CN104849203A - Device and method for testing electrochemical repassivation performance of metal material - Google Patents
Device and method for testing electrochemical repassivation performance of metal material Download PDFInfo
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- CN104849203A CN104849203A CN201510263039.7A CN201510263039A CN104849203A CN 104849203 A CN104849203 A CN 104849203A CN 201510263039 A CN201510263039 A CN 201510263039A CN 104849203 A CN104849203 A CN 104849203A
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Abstract
The invention relates to a device and a method for testing the electrochemical repassivation performance of a metal material, and belongs to the technical field of corrosion simulation experiments and transient electrochemical testing. The device mainly comprises a vacuum-tight box, a driving motor, a belt drive system, a rotary suction disc, an abrasive material fixedly arranged on the rotary suction disc, a metal sample clamp, a rotary cylinder, a horizontal translation cylinder, a vertical translation cylinder, a water bath system, a three-electrode electrochemical testing system. The testing process is carried out in an oxygen-free protection atmosphere environment in the vacuum-tight box, an oxidation film is removed from the surface of a passive metal sample by the abrasive material fixedly arranged on the rotary suction disc, then the sample is quickly soaked into a test solution, and the process of repassivating the exposed surface of metal from which a passive film is removed is monitored. According to the device and the method, different corrosion environments can be provided for testing the electrochemical repassivation performance of the surface of the film-free metal. An experiment result is true, stable and reliable, the automation degree of the operation is high, and the device is convenient to maintain and has an experiment standardization prospect.
Description
Technical field
The invention belongs to corrosion simulated experiment and transient state Electrochemical Measurement Technology field, be specifically related to a kind of metal inactivating performance proving installation and experimental technique again.Be applicable to test the electrochemical parameter of the fresh surface passivated membrane growth course without film of different metal, and the simulation of different corrosion environment can be realized.
Technical background
The passivity that passive metal (metal and the alloy thereof such as Fe, Cr, Ti, Al) shows is the metal-oxide film of the densification owing to there is one deck thin (nm level or μm level) on its surface, is referred to as passivating film.This layer of fine and close passivating film can hinder metal to contact with the direct of corrosion environment effectively, thus metallic matrix and corrosion environment is completely cut off.However, in the engineer applied of reality, be subject to the effect of mechanics or chemistry, passivation film easily deforms, dissolve and thinningly even to break, thus make metallic matrix corrosion dissolution.Meanwhile, the metal base surface of fresh exposure may form the passivating film that one deck has protective nature again, i.e. the passivation again (process) of metal.So metal again inactivating performance will determine passive metal generation local corrosion, stress corrosion, corrosion fatigue, the thermodynamic tendency of erosion corrosion and dynamic process.
The inactivating performance again of metal material is by carrying out transient state electrochemistry experiment to measure to the metal surface of fresh exposure.Metal surface due to fresh exposure has very high electrochemical activity, and therefore metal surface can in very short time (10 ~ 10
2ms) passivating film of very thin (nm rank) can just again be formed and covering metal is surperficial in, thus stop the contact of metal and etchant solution, show higher corrosion stability, and corresponding electrochemical source of current is from maximum value rapid decay to metastable value, the passivating process again of Here it is metal.For this feature of passivation again, passivation is again studied and first needs to remove the original oxide film of surface of metal electrode fast, in aqueous environment, then carry out electrochemical measurement fast characterize, be i.e. galvanochemistry transient measuring.The domestic and international research method to metal passivation again has at present: Rapid stretching Strain Method (Engseth P, Scully J C.
corrosion Science1975,15 (6): 505-519.) by applying strain on electrode, because oxide film Toughness Ratio parent metal is poor, therefore oxide film first breaks, thus matrix is exposed in corrosive medium passivating process again occurs, but the method has carried out serious plastic yield to test electrode, improve the electrochemical activity of metal electrode, change the electrochemical properties of test electrode, simultaneously for film rupture position with exposed area is unpredictable and manipulation; Needle point Rapid Scratch Technique method (Burstein G T, Newman R C.
electrochimica Acta, 1980,25 (8): 1009-1013.) and on flat metal, mark one cut by adamas point of a knife fast, thus reach destruction matrix surface oxide film object, but on the regional area of scoring position, there is comparatively large elastic-plastic deformation; Indentation method (Fushimi K, Takase K, Azumi K, et al..
