CN1080333A - A kind of electrolytic etching method of metal test-piece - Google Patents
A kind of electrolytic etching method of metal test-piece Download PDFInfo
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- CN1080333A CN1080333A CN 92112290 CN92112290A CN1080333A CN 1080333 A CN1080333 A CN 1080333A CN 92112290 CN92112290 CN 92112290 CN 92112290 A CN92112290 A CN 92112290A CN 1080333 A CN1080333 A CN 1080333A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/02—Etching
Abstract
The present invention relates to a kind of electrolytic etching method of metal test-piece, belong to physics of metals research method field.The present invention is development and the innovation on traditional electropolishing and carbide electrolytic separation technical foundation.The present invention selects power supply, electrolytic solution, electrowinning process, matting and designs, make its method have electrolytic solution and can be common to steel and cast iron, the etch depth of sample sightingpiston can be controlled arbitrarily, multiple phase can show simultaneously, can extract some carbide, phase separately, and non-metallic inclusion, specimen preparation success ratio height, speed is fast, the advantage that electrolytic solution can be repeatedly used.Can be used for the preparation of test button, be specially adapted to scanning electron microscope analysis.
Description
The present invention relates to a kind of electrolytic etching method of metal test-piece, belong to physics of metals research method field.
Up to now, chemical corrosion method is all adopted in the deep corrosion of cast iron sample both at home and abroad.This method is to soak tens hours in 10～20% the hydrochloride alcohol sample in concentration, through cleaning and drying treatment, observes for scanning mirror then.The shortcoming of this method is that etching time is long, and the degree of depth of required etch is restive; Sample cleans difficulty, often have a large amount of halogenide on the surface of tissue that comes out or phase and pollute, so the success ratio of specimen preparation is very low; The space pattern that can only more clearly show some specific phase (being mingled with as graphite) is difficult to the constitutional features of clear demonstration metallic matrix simultaneously; Etching solution uses once promptly to be scrapped.Adopt electropolishing and traditional electrolysis corroding method to solve some mechanical polishing or the very preparation of the alloy sample of difficulty of chemical corrosion both at home and abroad, this method can only be carried out shallow degree etch and be shown in the dark scope of metaloscope, and electrolytic solution and specific technological specification thereof can't satisfy the needs of the very big high resolution scanning electrolysis observation analysis of the depth of field.Therefore, the observation analysis of the three-dimensional appearance of the intragranular of metallic matrix and crystal boundary is subjected to the specimen preparation technology limitation in the steel, is difficult to so far realize.
The objective of the invention is to overcome the deficiency of prior art and provide a kind of electrolytic solution can be common to steel and cast iron, the etch depth of test button sightingpiston can be controlled arbitrarily, multiple phase can show simultaneously, can extract some carbide, phase and non-metallic inclusion separately, specimen preparation success ratio height, the electrolytic etching method of metal test-piece that electrolytic solution can be repeatedly used.
The present invention is achieved in that this electrolytic etching method of metal test-piece finishes through sample correct grinding or polishing, plain conductor connection, reserved window processing, electrolytic etching, sample cleaning, seasoning, removal insulating cover layer operation.Plain conductor connect mode of connection in the operation be sample as anode, stainless steel is as negative electrode.All smeared thick melt paraffin of 0.1～0.3mm or insulating resin by etch surface (window) specimen surface and sample lead exposed part of drawing in addition in the reserved window treatment process.After above-mentioned operation, sample is put into known dc electrolysis device carry out electrolytic etching.The prescription of electrolytic solution is in the electrolyzer: hydrochloric acid 5～15%, distilled water 85～95%, thiocarbamide 3～5g.The electrolytic etching processing parameter is: 0 ℃～room temperature of temperature, voltage 3～12V, anodic current density 0.01～0.10A/cm
2, the shallow mordanting time of steel is 30～150 seconds, and the deep corrosion etch time of steel is 4～10 minutes, and the shallow mordanting time of cast iron is 5～15 minutes, and the deep corrosion etch time of cast iron is 30～70 minutes; The graphite extraction time is 6～8 hours in the cast iron.Test button after the electrolytic etching operation enters matting, and the cleaning step of matting with the distillation washing, cleans through ethanol, acetone subsequently for cleaning in 2～6% ethanol solution hydrochloride 20～40 seconds earlier again.Sample after the cleaning is peeled off the removal insulating cover layer subsequently by its seasoning.After above-mentioned operation, test button is promptly made.
