CN104611759A - Polarity-variable pulse acid-pickling control method - Google Patents
Polarity-variable pulse acid-pickling control method Download PDFInfo
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- CN104611759A CN104611759A CN201510080244.XA CN201510080244A CN104611759A CN 104611759 A CN104611759 A CN 104611759A CN 201510080244 A CN201510080244 A CN 201510080244A CN 104611759 A CN104611759 A CN 104611759A
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- pickling
- workpiece
- voltage
- acid pickling
- polarity
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F7/00—Constructional parts, or assemblies thereof, of cells for electrolytic removal of material from objects; Servicing or operating
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F1/00—Electrolytic cleaning, degreasing, pickling or descaling
- C25F1/02—Pickling; Descaling
- C25F1/04—Pickling; Descaling in solution
- C25F1/06—Iron or steel
Abstract
The invention discloses a polarity-variable pulse acid-pickling control method, which comprises the following steps: when a workpiece is put in acidic electrolyte to carry out acid pickling, carrying out real-time detection on the electrical characteristic information of the workpiece; and judging whether the electric characteristic information meets polarity switching conditions, if so, changing the polarity of an output pulse of a power supply system, so that the workpiece is subjected to acid pickling from cathodic acid pickling to anodic acid pickling or from anodic acid pickling to cathodic acid pickling. According to the invention, by controlling the polarity-variable output of the power supply system, a workpiece is alternately subjected to cathodic acid pickling and anodic acid pickling, thereby avoiding a fact that materials of the workpiece have a hydrogen embrittlement phenomenon, improving the acid pickling effect and increasing the efficiency of acid pickling.
Description
[technical field]
The present invention relates to technical field of surface, particularly a kind of Variable Polarity pulse pickling control method.
[background technology]
Metal all must carry out pickling before the surface treatments such as plating, electroless plating, conversion film, and its objective is corrosion thing and the zone of oxidation on removing metallic article surface, this is the important prerequisite obtaining high quality rete.Different derusting methods can be taked according to corrosion and the situation of oxide skin and the difference of character.Derusting method is mainly divided into two large classes, i.e. physical method and chemical process.Physical method mainly contains artificial rust cleaning and mechanical rust removal (as sandblasting, shot-peening, polishing etc.).Chemical rust removing is generally the method adopting pickling, and the iron and steel parts be about to oxide skin or iron rust corrodes, to remove oxide compound or the corrosion layer of surface of steel workpiece in pickle solution.
Compare traditional chemical pickling, electrolytic pickling is a kind of acid washing method efficiently, has corrosive power strong, the advantages such as speed is fast.During electrolytic pickling, workpiece both can as anode, also can as negative electrode.When workpiece is as negative electrode, the reaction that cathode of electrolytic tank region occurs is:
Fe
2++2e→Fe
Fe
3++3e→Fe
2H
++2e→2[H]→H
2↑
When workpiece is as anode, the reaction that electrolytic cell anode region occurs is:
Fe-2e→Fe
2+
Fe-3e→Fe
3+
4OH
--4e→2H
2O O O
2↑
As from the foregoing: when workpiece carries out Cathodic pickling as negative electrode, the H in electrolytic solution
+obtain electronics and become active hydrogen atom [H], a hydrogen atom part is combined into H
2effusion, has mechanically peel effect to oxide skin and iron rust, is conducive to the removal of oxide skin and iron rust, and pickling effect is also better, but pickling speed is slow, and a part of hydrogen can invade metal with atomic condition from interstitial void, diffuses to inside, causes the hydrogen embrittlement of material.When carrying out anodic acid pickling, although ooze hydrogen phenomenon to obtain certain control, metal is excessive erosion very easily, and pickling effect is general.
[summary of the invention]
Based on this, the invention provides a kind of Variable Polarity pulse pickling control method, the Variable Polarity pulse waveform that all can independently be regulated by power-supply system output amplitude, frequency, workpiece is hocketed anodic acid pickling and Cathodic pickling, while raising pickling efficiency, suppress workpiece to ooze hydrogen, reduce the roughness of workpiece surface, make the workpiece surface after process more smooth, present metalluster.