electrochimica acta, 2006,51 (7): 1255-1263.) and be metal surface under the pressure of insulation needle point, oxide film occurs to destroy or break, and exposes the metallic matrix under film, and the method exists the elastic-plastic deformation impact larger on metallic matrix equally.The sharing problem that above-mentioned experimental technique exists is: carry out at effects on surface removing in the process of passivating film, the surface exposed in advance in fact with corrosion environment, passivation reaction again occurs, and the passivating process again on the surface of follow-up exposure not yet starts.Such as Rapid stretching Strain Method or indentation method, as long as film rupture, then passivation just starts to occur, and so now stretches and not to terminate or pressure head does not also leave surface; And for example needle point Rapid Scratch Technique method, along with streaking of needle point, metallic matrix is exposed to etchant solution gradually.Therefore metal exposes without the priority on film surface the degree of passivation again that result in exposed surface and successively differs, thus causes measuring and obtain real passivation electrochemical signals again, is difficult to realize quantitative evaluation metal inactivating performance again.The elastic-plastic deformation caused in order to avoid mechanical means and open-assembly time sequence problem, laser ablation method (Sakairi M, Kinjyo M, Kikuchi T. Electrochimica Acta, 2011,56 (4): 1786-1791.) propose to adopt superlaser to carry out ablation removal to metal oxide film.But but introduce another unavoidable problem, namely while removal oxide film, matrix is under laser irradiation, and the regional area of high temperature easily produces re cast layer, this will fundamentally change, and metal material is original surrounds and watches institutional framework and inactivating performance again.
In sum, prior art is for removing virgin metal surface passivated membrane thus obtain mainly containing without film surface process Problems existing of fresh exposure: large elastic-plastic deformation change electrochemical activity, exposed surface area uncontrollable, more uncertain, the re cast layer change metal of passivating process start time surround and watch institutional framework and inactivating performance again.These problems for the real passivation transient state process again of understanding metal material and accurate evaluation metal again inactivating performance bring restriction.Therefore, need one to forgo above-mentioned deficiency, automatically controlled, use and simply measure accurately real metal inactivating performance proving installation again.
Summary of the invention
The object of the present invention is to provide a kind of metal inactivating performance proving installation and use the method for testing of this device again.This device is by the many deficiencies in the past method of improvement, greatly reduce the elastic-plastic deformation of test metal surface, the metal surface area exposed can be accurately controlled, whole exposure contact corrosion simultaneously medium makes passivation initial state more same, can realize the electrochemical signals test in metallic surface passivating film under different corrosion environment or oxide growth process, and under passivating film removal condition completely, Measurement accuracy can be carried out to the passivating process again of the passivating film that metal surface regenerates.
Technical solution problem of the present invention technical scheme used is:
The proving installation of metal material galvanochemistry of the present invention inactivating performance again, comprise and be fixed on closed box on base and drive motor, belt drive system connects the axle of drive motor and rotating suction disc, and axle is fixed on the left wall of closed box by bearing and outer axle bed, and abrasive material is fixed on rotating suction disc; Vacuum pump is fixed on outside closed box, access closed box and rotating suction disc, and gas admittance valve also accesses closed box; Sample installing port is offered in specimen holder one end, and the other end is fixed on rotary cylinder, and rotary cylinder is fixed on horizontal dynamic air cylinder free end, and horizontal dynamic air cylinder is fixed on vertical translation cylinder free end, and vertical translation cylinder is fixed on the rear wall of closed box; Electrolytic cell is inner at closed box, and is positioned in water bath with thermostatic control system; Test button is as working electrode, and platinized platinum connects platinum filament as auxiliary electrode, and saturated calomel electrode is passed through salt bridge insert experiment solution thus formed three electric systems, and three electrodes are electrically connected to outside electro-chemical test instrument by wire.
Further, closed box top is bolted gland bonnet, and at the contact position of gland bonnet and closed box, rubber weather strip is installed, vacuum pump and gas admittance valve all access the arranged on left and right sides wall of closed box, oxygen probe is installed between vacuum pump and closed box, rain glass is installed between gas admittance valve and closed box, ensures to reach certain vacuum condition in seal box, meet experiment demand, controlled hypoxemia vacuum environment to be formed.
Further, then passivation proving installation, rotating suction disc is equipped with centralized positioning screw, platen, O type rubbery flat gasket circle, mounting O-shaped O-ring seal on the joint face of bearing and closed box, the joint face of outer axle bed and axle installs rotating seal ring.
Further, passivation proving installation again, also be included in insulcrete fixing on closed box right side wall and conducting metal post, saturated calomel electrode, electrochemical metal sample, platinized platinum wire are bolted and realize electrical connection on conducting metal posts inside and outside casing, to ensure to form corrosion electrochemistry test loop.
Further, sample is fixed by fixture and screw, and the surface of test button is stretched in electrolytic cell after solution, and distance liquid level is no less than 3cm, marks scale mark, with the time of immersion test solution quick after Control Assay surface removal passivating film at electrolytic cell sidewall.
