, make Rockwell hardness scope height to 70 (corresponding to Vickers' hardness 1030).
[table 1]
The material of anodic oxide coating and thickness HRC HV
AL?5058-25μm 70 1030
AL?6061-30μm 57 636
AL?6061-40μm 59 675
AL?6061-50μm 58 655
AL?6061-60μm 59 675
AL?6061-0μm 0 90
Titanium 32 317
SUS?316 0 155
The aluminium sheet with anodic oxide coating to forming through one embodiment of the present of invention is implemented salt water atomization test (KS D9502:2007) three months, and the result has been shown in table 2.The test soln that is used for this test comprises 5% ± 1% sodium-chlor (PH 6.8 ± 0.3), and probe temperature remains on 35 ± 2 ℃, and atomization quantity is 2 ± 0.5ml/h/80cm 2As shown in table 2, even observe any corrosion that in trimestral saltwater environment, on each test sample, also can not occur such as expanding or getting rusty.According to this result, can understand, the erosion resistance with aluminium sheet of the anodic oxide coating of growing through one embodiment of the present of invention has been significantly increased.
[table 2]
Figure BPA00001462432100141
Table 3 shows the corrosion-resistant data as some kinds of the metal of corrosion resistant material, with the salt solution erosion resistance of indirect above metal and the salt solution erosion resistance of the aluminium sheet with the anodic oxide coating of growing through one embodiment of the present of invention.According to these data, be appreciated that the product that produces through the present invention has fabulous opposing brinish erosion resistance.The data of table 3 are from " corrosion resistance tables:metals, plastics, nonmetallic, and rubbers ", Schweitzer, Philip A, M.Dekker, 1985.
[table 3]
Figure BPA00001462432100142
Table 4 shows the result according to the wearability test of the aluminium sheet with anodic oxide coating of the present invention.Here, carry out wearability test through the U.S.ASTM D 3884:1992 standard method of test of wear resistance.As shown in table 4, the antiwear characteristic of aluminium sheet with anodic oxide coating is well more a lot of than the antiwear characteristic of the aluminium sheet that does not have anodic oxide coating.Particularly, having thickness is that the wear-resisting grade of aluminium sheet of the anodic oxide coating of 40 μ m is 60 times of wear-resisting grade that do not have the aluminium sheet of anodic oxide coating.
[table 4]
#1(mg) #2(mg) #3(mg) MV
Al-0 μ m top layer 132 125 133 130.0
Al-20 μ m top layer 23 19 14 18.7
Al-30 μ m top layer 3 4 7 4.7
Al-40 μ m top layer 1 3 3 2.3
Table 5 shows the result that the thermal conductivity with aluminium sheet of anodic oxide coating according to the present invention is tested.Carry out the thermal conductivity test through the laser scintillation technique.When on aluminium sheet, not forming anodic oxide coating, the observed value of thermal conductivity coefficient k is 153.4 (W/mK); When formation thickness was the anodic oxide coating of 20 μ m, the observed value of thermal conductivity coefficient k was 150.7 (W/mK); And when formation thickness was the anodic oxide coating of 40 μ m, the observed value of thermal conductivity coefficient k was 149.7 (W/mK).According to this result, be appreciated that the thermal conductivity coefficient value is reduced to less than 3% when utilizing anodic oxide coating to cover aluminium sheet.The thermal conductivity coefficient of more than measuring is greater than titanium or stainless thermal conductivity coefficient with the material that acts on the heat exchanger that uses seawater.
[table 5]
Figure BPA00001462432100151
Table 6 shows the electrical insulation capability of the aluminium sheet with the anodic oxide coating that forms through the present invention.Carry out the electrical isolation test through following method:
Figure BPA00001462432100152
electrode is set at the sample place; 2000V voltage was applied to sample one minute, and checks any insulation failure of sample then to confirm whether to occur.According to this result, be appreciated that anodic oxide coating according to the present invention has the good insulation performance performance.
[table 6]
The result
Al-30 μ m top layer Insulating fault does not appear
Al-40 μ m top layer Insulating fault does not appear
Table 7 shows the result of the flexural strength test of the aluminium sheet with the anodic oxide coating that forms through the present invention.Carry out the flexural strength test through the U.S.ASTM D790:2003 standard method of test of flexural property.Test set is the C.R.E. type, and test speed is 2mm/min.As shown in table 7, the flexural strength level of aluminium sheet with anodic oxide coating is high more a lot of than the flexural strength level of the aluminium sheet that does not have anodic oxide coating.