The content of the embodiment of the present invention is as follows:
A kind of Variable Polarity pulse pickling control method, comprises the steps:
When workpiece being placed in acid electrolyte and carrying out pickling, detect the electrical feature information of described workpiece in real time;
Judge whether described electrical feature information meets polarity switching condition:
If meet, then change the polarity that power-supply system exports pulse, make described workpiece switch to anodic acid pickling by Cathodic pickling or switch to Cathodic pickling by anodic acid pickling.
Variable Polarity pulse pickling control method provided by the invention, by detecting the electrical feature information of workpiece in real time, can adjust the output polarity of power-supply system automatically, ensures that the acid cleaning process of workpiece is in or close to optimum state.The present invention carries out Variable Polarity output by controlling power-supply system, and workpiece is hocketed anodic acid pickling and Cathodic pickling, while the higher pickling speed of guarantee, improves pickling effect, avoids workpiece material generation Hydrogen Brittleness Phenomena.
[accompanying drawing explanation]
Fig. 1 is the schematic flow sheet of a kind of Variable Polarity pulse pickling control method in the embodiment of the present invention;
Fig. 2 is the waveform schematic diagram of Variable Polarity pulse in the embodiment of the present invention;
Fig. 3 is typical anodic polarization curves figure in the embodiment of the present invention;
Fig. 4 is the schematic flow sheet of the polarity switching deciding method of Variable Polarity pulse in the embodiment of the present invention;
Fig. 5 is for the electrical characteristic waveform schematic diagram in different frequency treating processes in the embodiment of the present invention;
Fig. 6 is the workpiece surface design sketch for different frequency process gained in the embodiment of the present invention;
Fig. 7 is the relation curve in the embodiment of the present invention between best switching frequency and current density.
[embodiment]
Below in conjunction with accompanying drawing, content of the present invention is further described.
As shown in Figure 1, the invention provides a kind of Variable Polarity pulse pickling control method, comprise the steps:
S11: when workpiece being placed in acid electrolyte and carrying out pickling, detects the electrical feature information of described workpiece in real time;
S12: judge whether described electrical feature information meets polarity switching condition, if meet, then enters S13;
S13: change the polarity that power-supply system exports pulse, make described workpiece switch to anodic acid pickling by Cathodic pickling or switch to Cathodic pickling by anodic acid pickling.
In a specific examples, workpiece is 304 stainless steel hot-rolling plates, and it is of a size of 4cm × 4cm × 0.4cm, and acid electrolyte is: concentration is the Na of 150g/L (gram often liter)
2sO
4(sodium sulfate) and concentration are the HNO of 60g/L (gram often liter)
3(nitric acid).
Two blocks of identical 304 stainless steel hot-rolling plates are connected to respectively output plus terminal and the negative terminal of power-supply system, both parallel placements, spacing 50mm; Then initial time anode is one piece of 304 stainless steel hot-rolling plate, and negative electrode is another block 304 stainless steel hot-rolling plate.Utilize power-supply system to export Variable Polarity pulse square wave as shown in Figure 2, two piece of 304 described stainless steel hot-rolling plate is hocketed anodic acid pickling and Cathodic pickling; In Fig. 2, I
p=10A, I
n=-10A, t
p=2ms, t
n=3ms, processes 2min under room temperature.
The composition of 304 stainless steel hot-rolling plate surface scales is mainly divided into three layers from outside to inside: outermost layer is the oxide compound of iron, comprises Fe
2o
3, Fe
3o
4, FeO; Middle layer is more stable iron chromium oxide FeOCr
2o
3, be Cr near the internal layer of matrix
2o
3, NiO etc., matrix surface is " poor layers of chrome ".