The present invention also provides a kind of metal passivation method of testing again, and the method adopts proving installation of the present invention to carry out metal oxide film removal and carries out electrochemistry experiment, comprises the following steps:
Step 1, sample pre-grinding: vertical translation cylinder Control Assay moves to extreme higher position, open drive motor, after rotatory vacuum sucker stabilization of speed, rotary cylinder by fixture rotate to level, specimen surface just to the abrasive material on rotating suction disc, under the promotion of horizontal dynamic air cylinder, sample contacts abrasive material starts pre-grinding, after the time is determined in lasting pre-grinding, horizontal dynamic air cylinder Control Assay leaves abrasive material, and drive motor quits work; Change abrasive material and repeat pre-grinding step, until reach required surfaceness; From fixture installing port, take out sample, sample cleaning is dried up for subsequent use.
Step 2, Preparatory work of experiment: sample is installed according to mounting means during pre-grinding, the wire of sample, platinized platinum, saturated calomel electrode is connected respectively to the conducting metal post on insulcrete, realize electrical connection, closed box also adopts wire to be connected to additional electro-chemical test instrument from different conducting metal post respectively outward; In electrolytic cell, inject solution reach more than scale mark, namely test button immersion solution rear surface distance liquid level is not less than 3cm, and regulates three electrode position; Inject water in water bath, jointly realize water bath with thermostatic control by thermopair and temperature sensor; Press play button, automatically start to vacuumize, open gas admittance valve and be filled with protective atmosphere in closed box, controlled oxygen stable content is not extremely higher than 0.001% vol., and air pressure remains on normal pressure 0.1MPa.
Step 3, Inactivation experiment again: start drive motor, after motor speed to be driven is stable, cylinder moving is controlled by during pre-grinding sample, make sample contacts abrasive material, write down the time starting to grind simultaneously, after grinding proceeds to the schedule time, close drive motor power supply, level of control translation cylinder is moved horizontally to the stroke other end, rotary cylinder relative level line is rotated down 90 °, i.e. specimen surface parallel solution liquid level, open electro-chemical test order to start to record electric signal, vertical translation vertical cylinder drops to minimum point, to guarantee that sample immerses solution and can carry out electrochemical signals measurement, after electrochemical measurement terminates, stop electro-chemical test order, vertical translation cylinder rises to peak, and sample leaves test solution, completes test experiments, takes out sample, according to measuring the electrochemical signals obtained, analyzing passivation transient state process again, obtaining metal inactivating performance again.
Further, described test button is electrically connected with wire, and with insulating material and encapsulant encapsulation sample, insulating material is selected from teflon heat-shrink tube, and encapsulant is selected from epoxy resin.
Further, described wire is the wire of other material of copper conductor or good conductivity.
Further, described protective atmosphere adopts high pure nitrogen or high-purity argon gas.
Further, the switch of described drive motor, vacuum pump, oxygen probe, rotary cylinder, vertical translation cylinder, horizontal dynamic air cylinder, gas admittance valve, temperature sensor, thermopair is controlled by separate relay, each relay and the outside gas circuit control integration of each cylinder are in control box, then the manipulation key on connection control case, wherein motor speed, oxygen content, temperature can transform into digital signal display by ADC.
Compared with prior art, the invention has the beneficial effects as follows:
1, the proving installation of passivation more of the present invention, a face of electrode is only exposed after sealing owing to adopting sample, whole electrode surface is all polished, therefore milling area can accurately be measured and control, the roughness of lapped face can be controlled by abrasive grade, so solve the uncontrollable technical matters of area; Owing to carrying out under the protective atmosphere of the anaerobic of whole experimentation in closed box, grinding environment and corrosion test environment separation, therefore avoid the technical matters that passivation again occurs in process of lapping; When grinding in addition, the rotating speed of rotating suction disc is controlled by drive motor, the normal pressure of the air pressure Control Assay of horizontal dynamic air cylinder, sample can be made to be in low strain rate and low-stress state, the elastic-plastic deformation of metal exposed surface is decreased to can ignore, solve large elastic-plastic deformation intensifier electrode surface electrochemistry this technical matters active, thus guarantee the sample validity of Inactivation experiment result and the property assessed again.
2, the proving installation of passivation more of the present invention, drive motor, vacuum pump, oxygen probe, gas admittance valve, rotary cylinder, horizontal dynamic air cylinder, vertical translation cylinder, thermopair, the switch of temperature sensor is by Control, and be integrated in control box, independently can be controlled each parts by the button on manipulation plate, and wherein motor speed, oxygen content, temperature can transform into digital signal display by ADC, complete experimentation to be completed by the coordinated remote control of each parts, improve again accuracy and the controllability of Inactivation experiment, the property assessed of experimental result.
