CN105954187B - A kind of the thin liquid film corrosion electrochemical test system and method for controllable thickness of liquid film - Google Patents

A kind of the thin liquid film corrosion electrochemical test system and method for controllable thickness of liquid film Download PDF

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CN105954187B
CN105954187B CN201610523157.1A CN201610523157A CN105954187B CN 105954187 B CN105954187 B CN 105954187B CN 201610523157 A CN201610523157 A CN 201610523157A CN 105954187 B CN105954187 B CN 105954187B
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liquid film
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electrochemical
electrode
thickness
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CN105954187A (en
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李晓刚
柳伟
齐小龙
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University of Science and Technology Beijing USTB
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Abstract

The present invention provides the thin liquid film corrosion electrochemical test system and method for a kind of controllable thickness of liquid film, belongs to the humidity corrosion simulated experiment including atmospheric corrosion and Electrochemical Measurement Technology field.The device is made of the part such as lifting controller, lifting column, objective table, ammeter, electrode catheter, liquid-level controller, experiment container, sample table, specimen holder, temp probe, water-bath, level meter, electrochemical test system and horizontal adjustment bolt.By adjusting coarse adjustment and the accurate adjustment knob of lifting controller, the accurate control to aqueous solution liquid level position in experiment container is realized, to obtain the thin liquid film thickness set within 1000 μm.Meanwhile thermostatic control is carried out to solution in experiment container and electrochemical sample using water-bath.Using the thin liquid film of device acquisition setting thickness and in conjunction with external electrochemical test system, the corrosion electrochemistry test of setting thickness of liquid film condition is carried out.

Description

A kind of the thin liquid film corrosion electrochemical test system and method for controllable thickness of liquid film
Technical field
It is special the present invention relates to the corrosion simulated experiment of the thin liquid film including atmospheric corrosion and Electrochemical Measurement Technology field Do not refer to the thin liquid film corrosion electrochemical test system and method for a kind of controllable thickness of liquid film.
Background technique
Thin liquid film existing for metal material surface can make metal material that thin liquid film electrochemical corrosion, thin liquid film electrochemistry occur Corrosion is one of corrosion phenomenon extremely common in nature and industrial environment, and it is rotten that atmospheric corrosion belongs to a kind of typical thin liquid film Erosion.The temperature difference of metal material and environment in wet gas environments can cause the moisture in moisture to condense shape in metal material surface At certain thickness thin liquid film, when thin liquid film film thickness reaches the above thickness of tens water molecule layers, it is anti-to have electrochemistry It answers occurrence condition and thin liquid film electrochemical corrosion occurs.With the variation of ambient humidity and temperature etc., the thin liquid of metal material surface Film thickness also correspondingly changes, the variation of this thin liquid film thickness will affect diffusion of the corrosive media in thin liquid film from And corrosion electrochemistry process is had an impact, for example, atmospheric corrosion behavior is with thin liquid film thickness, there are close relationships, usually recognize Corrosion to generate with a thickness of 1000 μm of liquid films below is thin liquid film corrosion.Further investigation and understanding metal material are Bu Tong thin Corrosion electrochemical action and mechanism under thickness of liquid film, and then thin liquid film corrosion is effectively controlled with important theoretical value and reality Border meaning.
In traditional corrosion electrochemistry test method, usually the established thin liquid film thickness of metal material surface is carried out Measurement, and lack and accurately effectively control the device and method for forming specific thin liquid film thickness, therefore metal material thin liquid film corrodes Electro-chemical test receives a degree of limitation.The thin liquid film corrosion electrochemistry that the present invention provides a kind of controllable thickness of liquid film is surveyed Device and method is tried, can be in the thin liquid film of metal material surface acquisition setting thickness using the device, and it is thin to carry out specific thicknesses Corrosion electrochemistry test under the conditions of liquid film.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of tests of the thin liquid film corrosion electrochemistry of controllable thickness of liquid film to fill It sets and method.