[table 7]
The result
There is not anodic oxide coating 1140.1
Al-20 μ m top layer 1298.1
According to above test result, all aluminium sheets with anodic oxide coating according to the present invention all have improved surface property, and it can not be realized through traditional anode oxidation method.Be appreciated that and obtain having anodic oxide coating through the present invention than the better characteristic of zone of oxidation that can pass through the traditional method acquisition.
Utilization can be with the pulse wave with various waveforms according to power supply of the present invention, and for example, DC pulse wave, DC/DC assembled pulse ripple and DC/AC assembled pulse ripple provide between the pair of electrodes, are used for anodic oxidation.
In addition, the anodic oxide coating of growing through anode oxidation method according to the present invention has uniform structure, and the thickness of this anodic oxide coating is than the thickness thicker of the anodic oxide coating that forms through traditional method.
Because according to the improved structural performance of anodic oxide coating of the present invention, anodic oxide coating has the improved mechanical property of hardness, wear resistance and flexural strength aspect, and improved erosion resistance and insulation characterisitic.
In presents, first rectification unit, second rectification unit and AC modulating unit can be made the pulse wave generation unit by general designation.
Above-mentioned exemplary embodiment is element of the present invention and combination of features.This element or characteristic can be thought optionally except as otherwise noted.Each element or characteristic can be implemented, and need not and other elements or characteristics combination.In addition, embodiments of the invention can be realized through the part of composition element and/or characteristic.The working order of describing in an embodiment of the present invention can be arranged again.Some structures of arbitrary embodiment can be included among another embodiment, and can replace with the counter structure of another embodiment.Clearly, can realize the present invention, perhaps make the present invention can comprise new claim through after application, making amendment through the combination that in accompanying claims, does not have the claim of knowing the relation of quoting.
It will be apparent to those skilled in the art that under the situation that does not deviate from the spirit or scope of the present invention, can modifications and variations of the present invention are.Therefore, the present invention is intended to cover through paying claim and is equal to change of the present invention and the change that provides in the scope of replacement.
Claims (according to the modification of the 19th of treaty)
1. one kind is used to the device that anode oxidation process provides the assembled pulse ripple, and said device comprises:
The first pulse wave generation unit is configured to provide first pulse wave;
The second pulse wave generation unit is configured to provide second pulse wave; And
The pulse wave synthesis unit is configured to make up said first pulse wave and said second pulse wave.
2. device according to claim 1 further comprises:
Control unit is configured to control the operation of the said first pulse wave generation unit, the said second pulse wave generation unit and said pulse wave synthesis unit.
3. device according to claim 1, wherein,
Said first pulse wave is the first modulation DC pulse wave,
The said first pulse wave generation unit is first rectification unit; Said first rectification unit is configured to produce a DC pulse wave through rectification from the AC voltage wave of AC power supplies; And modulate first and/or first amplitude of a said DC pulse wave, the said first modulation DC pulse wave is provided
Said second pulse wave is the second modulation DC pulse wave, and
The said second pulse wave generation unit is second rectification unit; Said second rectification unit is configured to produce the 2nd DC pulse wave through rectification from the said AC voltage wave of said AC power supplies; And modulate said the 2nd DC pulse wave second and/or second amplitude, the said second modulation DC pulse wave is provided.
4. device according to claim 3, wherein,
The said first pulse wave generation unit is independent of said second pulse wave generation unit operation.
5. device according to claim 3 further comprises: the AC modulating unit, and being configured to provides AC pulse wave through the period 3 or the 3rd amplitude of modulation from the said AC voltage wave of said AC power supplies, wherein,
Said pulse wave synthesis unit is configured to make up the said first modulation DC pulse wave, said second modulation DC pulse wave and the said AC pulse wave.
6. device according to claim 5; Wherein, the electrical condenser of voltage rating that comprises 600KHzFET (field-effect transistor) and have electrostatic capacitance and the 400V of 1500uF of at least one in the said first pulse wave generation unit, the said second pulse wave generation unit and the said AC modulating unit.