The present invention compared with prior art has electrolytic solution can be common to steel and cast iron, the etch depth of test button sightingpiston can be controlled arbitrarily, multiple phase can show simultaneously, can extract some carbide, phase and non-metallic inclusion separately, specimen preparation success ratio height, the advantage that electrolytic solution can be repeatedly used.
The used technical process of the present invention is identical with known technical process, so omit process flow diagram.
The present invention is described in further detail below in conjunction with accompanying drawing (embodiment):
The electrolytic etching of metal etching method is finished through sample correct grinding or polishing, plain conductor connection, reserved window processing, electrolytic etching, sample cleaning, seasoning, removal insulating cover layer operation.In sample correct grinding or polishing process, should be to the specimen surface that carries out shallow degree etch through conventional polished finish, the specimen surface of deep-etch is only needed polish with medium-grained abrasive paper for metallograph.If the observation degree of depth of sample only limits to surperficial several crystal grain, also should carry out polishing in advance.Plain conductor connect mode of connection in the operation be sample as anode, stainless steel is as negative electrode.All smeared thick melt paraffin of 0.1mm or insulating resin by etch surface (window) specimen surface and sample lead exposed part of drawing in addition in the reserved window treatment process.After above-mentioned operation, sample is put into known dc electrolysis device carry out electrolytic etching.The prescription of electrolytic solution is in the electrolyzer: hydrochloric acid 8%, distilled water 92%, thiocarbamide 3.5g.The electrolytic etching processing parameter is: 0 ℃～room temperature of temperature, voltage 3～12V, anodic current density 0.01～0.10A/cm
2, the shallow mordanting time of steel is 30～150 seconds, and the deep corrosion etch time of steel is 4～10 minutes, and the shallow mordanting time of cast iron is 5～15 minutes, and the deep corrosion etch time of cast iron is 30～70 minutes; The graphite extraction time is 6～8 hours in the cast iron; Test button after the electrolytic etching operation enters matting, and the cleaning step of matting is to clean 25 seconds in 4% ethanol solution hydrochloride earlier, with the distillation washing, cleans through ethanol, acetone more subsequently.The time of cleaning in distilled water, ethanol, acetone is accustomed to carrying out routinely.Sample after the cleaning is peeled off the removal insulating cover layer subsequently by its seasoning.After above-mentioned operation, test button is promptly made.Above-mentioned each operation is applicable to the sample electrolytic etching of cast iron and steel.
Embodiment one:
Ferrite crystal grain shows (Fig. 1) in the steel.
The electrolytic etching method of test button as mentioned above.Wherein 2 ℃ of electrolysis temperatures, voltage 8V, anodic current density 0.03A/cm
2, the etch time is 150 seconds.Owing to kept the Fe3Cm film of ferrite crystal boundary, the clear ferrite crystal grain pattern that has shown shallow degree etch.
Embodiment two:
Ferrite crystal grain shows (Fig. 2) in the steel.
The electrolytic etching method of test button as mentioned above.Wherein 2 ℃ of electrolysis temperatures, voltage 8V, anodic current density 0.03A/cm
2, the etch time is 10 minutes.Owing to kept the Fe3Cm film of ferrite crystal boundary, the clear ferrite crystal grain three-dimensional appearance that has shown deep-etch.
Embodiment three:
Steel Medium pearlite crystal grain shows (Fig. 3).
The electrolytic etching method of test button as mentioned above.Wherein 4 ℃ of electrolysis temperatures, voltage 10V, anodic current density 0.05A/cm
2, the etch time is 40 seconds.Fig. 3 has shown the hypereutectoid steel annealed structure, the perlite of the different synusia of an austenite crystal position, and austenite grain boundary is Fe3C
II
Embodiment four:
Steel Medium pearlite crystal grain shows (Fig. 4).