A kind of thin liquid film corrosion electrochemical test system of controllable thickness of liquid film, it is characterised in that: including accurate adjustment knob, branch Support, electrode catheter one, electrode catheter two, ammeter, water-bath, objective table, accurate adjustment lifting column, aqueous solution, annular platinum electrode, Coarse adjustment knob, lifting controller, liquid-level controller, coarse adjustment lifting column, transparent observing lid, temp probe, blow vent, experiment are held Device, horizontal adjustment bolt, sample table, electrochemical sample conducting wire, solid state reference electrode conducting wire, screw, annular platinum electrode, specimen holder Tool, level meter, solid state reference electrode, electrochemical sample;Keep sample table holding horizontal by adjusting horizontal adjustment bolt, is testing A certain amount of aqueous solution is added in container, liquid level is carried out by the coarse adjustment knob and accurate adjustment knob that adjust lifting controller It adjusts.The circuit being made up of electrode catheter and ammeter, can make the initial position of liquid level and sample be in same level;So Afterwards, it by adjusting the coarse adjustment knob and accurate adjustment knob of lifting controller, adjusts coarse adjustment lifting column and accurate adjustment lifting column enters in water Depth and increase liquid level, thus electrochemical sample surface obtain setting thickness thin liquid film;Experiment container top has transparent Observation lid and small size blow vent had not only kept communicating but also can reducing solution moisture content testing evaporation inside experiment container with ambient atmos; Experiment container is internally provided with sample table, is provided with temp probe above sample table, the sample on sample table and external electrification Test macro is learned to be connected.
Further electrochemical sample draws electrochemical sample conducting wire, and solid state reference electrode draws solid state reference electrode conducting wire, Annular platinum electrode draws annular platinum electrode wire, and electrochemical sample conducting wire, solid state reference electrode conducting wire, annular platinum electrode wire are logical It draws in crossed beam trunking hole.
Further electrode catheter one and electrode catheter two are fixed on liquid-level controller inner sidewall, electrode catheter one and sample table Face is in same level, and electrode catheter two is under liquid level arbitrarily fixed position, electrode catheter one and electrode catheter two and electricity Flow table forms circuit;The aqueous solution initial position being put into experiment container is between electrode catheter one and electrode catheter two, is led to Overregulate coarse adjustment knob and the accurate adjustment knob on lifting controller adjust respectively coarse adjustment lifting column and accurate adjustment lifting column decline Distance increases the height of liquid level in experiment container;When ammeter pointer just deflects, and show circuit is in channel status, The liquid level of solution is in and specimen surface same level in liquid-level controller and experiment container.
Using the method for above-mentioned apparatus observing and controlling thin liquid film thickness, it is characterised in that: according to thin liquid film thickness control formula h1s1 +h2s2=h3(s'3+s”3), by adjust lifting controller coarse adjustment knob and accurate adjustment knob come control coarse adjustment lifting column decline away from From h1, accurate adjustment lifting column dropping distance h2, and then obtain the thickness value h of electrochemical sample surface liquid film3;To improve thickness of liquid film Value h3Control precision, it is desirable that liquid-level controller liquid level area S'3With experiment container liquid level area S "3The sum of should be noticeably greater than it is thick Adjust lifting column cross-sectional area S1With accurate adjustment lifting column cross-sectional area S2Value, under the conditions of meeting thin liquid film thickness control formula, In the h for meeting thickness formula condition1And h2In value range, h1Numerical value takes the larger value, h2Numerical value takes smaller value, realizes more accurate Obtain thickness value h3For the thin liquid film within 1000 μm, controls precision and be smaller than 20 μm.
Sample table quadrangle is screwed, and places electrochemical sample, and electrochemical sample is fixed on by specimen holder On sample table, solid state reference electrode and level meter are placed in electrochemical sample side, set outside electrochemical sample, solid state reference electrode Set annular platinum electrode.