7. device according to claim 5 further comprises:
First switch on and off between one in said first rectification unit and said AC power supplies and said pulse wave synthesis unit,
Second switch on and off between said second rectification unit and said AC power supplies and said pulse wave synthesis unit one, and
Threeway between said AC modulating unit and said AC power supplies and said pulse wave synthesis unit one is broken off and being closed.
8. device according to claim 1, wherein,
Said first pulse wave is the first modulation DC pulse wave,
The said first pulse wave generation unit is first rectification unit; Said first rectification unit is configured to produce a DC pulse wave through rectification from the AC voltage wave of AC power supplies; And first and/or first amplitude of modulating a said DC pulse wave, the said first modulation DC pulse wave is provided
Said second pulse wave is the AC pulse wave, and
The said second pulse wave generation unit is the AC modulating unit, and said AC modulating unit is configured to through period 3 or three amplitude of modulation from the said AC voltage wave of said AC power supplies AC is provided pulse wave.
9. anode oxidation method that is used on surface of aluminum plate the growth anodic oxide coating, said method comprises:
Anode and negative electrode are set in electrolyzer, and said anode comprises said aluminium sheet; And
Pulse wave is applied between said anode and the said negative electrode.
10. anode oxidation method according to claim 9, wherein, said pulse wave has PV at the starting point place of each pulse.
11. anode oxidation method according to claim 9, wherein, said pulse wave comprises at least two in the first modulation DC pulse wave component, the second modulation DC pulse wave component and the AC wave component.
12. anode oxidation method according to claim 9, wherein, each pulse waveform of said pulse wave is protruding upward, and voltage level is along with the time descends from voltage peak.
13. anode oxidation method according to claim 9 wherein, during from the end point of pulse to the timed interval the starting point of next pulse, is applied to negative voltage between said anode and the said negative electrode.
14. anode oxidation method according to claim 11, wherein, the said first modulation DC pulse wave component has and the said second modulation DC pulse wave component different phase.
15. anode oxidation method according to claim 9, wherein, the maximal voltage level or the average voltage level of each pulse of said pulse wave change in time.
16. anode oxidation method according to claim 9, wherein, the maximal voltage level of each pulse of said pulse wave or the track of average voltage level meet sinusoidal waveform.
17. anode oxidation method according to claim 16 wherein, forms said track through following steps:
Voltage level is increased to predetermined first level from original levels,
Said voltage level is remained on said first scheduled time of first level,
Said voltage is increased to second level from said first level, and said second level is higher than said first level, and
Said voltage level is remained on said second scheduled time of second level.
18. anode oxidation method according to claim 9, wherein, at least one that has in cycle and cycle of positive voltage with said pulse wave of negative voltage of said pulse wave changes in time.
19. an anodic oxide coating that forms through the technology that may further comprise the steps, said step is:
Pulse wave is applied between anode and the negative electrode, wherein,
Said anodic oxide coating is formed on aluminium sheet or the aluminium alloy plate surface, and the scope of the lattice diameter in said anodic oxide coating at 50nm between the 100nm.
20. anodic oxide coating according to claim 19, wherein, the thickness of said anodic oxide coating is smaller or equal to 300 μ m.

Claims (20)

  1. A kind ofly be used to the device that anode oxidation process provides the assembled pulse ripple, said device comprises:
    The first pulse wave generation unit is configured to provide first pulse wave;
    The second pulse wave generation unit is configured to provide second pulse wave; And
    The pulse wave synthesis unit is configured to make up said first pulse wave and said second pulse wave.
  2. Device according to claim 1 further comprises:
    Control unit is configured to control the operation of the said first pulse wave generation unit, the said second pulse wave generation unit and said pulse wave synthesis unit.
  3. Device according to claim 1, wherein,
    Said first pulse wave is the first modulation DC pulse wave,
    The said first pulse wave generation unit is first rectification unit; Said first rectification unit is configured to produce a DC pulse wave through rectification from the AC voltage wave of AC power supplies; And modulate first and/or first amplitude of a said DC pulse wave, the said first modulation DC pulse wave is provided
    Said second pulse wave is the second modulation DC pulse wave, and
    The said second pulse wave generation unit is second rectification unit; Said second rectification unit is configured to produce the 2nd DC pulse wave through rectification from the said AC voltage wave of said AC power supplies; And modulate said the 2nd DC pulse wave second and/or second amplitude, the said second modulation DC pulse wave is provided.