The electrolytic etching method of test button as mentioned above.Wherein 4 ℃ of electrolysis temperatures, voltage 10V, anodic current density 0.05A/cm
2, the etch time is 5 minutes.Fig. 4 has shown sample after deep corrosion, the eutectoid steel annealed state, different synusia position to two pearlitic grains.
Embodiment five:
A kind of lower bainite (Fig. 5) in the quenching attitude hypoeutectoid steel.
The electrolytic etching method of test button as mentioned above.Wherein 4 ℃ of electrolysis temperatures, voltage 8V, anodic current density 0.03A/cm
2, the etch time is 150 seconds.Fig. 5 has shown that supersaturation α-Fe is leaf of bamboo shape, and the thorn-like Fe2.4C of parallel growth is separated out at the edge, has more clearly shown the pattern of tissue.
Embodiment six:
The typical organization (Fig. 6) of ferrite China ink cast iron laser quench-hardened case.
The electrolytic etching method of test button as mentioned above.Wherein 0 ℃ of electrolysis temperature, voltage 12V, anodic current density 0.10A/cm
2, the etch time is 30 minutes.Fig. 6 more clearly reflects the globular graphite feature of annular sclerosis band tissue on every side.
Embodiment seven:
The graphite of extraction is mingled with (Fig. 7,8) separately.
The electrolytic etching method of test button as mentioned above.Wherein electrolysis temperature is room temperature, voltage 12V, anodic current density 0.10A/cm
2, the etch time is 8 hours.Fig. 7 has shown the quasiflake graphite eutectic cell that of independent extraction is more complete; Fig. 8 has shown a globular graphite of independent extraction.
Claims (3)
- A kind of electrolytic etching method of metal test-piece is finished through sample correct grinding or polishing, plain conductor connection, reserved window processing, electrolytic etching, sample cleaning, seasoning, removal insulating cover layer operation, it is characterized in that:(1) all smeared thick melt paraffin of 0.1～0.3mm or insulating resin by etch surface (window) specimen surface and sample lead exposed part of drawing in addition in the reserved window treatment process;
- (2) electrolyte prescription in the electrolytic etching operation is: hydrochloric acid 5～15%, distilled water 85～95%, thiocarbamide 3～5%; Electrolytic process parameter is: 0 ℃～room temperature of temperature, voltage 3～12V, anodic current density 0.01～0.10A/cm 2, the shallow mordanting time of steel is 30～150 seconds, and the deep corrosion etch time of steel is 4～10 minutes, and the shallow mordanting time of cast iron is 5～15 minutes, and the deep corrosion etch time of cast iron is 30～70 minutes, the graphite extraction time is 6～8 hours in the cast iron;
- (3) cleaning step of sample matting is for cleaning in 2～6% ethanol solution hydrochloride 20～40 seconds earlier.With the distillation washing, clean through ethanol, acetone more subsequently.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92112290 CN1080333A (en) | 1992-10-06 | 1992-10-06 | A kind of electrolytic etching method of metal test-piece |
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| CN 92112290 CN1080333A (en) | 1992-10-06 | 1992-10-06 | A kind of electrolytic etching method of metal test-piece |
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| CN1080333A true CN1080333A (en) | 1994-01-05 |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1049257C (en) * | 1994-09-12 | 2000-02-09 | 北京科技大学 | Superfine etching method for stainless steel |
| CN100593706C (en) * | 2007-03-29 | 2010-03-10 | 上海大学 | Method for extracting steel superfine varia by electrolysis method |
