CN109387420A - A kind of metallographic sample preparation electrolyzing and corroding device and method - Google Patents

A kind of metallographic sample preparation electrolyzing and corroding device and method Download PDF

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Publication number
CN109387420A
CN109387420A CN201811291195.4A CN201811291195A CN109387420A CN 109387420 A CN109387420 A CN 109387420A CN 201811291195 A CN201811291195 A CN 201811291195A CN 109387420 A CN109387420 A CN 109387420A
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CN
China
Prior art keywords
electrolyte
sample
metallographic
electrolytic cell
power supply
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CN201811291195.4A
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Chinese (zh)
Inventor
胡萌
张晓峰
黄贵祥
李晓超
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No 5719 Factory of PLA
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No 5719 Factory of PLA
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Priority to CN201811291195.4A priority Critical patent/CN109387420A/en
Publication of CN109387420A publication Critical patent/CN109387420A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32Polishing; Etching

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention discloses a kind of metallographic sample preparation electrolyzing and corroding device and methods, including electrolytic cell (1), metal mesh (2), booster pump (9) and power supply (5), cathode plate (8) are provided on the side wall of described electrolytic cell (1) side, cathode plate (8) connects power supply (5) cathode, metal mesh (2) is placed in electrolytic cell (1), power supply (5) anode connection metal mesh (2), electrolyte entrance (10) are provided with below cathode plate (8), electrolyte entrance (10) connects booster pump (9), booster pump (9) connects electrolyte bottle (11) by pipeline, electrolyte outlet (12) are additionally provided on electrolytic cell (1), electrolyte outlet (12) connects electrolyte bottle (11).It is an advantage of the invention that adjusting electrolytic etching voltage parameter in real time in the case where the surface to be checked of sample is focused by metallographic microscope and observed, etch end point is determined so that realization is accurate.