After energising, 304 stainless steel hot-rolling plates as the electrochemical reaction occurred respectively during anode and cathode are:
Anodic reaction:
H
2O→[O]+2H
++2e
2[O]→O
2↑
Fe
xO
y+(3x-y)[O]+xH
2O→xFeO
4 2-+2xH
+
Cr
2O
3+3[O]+2H
2O→2CrO
4 2-+4H
+
Cr
2O
3+3[O]+H
2O→Cr
2O
7 2-+2H
+
NiO+2H
+→Ni
2++2H
2O
Cathodic reaction:
FeO
4 2-+8H
++3e→Fe
3++4H
2O
2H
++2e→H
2↑
304 stainless steel hot-rolling plate surface scales have loose porous property, the anodic acid pickling stage, and the Sauerstoffatom of status nascendi is the major impetus of oxidizing reaction, and the reactive behavior point places such as the hole that anodizing is first tiny on surface and crack occur, by FeO, Fe
3o
4, Fe
2o
3, FeOCr
2o
3change into FeO
3and FeO
3cr
2o
3, and then with
be dissolved in acid electrolyte, the picotite of indissoluble loosened and is separated, the skeleton structure of disruptive oxidation skin.Cr simultaneously
2o
3be oxidized to CrO
3, in sour environment with
with
exist, NiO is dissolved in acid and becomes Ni
2+deng, the effect of loose scale is played in the dissolving of these oxide compounds further, causes peeling off of oxide skin to be expanded centered by aperture and crack; A part of active oxygen atom becomes oxygen molecule in the surface bonding of 304 stainless steel hot-rolling plates simultaneously, and the gathering of oxygen molecule makes bubble constantly expand change greatly, and the final 304 stainless steel hot-rolling plates that depart from are overflowed in gaseous form, and this process has mechanically peel effect to oxide skin.
The Cathodic pickling stage, ate electrode
with
obtain electronics and become Fe
3+and Cr
3+, H simultaneously
+obtain electronics and produce hydrogen atom, a part of hydrogen atom is combined into H
2effusion, mechanically peel effect is produced to oxide skin; Part hydrogen invades metal with atomic condition from interstitial void, diffuses to inside, causes the hydrogen embrittlement of 304 stainless steel hot-rolling panel materials.
It can thus be appreciated that during anodic acid pickling, the mechanically peel effect that the electrochemical dissolution of 304 stainless steel hot-rolling plate oxide on surface is aided with oxygen again causes coming off of oxide skin, therefore the speed of anodic acid pickling is very fast.When carrying out Cathodic pickling, oxide compound does not participate in electrochemical reaction, and the removal of oxide skin can only rely on the mechanically peel effect of hydrogen, and oxide skin exfoliation rates is slower.During independent employing anodic acid pickling, easily cause overpickling and pickling effect is general; During independent employing Cathodic pickling, although effect is better, pickling speed is slow, and easily causes the hydrogen embrittlement of workpiece, destroys the mechanical property of workpiece.
For the above-mentioned reasons, the present invention proposes to adopt Variable Polarity pulse pickling control method, by anodic acid pickling being switched in time Cathodic pickling, switching back the over-over mode of anodic acid pickling again after for some time, hydrogen and oxygen are alternately generated at workpiece surface, can not hydrogen be oozed and destroy the mechanical property of workpiece material.
Moreover, adopt Variable Polarity pickling time, in the anodic acid pickling stage, with scale surface aperture, crackle for reactive behavior point place occur electrochemical reaction, oxide skin starts to come off centered by active site, when being switched to the Cathodic pickling stage, reactive behavior point disappear.When next anodic acid pickling stage arrives, forming reactions active site again, and an active site position upper anodic acid pickling stage change.Circulation like this, reactive behavior point dissociates at workpiece surface, and oxide skin dissolution is removed more even, can reduce the roughness of workpiece surface greatly, make the workpiece surface after process more smooth, present metalluster.And when adopting separately anodic acid pickling, reactive behavior point position is tending towards maintaining static, be easy to, in a certain position, overpickling occurs, form corrosion pit, make the workpiece surface after process uneven, roughness increases, and lacks metalluster.