  4. Device according to claim 3, wherein,
    The said first pulse wave generation unit is independent of said second pulse wave generation unit operation.
  5. Device according to claim 3 further comprises: the AC modulating unit, and being configured to provides AC pulse wave through the period 3 or the 3rd amplitude of modulation from the said AC voltage wave of said AC power supplies, wherein,
    Said pulse wave synthesis unit is configured to make up the said first modulation DC pulse wave, said second modulation DC pulse wave and the said AC pulse wave.
  6. Device according to claim 5; Wherein, the electrical condenser of voltage rating that comprises 600KHzFET (field-effect transistor) and have electrostatic capacitance and the 400V of 1500uF of at least one in the said first pulse wave generation unit, the said second pulse wave generation unit and the said AC modulating unit.
  7. Device according to claim 5 further comprises:
    First switch on and off between one in said first rectification unit and said AC power supplies and said pulse wave synthesis unit,
    Second switch on and off between said second rectification unit and said AC power supplies and said pulse wave synthesis unit one, and
    Threeway between said AC modulating unit and said AC power supplies and said pulse wave synthesis unit one is broken off and being closed.
  8. Device according to claim 1, wherein,
    Said first pulse wave is the first modulation DC pulse wave,
    The said first pulse wave generation unit is first rectification unit; Said first rectification unit is configured to produce a DC pulse wave through rectification from the AC voltage wave of AC power supplies; And first and/or first amplitude of modulating a said DC pulse wave, the said first modulation DC pulse wave is provided
    Said second pulse wave is the AC pulse wave, and
    The said second pulse wave generation unit is the AC modulating unit, and said AC modulating unit is configured to through period 3 or three amplitude of modulation from the said AC voltage wave of said AC power supplies AC is provided pulse wave.
  9. A kind of anode oxidation method that is used for growth anodic oxide coating on surface of aluminum plate, said method comprises:
    Anode and negative electrode are set in electrolyzer, and said anode comprises said aluminium sheet; And
    Pulse wave is applied between said anode and the said negative electrode.
  10. Anode oxidation method according to claim 9, wherein, said pulse wave has PV at the starting point place of each pulse.
  11. Anode oxidation method according to claim 9, wherein, said pulse wave comprises at least two in the first modulation DC pulse wave component, the second modulation DC pulse wave component and the AC wave component.
  12. Anode oxidation method according to claim 9, wherein, each pulse waveform of said pulse wave is protruding upward, and voltage level is along with the time descends from voltage peak.
  13. Anode oxidation method according to claim 9 wherein, during from the end point of pulse to the timed interval the starting point of next pulse, is applied to negative voltage between said anode and the said negative electrode.
  14. Anode oxidation method according to claim 11, wherein, the said first modulation DC pulse wave component has and the said second modulation DC pulse wave component different phase.
  15. Anode oxidation method according to claim 9, wherein, the maximal voltage level or the average voltage level of each pulse of said pulse wave change in time.
  16. Anode oxidation method according to claim 9, wherein, the maximal voltage level of each pulse of said pulse wave or the track of average voltage level meet sinusoidal waveform.
  17. Anode oxidation method according to claim 16 wherein, forms said track through following steps:
    Voltage level is increased to predetermined first level from original levels,
    Said voltage level is remained on said first scheduled time of first level,
    Said voltage is increased to second level from said first level, and said second level is higher than said first level, and
    Said voltage level is remained on said second scheduled time of second level.
  18. Anode oxidation method according to claim 9, wherein, at least one that has in cycle and cycle of positive voltage with said pulse wave of negative voltage of said pulse wave changes in time.
  19. A kind of anodic oxide coating that forms through the technology that may further comprise the steps, said step is:
    Pulse wave is applied between anode and the negative electrode, wherein,
    Said anodic oxide coating is formed on aluminium sheet or the aluminium alloy plate surface, and the scope of the lattice diameter in said anodic oxide coating at 50nm between the 100nm.
  20. Anodic oxide coating according to claim 19, wherein, the thickness of said anodic oxide coating is smaller or equal to 300 μ m.
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