Description

A kind of metallographic sample preparation electrolyzing and corroding device and method
Technical field
The present invention relates to input tax detection device technology field, especially a kind of metallographic sample preparation electrolyzing and corroding device and side Method.
Background technique
.Metallographic sample preparation generally includes cutting sampling, inlaying samples, sample preparation and tissue and judges four steps.Wherein, sample system Standby is to be ground, polished and organized corrosion to carry out tissue judgement after sample is inlayed.The corrosion of metallographic specimen tissue is often divided into Chemical corrosion method and electrolytic etching method.Wherein, electrolytic etching be additional power source make electrode potential high dithizone in yin Pole electric discharge reduction, and electrode potential low relatively active metal betatopic in anode region is oxidized, becoming cation is detached from material surface, Form the corrosion of anode.It is each under weak current effect since current potential is different between crystal grain and crystal boundary between each phase in face to be checked Phase extent of corrosion is different, thus shows that tissue is judged for tissue.But shortcoming is, due to material category difference and criticizes Secondaryization difference, is affected by human factors larger using the corrosive effect of electrolytic etching method, and to prevent sample excessive erosion, is electrolysed Corrosion parameter is usually slight erosion parameter to gradually excessive compared with high corrosion parameter, test process is relatively complicated and etch end point not Can accurately it determine.Patent No. CN102168298B " a kind of use for laboratory metallographic sample electrolyzing and corroding device and electrolytic etching method " A kind of use for laboratory metallographic sample electrolyzing and corroding device is disclosed, including cathode electrolytic cell, electro bath-lid with holes, electrolyte storage Deposit slot, pressure transfusion cork and cathode plate etc..Metallographic sample working face is aligned at electro bath-lid hole and is placed, electrolyte is injected, Pressure transfusion cork is pushed to come into full contact with metallographic sample working face with electrolyte;Using certain voltage and current, work is certain The electrolytic etching to metallographic specimen can be realized in time." live metallographic electrobrightening corrodes instrument to application number CN105714369A Anode cathode device and its application method " provide a kind of anode cathode device of live metallographic electrobrightening corrosion instrument, Include: power supply, anode assemblies, with positive pole circuit connection, be fixed on large-scale workpiece, and with metal lographic examination position point It is spaced apart;Cathode assembly, and power cathode circuit connection, draw after chemical polishing reagent with the metallographic on large-scale workpiece Check portion site is in contact, and after powering on, carries out electrobrightening corrosion to metal lographic examination position point.The patent is mainly existing Electrochemical corrosion is carried out on the large-scale workpiece of field.A kind of patent No. CN202903572U " use for laboratory metallographic sample electrolytic etching dress Set " disclose a kind of use for laboratory metallographic sample electrolyzing and corroding device, including cathode electrolytic cell, electrolyte reserve tank, cathode plate, Partition and manual impeller etc..When described device works, cathode electrolytic cell and electrolyte reserve tank are separated with partition, made in two slots Electrolyte is opposing stationary;When the working clearance, partition is promoted, manual impeller rotation in electrolyte reserve tank is driven, drives in two slots Electrolytic etching liquid forms exchange, keeps the temperature of cathode electrolytic cell Inner electrolysis corrosive liquid and the stabilization of concentration.The patent No. " throw by electrolysis Photoetch instrument " provide a kind of electrobrightening corrosion tester, including anode, cathode, specimen cup, anode cassette, electrolytic bath, coolant liquid And circulating pump, electrolytic bath are set in cooling bath, cooling bath is sealed by cooling down slot cover, is provided with specimen cup, sample in anode cassette Cup is made of plastics, and circulating pump is connected to by another inlet tube with electrolytic bath inner space, and circulating pump passes through inlet tube and sun The inner space of pole box is connected to.Above-mentioned patent all imitate to a certain extent by optimization metallographic specimen electrolytic etching process and raising corrosion Fruit, but the problem of all not can solve accurate judgement etch end point.
Summary of the invention
The purpose of the present invention is to overcome the shortcomings of the existing technology, provides a kind of metallographic sample preparation electrolyzing and corroding device and side Method.
The purpose of the present invention is achieved through the following technical solutions: a kind of metallographic sample preparation electrolyzing and corroding device and method, packet Electrolytic cell, metal mesh, booster pump and power supply are included, cathode plate, cathode plate connection are provided on the side wall of the electrolytic cell side Power cathode, metal mesh are placed in electrolytic cell, and positive pole connects metal mesh, are provided with electrolyte entrance below cathode plate, Electrolyte entrance connects booster pump, and booster pump connects electrolyte bottle by pipeline, is additionally provided with electrolyte outlet on electrolytic cell, electricity Solve liquid outlet connection electrolyte bottle.
Specifically, the metal mesh is L-type.
Specifically, the bottom of the electrolytic cell is transparent glass.
Specifically, voltmeter and adjustable resistance are also in series on the power supply.
Specifically, the bottom of the electrolytic cell is provided with a metallographic microscope.