In actual treatment, Variable Polarity pulse parameter, as pulse amplitude, pulse duration, all there is considerable influence to processing efficiency and workpiece performance, wherein the selection of positive-negative polarity impulsive switched frequency directly affects pickling efficiency especially, and the positive-negative polarity pulse duration best in treating processes should be change and revocable.
In the anodic acid pickling stage, anodic scale participates in electrochemical reaction, with speed dissolving faster, generates near anode simultaneously
with
ignore convection current and electromigratory effect, these ions in the liquid phase mass transfer process depend on diffusion, but when not adding external force, the limited use of diffusion.Along with the carrying out of time, will produce concentration polarization phenomenon, above-mentioned ionic concn raises, and will reduce the speed of reaction of the oxidized dissolving of oxide compound.Therefore, thinking of the present invention be resultant ion aggregation near the anode to a certain extent so that when producing concentration polarization phenomenon and reduce the speed of reaction of the oxidized dissolving of oxide compound, be switched to the Cathodic pickling stage in time, will
with
convert Fe to
3+and Cr
3+, the hydrogen simultaneously generated continues to produce mechanically peel effect to oxide skin.After Cathodic pickling carries out for some time, when
with
be consumed to low concentration even complete reaction time, again switch back the anodic acid pickling stage, now do not have concentration polarization phenomenon, the dissolution rate of oxide skin returns to higher state, so circulates, and just can obtain using than simple the pickling speed that anode electrolysis is higher.Meanwhile, the negative electrode time length is short, and hydrogen and oxygen alternately generate at workpiece surface, can not ooze hydrogen, destroy the mechanical property of material.
Fig. 3 is typical anodic polarization curves, and the AB section in Fig. 3 is anode dissolution district, generates without gas; BC section anode voltage is just becoming, and electric current declines, and represents that metal starts passivation; CD section is for stablize passive state; DE section raises with anode voltage, and current density rises again, and metal dissolves with high price form, and in solution, aerobic is separated out; EF section is secondary passivity district; FG section is secondary trans-passive region, now may occur new electrode reaction.
Along with the generation of oxygen in anodic acid pickling preliminary process, workpiece surface oxide skin dissolution speed is very fast, anode voltage (i.e. the voltage at workpiece two ends) is positioned at DE interval, after concentration polarization extremely to a certain degree, in addition oxygen bubbles makes anode voltage raise in the attachment of workpiece surface, anode voltage will be crossed E point and enter secondary passivity district, and the passive film that surface is formed hinders the dissolving of oxide skin further, thus makes pickling speed slack-off.Therefore, best treating processes is: due to the impact of concentration polarization, in the anodic acid pickling stage when anode voltage is close to anode voltage (above-mentioned first threshold can be slightly less than anode voltage corresponding to E point) that E point is corresponding, timely control power-supply system changes output polarity, switch to the Cathodic pickling stage, eliminate concentration polarization phenomenon, after continuing to carry out the Cathodic pickling of for some time, switch to the next anodic acid pickling stage, make the dissolution rate of workpiece surface oxide skin return to higher state.
When negative electrode and anode all hang described workpiece, when anode workpiece carries out anodic acid pickling, cathode-workpiece is then in the Cathodic pickling stage; After polarity switches, when cathode-workpiece carries out anodic acid pickling, anode workpiece is then in the Cathodic pickling stage.So, then can while guarantee oxide skin be dissolved with higher dissolution rate all the time, the hydrogen that negative electrode produces fully " can drive " oxygen bubbles that the anodic acid pickling stage is attached to workpiece surface away, thus improve pickling effect, reduce the hydrogen embrittlement of material, reduce the roughness of the rear workpiece surface of process, remove oxide skin and " the poor layers of chrome " of workpiece surface thoroughly, make the condition of surface of workpiece better adapt to next process.
Due in actual mechanical process, cannot determine that anode voltage rises to the moment boundary of E point accurately, namely above-mentioned first threshold is difficult to accurately determine, therefore the present invention also provide with dynamic resistance velocity of variation level off to zero moment for boundary, accurately determine the dipole inversion time further.