| CN101655426B (en) * | 2009-09-16 | 2011-02-16 | 北京科技大学 | Electrochemical metallographic etching method universal for nickel-based alloys |
| CN101216477B (en) * | 2008-01-04 | 2011-06-22 | 莱芜钢铁股份有限公司 | In situ quantitative determination method for large-sized metallic inclusion |
| CN102517623A (en) * | 2012-01-13 | 2012-06-27 | 武汉大学 | Method for extracting oxide film from steel material |
| CN102965719A (en) * | 2011-08-30 | 2013-03-13 | 西部数据（弗里蒙特）公司 | Low-rate electrochemical etch of thin film metals and alloys |
| CN103451714A (en) * | 2013-09-09 | 2013-12-18 | 昆山奥德鲁自动化技术有限公司 | Electrochemical renovation treatment technology for cutting tool |
| CN103526276A (en) * | 2005-05-30 | 2014-01-22 | 株式会社爱发科 | Surface treatment |
| CN103983501A (en) * | 2014-05-16 | 2014-08-13 | 深圳大学 | Test method and test system for manufacturing metal test specimen with local corrosion in batch |
| CN104805481A (en) * | 2015-03-12 | 2015-07-29 | 中国人民解放军装甲兵工程学院 | Method for remanufacturing 6DL connecting rod by adopting nano brush electroplating |
| CN106048704A (en) * | 2016-08-05 | 2016-10-26 | 广州三孚新材料科技股份有限公司 | Electrolytic etching agent for chromium-zirconium-copper alloy and electrolytic etching method |
| CN108166049A (en) * | 2017-12-18 | 2018-06-15 | 江门职业技术学院 | It is a kind of for the electrolyte of high-entropy alloy and electro-etching processing method |
-
1992
- 1992-10-06 CN CN 92112290 patent/CN1080333A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1049257C (en) * | 1994-09-12 | 2000-02-09 | 北京科技大学 | Superfine etching method for stainless steel |
| CN103526276A (en) * | 2005-05-30 | 2014-01-22 | 株式会社爱发科 | Surface treatment |
| CN100593706C (en) * | 2007-03-29 | 2010-03-10 | 上海大学 | Method for extracting steel superfine varia by electrolysis method |
| CN101216477B (en) * | 2008-01-04 | 2011-06-22 | 莱芜钢铁股份有限公司 | In situ quantitative determination method for large-sized metallic inclusion |
| CN101655426B (en) * | 2009-09-16 | 2011-02-16 | 北京科技大学 | Electrochemical metallographic etching method universal for nickel-based alloys |
| CN102965719B (en) * | 2011-08-30 | 2016-08-10 | 西部数据（弗里蒙特）公司 | The low rate chemical etching of film metal and alloy |
| CN102965719A (en) * | 2011-08-30 | 2013-03-13 | 西部数据（弗里蒙特）公司 | Low-rate electrochemical etch of thin film metals and alloys |
| CN102517623A (en) * | 2012-01-13 | 2012-06-27 | 武汉大学 | Method for extracting oxide film from steel material |
| CN103451714A (en) * | 2013-09-09 | 2013-12-18 | 昆山奥德鲁自动化技术有限公司 | Electrochemical renovation treatment technology for cutting tool |
| CN103983501A (en) * | 2014-05-16 | 2014-08-13 | 深圳大学 | Test method and test system for manufacturing metal test specimen with local corrosion in batch |
| CN104805481A (en) * | 2015-03-12 | 2015-07-29 | 中国人民解放军装甲兵工程学院 | Method for remanufacturing 6DL connecting rod by adopting nano brush electroplating |
| CN106048704A (en) * | 2016-08-05 | 2016-10-26 | 广州三孚新材料科技股份有限公司 | Electrolytic etching agent for chromium-zirconium-copper alloy and electrolytic etching method |
| CN106048704B (en) * | 2016-08-05 | 2018-06-19 | 广州三孚新材料科技股份有限公司 | For the electrolytic etching agent of chrome zirconium copper alloy and electrolytic etching method |
| CN108166049A (en) * | 2017-12-18 | 2018-06-15 | 江门职业技术学院 | It is a kind of for the electrolyte of high-entropy alloy and electro-etching processing method |
| CN108166049B (en) * | 2017-12-18 | 2019-06-28 | 江门职业技术学院 | A kind of electrolyte and electro-etching processing method for high-entropy alloy |
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