3, passivation method of testing more of the present invention, due to rotary cylinder, horizontal dynamic air cylinder, vertical translation cylinder Control Assay moves in closed cabin, can ensure that the surperficial parallel solution liquid level of fresh exposure immerses solution, namely the passive state again of specimen surface is consistent, solves the uncertain technical matters of passivation time starting point again; Electro-chemical test instrument electrical connection three-electrode system, before signal record starts from sample contacts solution, electrode surface contact solution reacts and triggers electrochemical signals generation, the result measured can quantitative calculation and analysis, guarantee the validity of Inactivation experiment result again and the property assessed, react the ability of sample passivation more truely and accurately.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.Wherein base 1, drive motor 2, closed box 3, belt drive system 4, vacuum pump 5, oxygen content probe 6, axle 7, bearing 8, outer axle bed 9, rotating suction disc 10, gland bonnet 11, bolt 12, rubber weather strip 13, platen 14, O type rubbery flat gasket circle 15, abrasive material 16, test button 17, fixture 18, rotary cylinder 19, vertical translation cylinder 20, horizontal dynamic air cylinder 21, rain glass 22, gas admittance valve 23, insulcrete 24, conducting metal post 25, saturated calomel electrode wire 26, test button wire 27, platinized platinum wire 28, lid 29, saturated calomel electrode 30, salt bridge 31, platinized platinum 32, solution 33, electrolytic cell 34, temperature sensor 35, water bath 36, thermopair 37, dotted portion is the position that cylinder moving to test button immerses that solution carries out electrochemical measurement, in figure, arrow mark is rotation or the direction of motion of cylinder.
Fig. 2 is rotating suction disc working portion structural representation.Wherein closed box 3, belt drive system 4, axle 7, bearing 8, outer axle bed 9, rotating suction disc 10, platen 14, O type rubbery flat gasket circle 15, sand paper 16, rotating seal ring 38, O RunddichtringO 39, centralized positioning screw 40, internal gas passageways 41.
Fig. 3 is the side view of specimen holder, test button 17, fixture 18, encapsulant 42, insulating material 43, screw 44.
Embodiment
It is as follows that the invention will be further described in conjunction with the accompanying drawings and embodiments:
As shown in Figure 1, the proving installation of passivation more of the present invention, comprise and be fixed on closed box 3 on base 1 and drive motor 2, belt drive system 4 connects the axle 7 of drive motor 2 and rotating suction disc 10, axle is fixed on the left wall of closed box 3 by bearing 8 and outer axle bed 9, and abrasive material 16 is fixed on rotating suction disc 10; Vacuum pump 5 is fixed on outside closed box 3, access closed box 3 and rotating suction disc 10 air flue, and gas admittance valve 23 also accesses closed box 3; Sample installing port is offered in specimen holder 18 one end, and the other end is fixed on rotary cylinder 19, and rotary cylinder 19 is by being fixed on horizontal dynamic air cylinder 21, and horizontal dynamic air cylinder 21 is fixed on vertical translation cylinder 20, and vertical translation cylinder 20 is fixed on closed box 3 rear wall; Electrolytic cell 34 is in closed box, and be positioned in water bath with thermostatic control system, test button 17 is as working electrode, platinized platinum 32 connects platinum filament as auxiliary electrode, saturated calomel electrode 30 accesses testing liquid 33 by salt bridge 31 and forms three electric systems, and three electrodes are electrically connected outside electro-chemical test instrument by wire.