Electrochemical sample, annular platinum electrode and solid state reference electrode form three-electrode system.Electrochemical sample draws electrification Sample conducting wire is learned, solid state reference electrode draws solid state reference electrode conducting wire, and annular platinum electrode draws annular platinum electrode wire, electrification Sample conducting wire, solid state reference electrode conducting wire, annular platinum electrode wire is learned to draw by line groove hole.It is realized by water-bath to container The temperature of interior aqueous solution is controlled.
The advantageous effects of the above technical solutions of the present invention are as follows:
In above scheme, is formed by the coarse adjustment and accurate adjustment knob that adjust lifting controller respectively in specimen surface and set thickness The thin liquid film of angle value tests the thin liquid film corrosion electrochemistry of the setting thickness to realize.It is public according to thin liquid film thickness control Formula h1s1+h2s2=h3(s′3+s″3), it is realized using the adjusting of coarse adjustment knob and accurate adjustment knob on lifting controller to sample table The accurate control of face thin liquid film thickness, thickness of liquid film control range are within 1000 μm, and control precision is smaller than 20 μm.
Detailed description of the invention
Fig. 1 is the thin liquid film corrosion electrochemical test system structural schematic diagram of controllable thickness of liquid film of the invention;
Fig. 2 is the area the D enlarged plan view of the device;
Wherein: 1- accurate adjustment knob;2- support frame;3- electrode catheter one;4- electrode catheter two;5- ammeter;6- water-bath; 7- objective table;8- accurate adjustment lifting column;9- aqueous solution;10- annular platinum electrode wire;11- coarse adjustment knob;12- lifting controller; 13- liquid-level controller;14- coarse adjustment lifting column;15- transparent observing lid;16- temp probe;17- blow vent;18- experiment container; 19- horizontal adjustment bolt;20- sample table;21- electrochemical sample conducting wire;22- solid state reference electrode conducting wire;23- screw;24- ring Shape platinum electrode;25- specimen holder;26- level meter;27- solid state reference electrode;28- electrochemical sample.
Specific embodiment
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, below in conjunction with attached drawing and tool Body embodiment is described in detail.
The present invention provides the thin liquid film corrosion electrochemical test system and method for a kind of controllable thickness of liquid film.
As shown in Figure 1, the device includes accurate adjustment knob 1, support frame 2, electrode catheter 1, electrode catheter 24, ammeter 5, water-bath 6, objective table 7, accurate adjustment lifting column 8, aqueous solution 9, annular platinum electrode wire 10, coarse adjustment knob 11, lifting controller 12, liquid-level controller 13, coarse adjustment lifting column 14, transparent observing lid 15, temp probe 16, blow vent 17, experiment container 18, level Adjust bolt 19;Sample table 20;Electrochemical sample conducting wire 21;Solid state reference electrode conducting wire 22;Screw 23;24- annular platinum electrode; 25- specimen holder;26- level meter;27- solid state reference electrode, 28- electrochemical sample.Electrode catheter 1 and electrode catheter 24 With ammeter 5, aqueous solution 9 and electric power generating composition circuit.
Fig. 2 is D plot structure schematic diagram in Fig. 1.As shown in Fig. 2, the electrochemical sample 28 prepared is fixed on specimen holder In tool 25, and with the good edge voids of silica gel sealing;Specimen holder is fixed on 20 top of sample table with screw 23.Electricity shown in Fig. 1 Chemistry sample 28 is drawn by electrochemical sample conducting wire 21, and annular platinum electrode 24 is put into the platinum filament wire in 28 outside of electrochemical sample In slot, drawn by annular platinum electrode wire 10.Solid state reference electrode 27 is put into metallic channel and by solid state reference electrode conducting wire 22 It draws.Electrochemical sample 28, annular platinum electrode 24 and solid state reference electrode 27 form three-electrode system.By annular platinum electrode wire 10, electrochemical sample conducting wire 21, solid state reference electrode conducting wire 22 are connected in the electrochemical test system outside device.