A kind of metallographic sample preparation electrolytic etching method, includes the following steps;
Prepare before S1, electrolytic etching: sample is embedded in resin mass, after completion is inlayed, sample face to be checked is ground And polishing;Sample surface grinding to be checked and polishing after, by test specimen to inspection be placed on metal mesh downwards;
S2, electrolytic etching: the observation window of sample towards metallographic microscope is placed, and adjusts metallographic microscope until that can focus on examination The surface of sample, starting booster pump is extracted electrolyte out from electrolyte bottle, is flowed into electrolytic cell by electrolyte entrance, to be electrolysed After slot electrolyte inside liquid level stabilizing, startup power supply, adjusting adjustable resistance gradually increases voltage, sees while adjusting adjustable resistance The corrosion condition for examining specimen surface can close power supply after specimen surface crystal grain obviously shows, and stop electrolytic etching.
Specifically, a weight gain counterweight is placed on the resin mass to improve contact effect of the sample with metal mesh.
The invention has the following advantages that
(1) electrolytic etching is accurate, the present invention be the surface to be checked of sample by metallographic microscope focus observe in the case where, Electrolytic etching voltage parameter is adjusted, in real time to realize accurate judgement etch end point.
(2) easy to operate, device structure is simple.
(3) electrolytic etching specimen surface effect is good.Under the action of booster pump, the electrolyte in electrolytic cell is in flowing State, this can take away H from cathode2, and leak water the oxide with property iron and iron from specimen surface band, guarantee that sample obtains Clearly tissue topography.
Detailed description of the invention
Fig. 1 is schematic structural diagram of the device of the invention;
Fig. 2 is that apparatus of the present invention use schematic diagram;
In figure: 1- electrolytic cell, 2- metal mesh, 3- sample, 4- resin mass, 5- power supply, 6- voltmeter, 7- adjustable resistance, 8- cathode Plate, 9- booster pump, 10- electrolyte entrance, 11- electrolyte bottle, 12- electrolyte outlet, 13- weight gain counterweight, 14- observation window, 15- Metallographic microscope.
Specific embodiment
The present invention will be further described with reference to the accompanying drawing, but protection scope of the present invention is not limited to following institute It states.
As shown in Fig. 1~2, a kind of metallographic sample preparation electrolyzing and corroding device and method, including electrolytic cell 1, metal mesh 2, pressurization 9 and power supply 5 are pumped, cathode plate 8 is provided on the side wall of 1 side of electrolytic cell, cathode plate 8 connects 5 cathode of power supply, metal mesh 2 are placed in electrolytic cell 1, and 2 bottom of metal mesh is rounded and is slightly larger than 3 diameter of sample, 5 anode connection metal mesh 2 of power supply, yin The lower section of pole plate 8 is provided with electrolyte entrance 10, and electrolyte entrance 10 connects booster pump 9, and booster pump 9 is connected by pipeline and is electrolysed Liquid bottle 11 is additionally provided with electrolyte outlet 12 on electrolytic cell 1, and electrolyte outlet 12 connects electrolyte bottle 11, so that electrolyte exists It is drawn into electrolytic cell 1 under the action of booster pump 9 from electrolyte bottle 11, and since gravity from outlet 12 flow back into electricity It solves in liquid bottle 11.
Further, the metal mesh 2 is L-type.
Further, the bottom of the electrolytic cell 1 is transparent glass, and the transparent glass is that light transmittance is greater than 90% Quartz glass, organic glass or tempered glass.
Further, voltmeter 6 and adjustable resistance 7 are also in series on the power supply 5, it is ensured that sample 3 when electrolysis It powers on and is pressed in 10V or so.
Further, the bottom of the electrolytic cell 1 is provided with a metallographic microscope 15.
A kind of metallographic sample preparation electrolytic etching method, includes the following steps;
Prepare before S1, electrolytic etching: sample 3 is embedded in resin mass 4, after completion is inlayed, the face to be checked of sample 3 is ground Mill and polishing;The surface grinding to be checked of sample 3 and polishing after, by test specimen 3 to inspection be placed on metal mesh 2 downwards;
S2, electrolytic etching: the observation window 14 of sample 3 towards metallographic microscope 15 is placed, and adjusts metallographic microscope 15 until energy The surface of sample 3 is focused on, starting booster pump 9 is extracted electrolyte out from electrolyte bottle 11, is flowed by electrolyte entrance 10 In electrolytic cell 1, after 1 electrolyte inside liquid level stabilizing of slot to be electrolysed, startup power supply 5, adjusting adjustable resistance 7 gradually increases voltage, The corrosion condition that 3 surface of sample is observed while adjusting adjustable resistance 7, can close after 3 surface microstructure of sample obviously shows Power supply 5 stops electrolytic etching.
Further, a weight gain counterweight 13 is placed on the resin mass 4 to improve contact effect of the sample 3 with metal mesh 2.
The above, only presently preferred embodiments of the present invention not do limitation in any form to the present invention.It is any ripe Those skilled in the art is known, without departing from the scope of the technical proposal of the invention, all using technology contents described above Many possible changes and modifications or equivalent example modified to equivalent change are made to technical solution of the present invention.Therefore, all It is the content without departing from technical solution of the present invention, any change modification made to the above embodiment of technology according to the present invention, Equivalent variations and modification belong to the protection scope of the technical program.