As depicted in figs. 1 and 2, those skilled in the art, can be made into metal of the present invention passivation proving installation again by following operation.On the base 1 of metal enclosed case 3, chosen position settles drive motor 2 and vacuum pump 5, one end of belt drive system 4 is connected with the rotating shaft of drive motor, the other end is connected with the welding axle 7 of rotating suction disc 10, perforate on closed box 3, and be weldingly connected with bearing 8 outer, axle 7 is through closed box 3 and by bearing 8, outer axle bed 9 is fixed, gas passage 41 is left in axle 7 and rotating suction disc 10, rotating suction disc 10 center mounting center dog screw 40, rotating suction disc 10 and platen 14 are by being threaded, mounting O-shaped rubbery flat gasket circle 15 on rotating suction disc 10, at bearing 8 and closed box 3 endoporus junction mounting O-shaped O-ring seal 39, rotating seal ring 38 is installed between axle 7 and outer axle bed 9, two exhaust tubes of vacuum pump 5 access the gas passage 41 in closed box 3 sidewalls and axle 7, and gas admittance valve 23 accesses closed box 3 sidewall on opposite, fixed vertical translation cylinder 20 on closed box 3 sidewall adjacent with rotating suction disc 10, horizontal dynamic air cylinder 21 is arranged on the free end of vertical translation cylinder 20, rotary cylinder 19 is arranged on the free end of horizontal dynamic air cylinder 21, sample installing port is offered in specimen holder 18 one end, other end perforate, be fixed on the axle of rotary cylinder 19, sample can realize vertical movement, moves horizontally and action that relative level line is rotated down and resets, fitting insulating panels 24 on closed box 3 sidewall, conducting metal post 25 is through insulcrete 24, closed box 3 inside arranges water bath 36 and annular-heating thermopair 37, electrolytic cell 34 is placed in water bath 36, and be provided with lid 29, lid upper shed reserves three electrode position and temperature sensor 35 position, three electrodes and temperature sensor 35 stretch in electrolytic cell 34, the wire be connected with three electrodes through being fixed on metal column 25 both sides, and is connected with outside electro-chemical test instrument, gland bonnet 11 and rubber weather strip 13 are equipped with in closed box 3 top, and have bolt 12 to fix in surrounding.
The switch of drive motor 2, vacuum pump 5, oxygen probe 6, rotary cylinder 19, vertical translation cylinder 20, horizontal dynamic air cylinder 21, gas admittance valve 23, thermopair 37, temperature sensor 35 controls by separate relay; Each relay and the outside gas circuit of each cylinder control all to be integrated in independent control box, realize controlling separately to action each in closed box 3 by the manipulation plate on control box, and wherein motor speed, oxygen content, temperature can transform into digital signal display by ADC.
During use, in electrolytic cell 34, load solution 33 to be measured, according to test needs, water can be injected in water bath 36, by the real-time constant temperature water bath of thermopair 37 heating and temperaturel sensor 35; Ready test button 17(working electrode to be measured) be installed on fixture 18, platinum electrode 32(auxiliary electrode) be fixed on electrolytic cell lid, saturated calomel electrode 30(contrast electrode) connect solution by salt bridge 31, adjust three electrodes to correct position; Three electrode wires are connected respectively to the conducting metal post 25 on insulcrete 18, and closed box also adopts wire to be connected on additional electro-chemical test instrument from different conducting metal post 25 respectively outward; Abrasive material 16 central hole, is mounted on rotating suction disc 10 by centralized positioning screw 40 and platen 14; Cover closed cover 11, and be fixed on edge by bolt 12; Open vacuum pump 5 power supply, start to bleed in casing, and make abrasive material 16 be close to rotating suction disc 10, open gas admittance valve 23 and be filled with protective atmosphere (high pure nitrogen or high-purity argon gas), by the oxygen content in oxygen probe 6 and rain glass 22 difference Real-Time Monitoring closed box 31 and force value, oxygen content is stablized to not higher than 0.001% vol., and pressure remains on normal pressure (0.1MPa) to start to carry out sample experiment; Control vertical translation cylinder 20 and move to extreme higher position at stroke, horizontal dynamic air cylinder 21 moves to right-hand member, fixture 18 rotates to level by rotary cylinder 19, at this moment, sample 17 is just in the face of abrasive material 16 but do not contact, open drive motor 2 power supply, drive motor 2 driven rotary sucker 10 and abrasive material 16 rotate, after rotatory vacuum sucker stabilization of speed, level of control translation cylinder 21 promotes sample contacts abrasive material, writes down duration of contact simultaneously, after striping process proceeds to the time set, be generally 30s-60s, can from top seal lid observation striping situation; Level of control translation cylinder 21 is moved horizontally to stroke end, closes drive motor 2 power supply, closes vacuum pump 5 power supply, gas admittance valve 23; Control rotary cylinder 19 relative level line and be rotated down 90 °, i.e. sample 17 surperficial parallel solution 33 liquid level, open electro-chemical test order to start to record electric signal, control vertical translation cylinder 20 and vertically drop to minimum point, at this moment sample immerses solution, as the position of dotted portion in Fig. 1, sample 17 immerses the moment of solution 33, start to carry out again passivation reaction electrochemical signals to measure, after electrochemical measurement terminates, stop the order of electro-chemical test instrument; Vertical translation cylinder 20 rises to peak, and sample leaves test solution, opens closed box and takes out sample, closing control case power supply.
Experimentally measure the signal obtained, carry out passivation analysis of transient process again, thus quantitative evaluation is carried out to the again inactivating performance of this metal material in corresponding corrosion environment.