It adjusts horizontal adjustment bolt 19 and observes level meter 26 simultaneously, be in a horizontal position specimen surface.Experiment container 18 Middle a certain amount of aqueous solution 9 of injection.The surface of electrode catheter 1 and electrochemical sample 28 is in identical horizontal plane, and electrode is visited Needle 24 is in below the liquid level of liquid-level controller 13.
The coarse adjustment knob 11 and accurate adjustment knob 1 on lifting controller 12 are adjusted respectively, increase coarse adjustment lifting column 14 and accurate adjustment Lifting column 8 in aqueous solution depth and increase liquid level, until ammeter 5 just shows current value, liquid level is in and sample this moment At the identical horizontal plane O in surface.It then proceedes to adjust the coarse adjustment knob 11 and accurate adjustment knob 1 on lifting controller 12, adjusts thick Knob 11 is adjusted to control 14 dropping distance h of coarse adjustment lifting column1, adjusting accurate adjustment knob 1 makes 8 dropping distance h of accurate adjustment lifting column2, make essence 8 bottom surface of lifting column is adjusted to be in Fig. 1 at horizontal plane C, liquid level of solution rises and is in location A in Fig. 1.According to shown in equation 1 Thin liquid film thickness control formula, the thin liquid film on 28 surface of electrochemical sample is at this time with a thickness of setting value h3
h1S1+h2S2=h3(S'3+S"3) (1)
In above formula, S1For 14 cross-sectional area of coarse adjustment lifting column;S2For 8 cross-sectional area of accurate adjustment lifting column;S'3For liquid level Liquid level area in controller 13;S"3For the liquid level area in experiment container 18;h1For 14 dropping distance of coarse adjustment lifting column;h2For essence Adjust 8 dropping distance of lifting column;h3For liquid level climb, i.e. thin liquid film thickness value in liquid-level controller and experiment container 18.It is logical Coarse adjustment knob 11 and accurate adjustment knob 1 on lifting controller 12 are overregulated to control 14 dropping distance h of coarse adjustment lifting column1, accurate adjustment 8 dropping distance h of lifting column2, and then the thickness of liquid film value h set3.In order to improve thickness of liquid film h3Control precision, it is desirable that S'3With S "3The sum of be noticeably greater than S1And S2Value, under the conditions of meeting thin liquid film thickness control formula 1, should take biggish coarse adjustment liter Column h drops1Value and smaller fine tuning lifting column h2Value.The above method can realize the thin liquid film for obtaining and setting thickness within 1000 μm of thickness, And control precision is smaller than 20 μm.
Aqueous temperature in experiment container 18 is controlled using water-bath 7, and is held using 16 pairs of experiments of temp probe Aqueous solution 9 and 28 temperature of electrochemical sample measure in device.By transparent observing lid 15 to being seen inside experiment container 18 It examines.
The above is a preferred embodiment of the present invention, it is noted that for those skilled in the art For, without departing from the principles of the present invention, several improvements and modifications can also be made, these improvements and modifications It should be regarded as protection scope of the present invention.