Claims (7)

1. a kind of metallographic sample preparation electrolyzing and corroding device, it is characterised in that: including electrolytic cell (1), metal mesh (2), booster pump (9) and Power supply (5) is provided with cathode plate (8) on the side wall of the electrolytic cell (1) side, and cathode plate (8) connects power supply (5) cathode, Metal mesh (2) is placed in electrolytic cell (1), and power supply (5) anode connection metal mesh (2), cathode plate is provided with electrolyte below (8) Entrance (10), electrolyte entrance (10) connect booster pump (9), and booster pump (9) connects electrolyte bottle (11) by pipeline, electrolytic cell (1) it is additionally provided on electrolyte outlet (12), electrolyte outlet (12) connects electrolyte bottle (11).
2. a kind of metallographic sample preparation electrolyzing and corroding device according to claim 1, it is characterised in that: the metal mesh (2) For L-type.
3. a kind of metallographic sample preparation electrolyzing and corroding device according to claim 1, it is characterised in that: the electrolytic cell (1) Bottom be transparent glass.
4. a kind of metallographic sample preparation electrolyzing and corroding device according to claim 1, it is characterised in that: on the power supply (5) Also it is in series with voltmeter (6) and adjustable resistance (7).
5. a kind of metallographic sample preparation electrolyzing and corroding device according to claim 1, it is characterised in that: the electrolytic cell (1) Bottom be provided with a metallographic microscope (15).
6. the side that metallographic sample preparation electrolyzing and corroding device described in a kind of any one according to claim 1 ~ 5 carries out electrolytic etching Method, it is characterised in that: include the following steps;
Prepare before S1, electrolytic etching: sample (3) is embedded in resin mass (4), after completion is inlayed, by sample (3) face to be checked It is ground and is polished;Sample (3) surface grinding to be checked and polishing after, by test specimen (3) to inspection be placed in gold downwards Belong on net (2);
S2, electrolytic etching: the observation window (14) of sample (3) towards metallographic microscope (15) is placed, metallographic microscope is adjusted (15) until that can focus on the surfaces of sample (3), starting booster pump (9) extracts electrolyte out from electrolyte bottle (11), passes through electricity Solution liquid entrance (10) is flowed into electrolytic cell (1), and after slot (1) electrolyte inside liquid level stabilizing to be electrolysed, startup power supply (5) is adjusted Adjustable resistance (7) gradually increases voltage, the corrosion condition on sample (3) surface is observed while adjusting adjustable resistance (7), wait try Sample (3) surface microstructure can close power supply (5) after obviously showing, and stop electrolytic etching.
7. a kind of metallographic sample preparation electrolytic etching method according to claim 6, it is characterised in that: on the resin mass (4) Weight gain counterweight (13) is placed to improve the contact effect of sample (3) with metal mesh (2).
CN201811291195.4A 2018-10-31 2018-10-31 A kind of metallographic sample preparation electrolyzing and corroding device and method Pending CN109387420A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111912691A (en) * 2020-09-07 2020-11-10 盘锦忠旺铝业有限公司 Automatic change aluminum alloy sample positive pole tectorial membrane device

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JP2011039017A (en) * 2009-08-10 2011-02-24 Chemical Yamamoto:Kk Electrolytic polishing device of sample for analysis
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CN206706243U (en) * 2017-05-05 2017-12-05 辽宁工业大学 Electrolytically and mechanically burnishing device
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Publication number Priority date Publication date Assignee Title
CN111912691A (en) * 2020-09-07 2020-11-10 盘锦忠旺铝业有限公司 Automatic change aluminum alloy sample positive pole tectorial membrane device

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Application publication date: 20190226