It is more than the implementation process of infrastest mode of the present invention, as can be seen from above-mentioned implementation process, sample 17 is embedded in encapsulant 42 and insulating material 43, only expose a face of electrode, whole electrode surface all contacts abrasive material 16, and the roughness of lapped face can be controlled by abrasive grade, therefore striping area can accurately be measured and control; Owing to carrying out under the protective atmosphere of the anaerobic of whole experimentation in closed box 3, striping environment is separated with corrosion environment, compared to the mode of carrying out surperficial striping in the solution that prior art adopts, the mode that striping environment is separated with corrosion environment avoids the problem that passivation again occurs in striping process, thus ensure that the validity of experimental result; In addition in striping process, the rotating speed of rotating suction disc 10 is controlled by controlling drive motor 2, the normal pressure of the air pressure Control Assay of horizontal dynamic air cylinder 21, sample can be made to be in low strain rate and low-stress state, compare other mechanical striping mode existing, in the present invention, the elastic-plastic deformation of metal exposed surface is decreased to and can ignores, and guarantees the validity of sample Inactivation experiment result again; Sample 17 specimen surface parallel solution under the control of cylinder immerses solution, ensure the consistance of specimen surface passive state again, and can by the truly complete passivating process again of electrochemical measurement instrument record, measurement result can be used as quantitative calculation and analysis, ensure that the validity of Inactivation experiment result again and the property assessed, be conducive to the passivation ability again reflecting metal material more truely and accurately.
During enforcement, gland bonnet 11 is fixed by bolt 12 at closed box 3 top, and installs rubber weather strip 13 between gland bonnet 11 and closed box 3, ensures the impermeability of top interface; Vacuum pump 5 and gas admittance valve 23 all access the arranged on left and right sides wall of closed box 3, oxygen probe 6 is installed between vacuum pump 5 and closed box 3, rain glass 22 is installed between gas admittance valve 23 and closed box 3, ensure control in real time the oxygen content in closed box 3 and atmospheric pressure value and monitor, thus improve accuracy and the feasibility of experiment.
Sand paper is located and is fixed on rotating suction disc by centralized positioning screw 40 and platen 14, the inner air flue 41 of rotating suction disc connects vacuum pump 5, mounting O-shaped rubbery flat gasket circle 15, improves impermeability, ensure that abrasive material can be close to sucker in striping process, improve the surface quality of buck and striping; O RunddichtringO 39 is installed on the joint face place of bearing 8 and closed box 3, and rotating seal ring 38 is installed on outer axle bed 9 and the joint face of axle 7, ensures the axle flexible rotating through closed box and closed box self impermeability.
For ensureing that three-electrode system can be wired to the electro-chemical test instrument outside casing, ensure the accuracy of closed box impermeability and measurement electrochemical signals simultaneously, fitting insulating panels 24 and conducting metal post 25 on the right wall of closed box 3, saturated calomel electrode wire 26, test button wire 27 and platinized platinum wire 28 are bolted on conducting metal post 25 inside and outside casing, thus realize electrical connection.During enforcement, adopt hot-melt sealant to fix in the junction of insulcrete and closed box, insulcrete and conducting metal post, conducting metal post is provided with screw thread, and wire is fixed on conducting metal post by bolt.
For ensureing that the surface of test button is stretched in electrolytic cell after solution, distance liquid level is no less than 3cm, demarcates the liquid level of electrolytic cell, makes fixture front plan distance liquid level be 3cm, marks scale mark at electrolytic cell sidewall.During enforcement, sample 17 is fixed on fixture 18 by bolt 44, and sample stretches out fixture, and after immersing solution, specimen surface distance liquid level is no less than 3cm, thus guarantees the accuracy that electro-chemical test is tested and the property assessed.
Adopt the above-mentioned test unit of passivation again to carry out the test of passivation again, comprise the following steps:
Step 1, sample pre-grinding: vertical translation cylinder 20 Control Assay moves to extreme higher position, open drive motor 2, after rotatory vacuum sucker 10 stabilization of speed, fixture 18 rotates to level by rotary cylinder 19, sample 17 surface just to the abrasive material 16 on rotating suction disc 10, under the promotion of horizontal dynamic air cylinder 21, sample 17 contacts abrasive material 16 and starts pre-grinding, after the pre-time consuming continuing to determine, horizontal dynamic air cylinder 21 Control Assay 17 leaves abrasive material 16, and drive motor 2 quits work; Change abrasive material and repeat pre-grinding step, until reach required surfaceness; From fixture 18 installing port, take out sample, sample 17 cleaning is dried up for subsequent use.