As shown in Figure 4, in a kind of embodiment, described electrical feature information comprises voltage and the dynamic resistance velocity of variation of described output, and described dynamic resistance velocity of variation can be determined in conjunction with the voltage of output and electric current; The polarity switching judging of Variable Polarity pulse, realizes on-line control by following method, makes workpiece alternately be in optimum anodic acid pickling and Cathodic pickling stage:
S21, when described workpiece carries out anodic acid pickling, detects the voltage signal at described workpiece two ends and flows through the current signal of workpiece;
Concrete, detected the voltage signal at workpiece two ends by Hall voltage sensor in real time, flowed through the current signal of workpiece by Hall current sensor Real-time Collection;
The anode voltage value detected in real time compares with first threshold by S22, when judging whether described anode voltage value is more than or equal to first threshold, if so, enters S23;
S23 utilizes described voltage and current signal to calculate anode dynamic resistance velocity of variation;
Concrete, according to Ohm's law, namely by the voltage signal of Real-time Collection divided by current signal determination anode differential resistance values, more described anode dynamic resistance velocity of variation can be determined by the variable quantity of differential resistance values in the unit time;
Whether the anode dynamic resistance velocity of variation described in S24 real-time judge approaches zero gradually, if so, enters S25;
Power-supply system is exported pulse and changes negative polarity into by straight polarity by S25, makes described workpiece switch to Cathodic pickling by anodic acid pickling; Meanwhile, detect the voltage signal at workpiece two ends in real time by the way described in S21 and flow through the current signal of workpiece;
The cathode voltage detected in real time compares with first threshold by S26, when judging whether described cathode voltage is more than or equal to first threshold, if so, enters S27;
S27 utilizes described voltage and current signal to calculate negative electrode dynamic resistance velocity of variation;
Concrete, according to Ohm's law, namely by the voltage signal of Real-time Collection divided by current signal determination negative electrode differential resistance values, more described negative electrode dynamic resistance velocity of variation can be determined by the variable quantity of unit time inner cathode differential resistance values;
Whether the negative electrode dynamic resistance velocity of variation described in S28 real-time judge approaches zero gradually, if so, enters S29;
Power-supply system is exported pulse and is changed to positive polarity by negative polarity by S29, makes described workpiece switch to anodic acid pickling by Cathodic pickling;
Afterwards, circulation S21-S29 step, makes workpiece hocket anodic acid pickling and Cathodic pickling, until acid cleaning process terminates.
As follows by the concrete case of the switching instant of aforesaid method determination anodic acid pickling and Cathodic pickling:
Acid electrolyte is: concentration is the Na of 150g/L
2sO
4and concentration is the HNO of 60g/L
3.
Adopt symmetrical Variable Polarity Square-wave AC to carry out electrolytic pickling to workpiece, negative electrode, anode workpiece are the 304 stainless steel hot-rolling plates being of a size of 4cm × 4cm × 0.4cm, the parallel placement of negative electrode, anode workpiece, and spacing is 50mm, and current density is 60A/dm
2, under room temperature, process 2min.
Keep other conditions constant, only change negative electrode, anodic pulse frequency, the electrical characteristic waveform in the different frequency acid cleaning process of acquisition, as shown in Figure 5.Fig. 5 (a) medium frequency f is 100Hz, Fig. 5 (b) medium frequency f is 250Hz, Fig. 5 (c) medium frequency f is 500Hz, in Fig. 5 (a), Fig. 5 (b), Fig. 5 (c), transverse axis is time t, unit millisecond (ms); The longitudinal axis is respectively voltage U, and its unit is volt (V) and resistance R, and its unit is ohm (Ohm).In figure, voltage waveform has similar rule, and at initial stage (2 ~ 3ms) the voltage substantially constant of pulse, account for voltage remained unchanged substantially in this stage, and the dissolution rate of oxide skin maintains high value; Afterwards due to the impact of concentration polarization, oxide skin dissolution speed declines, and workpiece surface starts to enter secondary passivity district, makes workpiece current potential raise further.Equally, dynamic resistance curve also keeps similar rule, and rise with larger velocity of variation at initial stage (2 ~ 3ms) dynamic resistance of pulse, after rising to certain level, resistance change rate levels off to zero.If by aforesaid method, then can determine to ensure preferably pickling effect, the optimum frequency of Variable Polarity pulse is 250Hz.
