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 PDFInfo
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- 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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- electrolyte
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- electrolytic cell
- power supply
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- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000003792 electrolyte Substances 0.000 claims abstract description 46
- 238000000866 electrolytic etching Methods 0.000 claims abstract description 25
- 239000002184 metal Substances 0.000 claims abstract description 25
- 229910052751 metal Inorganic materials 0.000 claims abstract description 25
- 238000005260 corrosion Methods 0.000 claims description 14
- 230000007797 corrosion Effects 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 10
- 239000011347 resin Substances 0.000 claims description 7
- 229920005989 resin Polymers 0.000 claims description 7
- 230000000694 effects Effects 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 5
- 230000004584 weight gain Effects 0.000 claims description 4
- 235000019786 weight gain Nutrition 0.000 claims description 4
- 230000005611 electricity Effects 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000007689 inspection Methods 0.000 claims description 3
- 230000000087 stabilizing effect Effects 0.000 claims description 3
- 239000000284 extract Substances 0.000 claims 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000005192 partition Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000007799 cork Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UOFGSWVZMUXXIY-UHFFFAOYSA-N 1,5-Diphenyl-3-thiocarbazone Chemical compound C=1C=CC=CC=1N=NC(=S)NNC1=CC=CC=C1 UOFGSWVZMUXXIY-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000000712 assembly Effects 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011982 device technology Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 239000005341 toughened glass Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; 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
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).
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CN201811291195.4A CN109387420A (en) | 2018-10-31 | 2018-10-31 | A kind of metallographic sample preparation electrolyzing and corroding device and method |
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CN201811291195.4A CN109387420A (en) | 2018-10-31 | 2018-10-31 | A kind of metallographic sample preparation electrolyzing and corroding device and method |
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Cited By (1)
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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2018
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Application publication date: 20190226 |