Step 2, Preparatory work of experiment: sample 17 is installed according to mounting means during pre-grinding, the wire 26,27,28 of sample, platinized platinum, saturated calomel electrode is connected respectively to the conducting metal post 25 on insulcrete 24, the outer wire that also adopts of closed box 3 is connected to additional electro-chemical test instrument from different conducting metal post 25 respectively; In electrolytic cell 34, inject solution 33 reach more than scale mark, namely test button 17 immerses solution 33 rear surface distance liquid level and is not less than 3cm, and regulates three electrode position; Inject water in water bath 36, jointly realize water bath with thermostatic control by thermopair 37 and temperature sensor 35; Press play button, automatically start in closed box 3 to vacuumize, open gas admittance valve 23 and be filled with high pure nitrogen or high-purity argon gas protective atmosphere; open oxygen probe 6, monitoring oxygen content, atmospheric pressure value monitored by rain glass 22; controlling oxygen content stablizes to not higher than 0.001% vol., and air pressure remains on normal pressure 0.1MPa.
Step 3, Inactivation experiment again: start drive motor 2, after motor 2 stabilization of speed to be driven, cylinder moving is controlled by during pre-grinding sample, sample 17 is made to contact abrasive material 16, write down the time starting to grind simultaneously, after grinding proceeds to the schedule time, close drive motor 2 power supply, level of control translation cylinder 21 is moved horizontally to the stroke other end, rotary cylinder 19 relative level line is rotated down 90 °, i.e. sample 17 surperficial parallel solution 33 liquid level, open electro-chemical test order to start to record electric signal, vertical translation cylinder 20 vertically drops to minimum point, to guarantee that sample 17 immerses solution 33 and carries out electrochemical signals measurement, after electrochemical measurement terminates, stop electro-chemical test order, vertical translation cylinder 20 rises to peak, and sample 17 leaves test solution, completes test experiments, takes out sample 17, according to measuring the electrochemical signals obtained, analyzing passivation transient state process again, obtaining metal inactivating performance again.
For ensure three-electrode system test validity, the tie point of sample and the sample back side and wire by encapsulant epoxy sealing and insulating material teflon heat-shrink tube, to the front of exposing sample; The tie point of platinum electrode and wire is by the coated sealing of silicon rubber; Simultaneously for ensureing the precise acquisition of the signal of electro-chemical test, in experiment, all wires are other materials of copper conductor or good conductivity.Avoid other signal disturbing electrochemical measurements, improve the validity of experimental result.
On the whole, each building block of the proving installation of passivation more of the present invention, interrelated technically, use cooperatively interacts.Because the switch of drive motor 2, vacuum pump 5, oxygen probe 6, rotary cylinder 19, vertical translation cylinder 20, horizontal dynamic air cylinder 21, gas admittance valve 23, temperature sensor 35, thermopair 37 controls by separate relay, and be integrated in control box.During enforcement, can be completed by manipulation plate button and the independence of each parts is controlled and coordinated action, motor speed, oxygen content, bath temperature can transform into digital signal display by ADC, greatly improve the controllability of Inactivation experiment again, the validity of experimental result and the property assessed.
Claims (10)
1. metal material galvanochemistry inactivating performance proving installation again, comprise and be fixed on closed box (3) on base (1) and drive motor (2), belt drive system (4) connects the axle (7) of drive motor (2) and rotating suction disc (10), it is characterized in that, axle (7) is fixed on closed box (3) Zuo Bishang by bearing (8) and outer axle bed (9), and abrasive material (16) is fixed on rotating suction disc (10); Vacuum pump (5) is fixed on closed box (3) outward, access closed box (3) and rotating suction disc (10), and gas admittance valve (23) also accesses closed box (3); Sample installing port is offered in specimen holder (18) one end, the other end is fixed on rotary cylinder (19), rotary cylinder (19) is fixed on horizontal dynamic air cylinder (21) free end, horizontal dynamic air cylinder (21) is fixed on vertical translation cylinder (20) free end, and vertical translation cylinder (20) is fixed on closed box (3) rear wall; Electrolytic cell (34) is inner at closed box (3), and be positioned in water bath with thermostatic control system, test button (17) is as working electrode, platinized platinum (32) connects platinum filament as auxiliary electrode, saturated calomel electrode (30) forms three electric systems by salt bridge (31) insert experiment solution (33), and three electrodes are electrically connected outside electro-chemical test instrument by wire.