Shown in actual workpiece surface treatment effect Fig. 6, as shown in Figure 6, under current flow density, during the same treatment time, frequency is good than other frequency bands of the pickling effect of the Variable Polarity Square-wave AC of 250Hz, and oxide skin removal amount is many, surfacing, has metalluster, and this and above-mentioned conclusion are coincide.
Find in practical application, best polarity switching frequency and current density have comparatively Important Relations, and the frequency-current density plot obtained by above-mentioned way as shown in Figure 7, can be used for actual cleanup acid treatment process parameters.
In sum, Variable Polarity pulse pickling control method of the present invention, by the anodic acid pickling that replaces and Cathodic pickling process, avoids workpiece material generation Hydrogen Brittleness Phenomena, improves pickling effect, improve pickling efficiency.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (5)
1. a Variable Polarity pulse pickling control method, is characterized in that, comprise the steps:
When workpiece being placed in acid electrolyte and carrying out pickling, detect the electrical feature information of described workpiece in real time;
Judge whether described electrical feature information meets polarity switching condition:
If meet, then change the polarity that power-supply system exports pulse, make described workpiece switch to anodic acid pickling by Cathodic pickling or switch to Cathodic pickling by anodic acid pickling.
2. Variable Polarity pulse pickling control method according to claim 1, it is characterized in that, described electrical feature information comprises: the voltage at workpiece two ends, dynamic resistance velocity of variation.
3. Variable Polarity pulse pickling control method according to claim 2, it is characterized in that, the process obtaining described electrical feature information comprises:
Detected the voltage signal at workpiece two ends by Hall voltage sensor in real time, flowed through the current signal of workpiece by Hall current sensor Real-time Collection;
Utilize described voltage signal divided by described current signal determination differential resistance values, determine described dynamic resistance velocity of variation by the variable quantity of differential resistance values in the unit time.
4. Variable Polarity pulse pickling control method according to claim 2, is characterized in that, judges that the process whether described electrical feature information meets polarity switching condition comprises:
The magnitude of voltage detected in real time is compared with first threshold, judges whether described magnitude of voltage is more than or equal to first threshold;
When magnitude of voltage reaches first threshold, judge whether described dynamic resistance velocity of variation approaches zero gradually.
5. Variable Polarity pulse pickling control method according to claim 1, it is characterized in that, when carrying out anodic acid pickling, described magnitude of voltage is anode voltage value, described dynamic resistance velocity of variation is anode dynamic resistance velocity of variation, when carrying out Cathodic pickling, described magnitude of voltage is cathode voltage, and described dynamic resistance velocity of variation is negative electrode dynamic resistance velocity of variation.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111266678A (en) * | 2020-02-21 | 2020-06-12 | 苏州大学 | Method for strengthening mass transfer efficiency in electrolytic machining micro-gap based on cathodic hydrogen evolution and control system |
| CN111690977A (en) * | 2019-03-13 | 2020-09-22 | 上海梅山钢铁股份有限公司 | Electrode plate polarity switching control method of electrolytic cleaning tank in strip steel production process |
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| CN111690977A (en) * | 2019-03-13 | 2020-09-22 | 上海梅山钢铁股份有限公司 | Electrode plate polarity switching control method of electrolytic cleaning tank in strip steel production process |
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| CN111266678A (en) * | 2020-02-21 | 2020-06-12 | 苏州大学 | Method for strengthening mass transfer efficiency in electrolytic machining micro-gap based on cathodic hydrogen evolution and control system |
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