Claims (3)

1. a kind of thin liquid film corrosion electrochemical test system of controllable thickness of liquid film, it is characterised in that: including accurate adjustment knob, support It is frame, electrode catheter one, electrode catheter two, ammeter, water-bath, objective table, accurate adjustment lifting column, aqueous solution, annular platinum electrode, thick Adjust knob, lifting controller, liquid-level controller, coarse adjustment lifting column, transparent observing lid, temp probe, blow vent, experiment container, Horizontal adjustment bolt, sample table, electrochemical sample conducting wire, solid state reference electrode conducting wire, screw, annular platinum electrode, specimen holder, Level meter, solid state reference electrode, electrochemical sample;Keep sample table holding horizontal by adjusting horizontal adjustment bolt, holds in experiment A certain amount of aqueous solution is added in device, liquid level is adjusted by the coarse adjustment knob and accurate adjustment knob that adjust lifting controller Section;The circuit being made up of electrode catheter and ammeter, can make the initial position of liquid level and sample be in same level;So Afterwards, it by adjusting the coarse adjustment knob and accurate adjustment knob of lifting controller, adjusts coarse adjustment lifting column and accurate adjustment lifting column enters in water Depth and increase liquid level, thus electrochemical sample surface obtain setting thickness thin liquid film;Experiment container top has transparent Observation lid and small size blow vent had not only kept communicating but also can reducing solution moisture content testing evaporation inside experiment container with ambient atmos; Experiment container is internally provided with sample table, is provided with temp probe above sample table, the sample on sample table and external electrification Test macro is learned to be connected;
Electrochemical sample is placed inside specimen holder, and specimen holder is fixed on above sample table with screw;Electrochemical sample one Solid state reference electrode and level meter are placed in side, and electrochemical sample and the external of solid state reference electrode place annular platinum electrode;
Electrochemical sample draws electrochemical sample conducting wire, and solid state reference electrode draws solid state reference electrode conducting wire, annular platinum electrode Annular platinum electrode wire is drawn, electrochemical sample conducting wire, solid state reference electrode conducting wire, annular platinum electrode wire are drawn by line groove hole Out.
2. the thin liquid film corrosion electrochemical test system of controllable thickness of liquid film according to claim 1, one He of electrode catheter Electrode catheter two is fixed on liquid-level controller inner sidewall, and electrode catheter one and specimen surface are in same level, electrode catheter Two arbitrarily fix position, electrode catheter one and electrode catheter two and ammeter composition circuit under liquid level;It is put in experiment container The aqueous solution initial position entered is between electrode catheter one and electrode catheter two, is revolved by the coarse adjustment adjusted on lifting controller Button and accurate adjustment knob adjust the distance of coarse adjustment lifting column and the decline of accurate adjustment lifting column respectively, increase the height of liquid level in experiment container Degree;When ammeter pointer just deflects, and show circuit is in channel status, solution in liquid-level controller and experiment container Liquid level is in and specimen surface same level.
3. a kind of method using claim 1 described device observing and controlling thin liquid film thickness, it is characterised in that: according to thin liquid film thickness Control formula h1S1+h2S2=h3(S'3+S"3), coarse adjustment is controlled by adjusting coarse adjustment knob and the accurate adjustment knob of lifting controller Lifting column dropping distance h1, accurate adjustment lifting column dropping distance h2, and then obtain the thickness value h of electrochemical sample surface liquid film3;For Improve thickness of liquid film value h3Control precision, it is desirable that liquid-level controller liquid level area S'3With experiment container liquid level area S "3The sum of Greater than coarse adjustment lifting column cross-sectional area S1With accurate adjustment lifting column cross-sectional area S2Value, is meeting thin liquid film thickness control formula Under the conditions of, in the h for meeting thickness formula condition1And h2In value range, h1Numerical value takes the larger value, h2Numerical value takes smaller value, realizes Relatively accurately obtain thickness value h3For the thin liquid film within 1000 μm, precision is controlled less than 20 μm.
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CN106645144B (en) * 2016-09-29 2019-04-12 河海大学常州校区 A kind of flowing liquid membrane generating device and its application method
CN108895971B (en) * 2018-07-05 2024-01-23 北京科技大学 High-precision thin liquid film thickness control forming device and using method
CN109374520B (en) * 2018-11-14 2021-01-15 中车青岛四方机车车辆股份有限公司 Electrochemical test system for atmospheric corrosion of metal under flowing thin liquid film
CN110542648B (en) * 2019-09-29 2024-02-20 福州大学 Electrochemical corrosion experiment system
CN110987783B (en) * 2019-11-22 2021-04-20 北京科技大学 Method and device for fine evaluation of local corrosion/pitting corrosion of metal and alloy
CN112461744B (en) * 2020-10-21 2022-12-23 上海大学 Electrochemical testing device and method for metal failure under liquid film
CN113504174B (en) * 2021-05-24 2022-05-20 上海交通大学 Dynamic temperature difference corrosion testing system and method suitable for various materials

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