2. proving installation according to claim 1, it is characterized in that, described closed box (3) top is by bolt (12) fixing seal lid (11), and between gland bonnet (11) and closed box (3), rubber weather strip (13) is housed, vacuum pump (5) and gas admittance valve (23) all access the arranged on left and right sides wall of closed box (3), oxygen probe (6) is installed between vacuum pump (5) and closed box (3), rain glass (22) is installed between gas admittance valve (23) and closed box (3).
3. proving installation according to claim 1, it is characterized in that, centralized positioning screw (40), platen (14), O type rubbery flat gasket circle (15) rotating suction disc (10) be equipped with, O RunddichtringO (39) is installed on the joint face of bearing (8) and closed box (3), and rotating seal ring (38) is installed on the joint face of outer axle bed (9) and axle (7).
4. proving installation according to claim 1, it is characterized in that, fixed insulation plate (24) and conducting metal post (25) on closed box (3) right wall, saturated calomel electrode wire (26), test button wire (27), platinized platinum wire (28) are bolted and realize electrical connection on conducting metal posts (25) inside and outside casing.
5. proving installation according to claim 1, it is characterized in that, test button (17) is fixed by fixture (18) and screw (44), and the surface of test button (17) to be stretched in electrolytic cell after solution, distance liquid level is no less than 3cm, marks scale mark at electrolytic cell (34) sidewall.
6. adopt the device according to any one of claim 1-5 to carry out again the method for inactivating performance test, it is characterized in that, comprise the following steps:
Step 1, sample pre-grinding: vertical translation cylinder Control Assay moves to extreme higher position, open drive motor, after rotatory vacuum sucker stabilization of speed, rotary cylinder by fixture rotate to level, specimen surface just to the abrasive material on rotating suction disc, under the promotion of horizontal dynamic air cylinder, sample contacts abrasive material starts pre-grinding, after the time is determined in lasting pre-grinding, horizontal dynamic air cylinder Control Assay leaves abrasive material, and drive motor quits work; Change abrasive material and repeat pre-grinding step, until reach required surfaceness; From fixture installing port, take out sample, sample cleaning is dried up for subsequent use;
Step 2, Preparatory work of experiment: sample is installed according to mounting means during pre-grinding, the wire of sample, platinized platinum, saturated calomel electrode is connected respectively to the conducting metal post on insulcrete, realize test button to be electrically connected with wire, closed box also adopts wire to be connected to additional electro-chemical test instrument from different conducting metal post respectively outward; In electrolytic cell, inject solution reach more than scale mark, namely test button immersion solution rear surface distance liquid level is not less than 3cm, and regulates three electrode position; Inject water in water bath, jointly realize water bath with thermostatic control by thermopair and temperature sensor; Press play button, automatically start to vacuumize, open gas admittance valve and be filled with protective atmosphere in closed box, controlled oxygen stable content is not extremely higher than 0.001% vol., and air pressure remains on normal pressure 0.1MPa;
Step 3, Inactivation experiment again: start drive motor, after motor speed to be driven is stable, cylinder moving is controlled by during pre-grinding sample, make sample contacts abrasive material, write down the time starting to grind simultaneously, after grinding proceeds to the schedule time, close drive motor power supply, level of control translation cylinder is moved horizontally to the stroke other end, rotary cylinder relative level line is rotated down 90 °, i.e. specimen surface parallel solution liquid level, open electro-chemical test order to start to record electric signal, vertical translation vertical cylinder drops to minimum point, to guarantee that sample immerses solution and can carry out electrochemical signals measurement, after electrochemical measurement terminates, stop electro-chemical test order, vertical translation cylinder rises to peak, and sample leaves test solution, completes test experiments, takes out sample, according to measuring the electrochemical signals obtained, analyzing passivation transient state process again, obtaining metal inactivating performance again.
7. according to method of testing according to claim 6, it is characterized in that, the described test button described in step 2 is electrically connected with between wire, with insulating material and encapsulant encapsulation sample, insulating material is selected from teflon heat-shrink tube, and encapsulant is selected from epoxy resin.
8. according to the method for testing described in claim 6 or 7, it is characterized in that, described wire is the wire of other materials of copper conductor or good conductivity.
9. according to method of testing according to claim 6, it is characterized in that, the switch of drive motor (2), vacuum pump (5), oxygen probe (6), rotary cylinder (19), vertical translation cylinder (20), horizontal dynamic air cylinder (21), gas admittance valve (23), temperature sensor (35), thermopair (37) is controlled by separate relay, each relay and the outside gas circuit control integration of each cylinder are in control box, then the manipulation key on connection control case, wherein motor speed, oxygen content, temperature transform into digital signal display by ADC.
10. according to method of testing according to claim 6, it is characterized in that, the protective atmosphere described in step 2 is high pure nitrogen or high-purity argon gas.
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