CN111910244B - Method for preparing dual-phase stainless steel EBSD sample by pulse wave electrolytic polishing - Google Patents
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- CN111910244B CN111910244B CN202010648265.8A CN202010648265A CN111910244B CN 111910244 B CN111910244 B CN 111910244B CN 202010648265 A CN202010648265 A CN 202010648265A CN 111910244 B CN111910244 B CN 111910244B
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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
- C25F3/16—Polishing
- C25F3/22—Polishing of heavy metals
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- G—PHYSICS
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G01N1/32—Polishing; Etching
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The invention discloses a method for preparing a duplex stainless steel EBSD sample by pulse wave electrolytic polishing, which comprises the steps of adopting a linear cutting method to treat the sample, fixing the linear cutting method by adopting thermal mosaic, grinding the mosaic sample, and mechanically polishing after grinding; preparing perchloric acid, ethylene glycol and ethylene glycol monobutyl ether into electrolytic polishing solution according to the volume ratio of 1:7:1-1:9:2; immersing a duplex stainless steel sample into an electrolytic polishing solution to serve as an anode, wherein a cathode material is ultrapure ferrite stainless steel, and performing anode pulse wave electrolytic polishing by using an electrochemical workstation or a pulse voltage output device; the electrolytic polishing is performed for 1-2 s under the condition that the pulse wave voltage is 22-26V, then for 3-4 s under the condition that the pulse wave voltage is 14-18V, and continuously and alternately performing 10-12 cycles. The invention polishes the duplex stainless steel by adopting a pulse wave mode, and balances the problem that the two-phase selective corrosion is serious under the conventional single voltage. The surface of the sample after electrolytic polishing is clean and has no dirt, the calibration rate of the EBSD is greatly improved, and the EBSD result is more reliable.
Description
Technical Field
The invention belongs to the field of microscopic detection of stainless steel, and relates to a method for preparing a duplex stainless steel EBSD sample by pulse wave electrolytic polishing.
Background
Since microscopic detection analysis of stainless steel materials often involves orientation analysis, common orientation analysis means are XRD macroscopic texture analysis and EBSD microscopic texture analysis. The two analysis means have relatively high requirements on sample preparation, and the surface cannot be provided with a strain layer, so that the sample needs to be prepared by means of focused ion beams, chemical mechanical polishing or electrolytic polishing and the like. At present, the lowest and simplest method in the laboratory is to prepare the sample by electrolytic polishing, so that the sample is favored by researchers. At present, the conventional stainless steel with two structures of ferrite and austenite is easy to electropolish, and a good polished sample can be obtained by applying a proper constant voltage value to a sample after testing a voltage-current characteristic curve of the sample in an electropolishing solution in advance.
Because the internal structure of the duplex stainless steel is two structures of ferrite and austenite, and the existence of a grain boundary phase boundary and the difference of corrosion resistance of the two structures, the conventional method can generate serious selective corrosion, so that the part originally being ferrite or austenite is corroded, the exposed structure changes, the texture information of the section of the sample cannot be truly reflected, and the prepared sample is low in calibration rate or cannot be calibrated.
Disclosure of Invention
The invention aims to provide a method for preparing a duplex stainless steel EBSD sample by pulse wave electropolishing, which solves the problem of serious selective corrosion of the conventional electropolishing method of the duplex stainless steel.
The invention relates to a method for preparing a duplex stainless steel EBSD sample by pulse wave electrolytic polishing, which comprises the following steps:
(1) Sample pretreatment: cutting a sample by adopting linear cutting, wherein the cutting specification is RD multiplied by TD multiplied by thickness=8-12 mm multiplied by 6-10 mm multiplied by 0.1-20 mm, RD is the rolling direction, and TD is the rolling width direction; fixing the wire-cut sample by adopting thermal mosaic, grinding the section of the fixed sample by using 600# abrasive paper, 800# abrasive paper, 1200# abrasive paper and 2000# abrasive paper in sequence, and mechanically polishing after grinding;
(2) Sample cleaning: taking out the mechanically polished sample from the thermal mosaic material, putting the sample into ethanol for ultrasonic cleaning, and drying the surface of the sample with cold air after 160-180 s of cleaning;
(3) Preparing electrolytic polishing solution: preparing perchloric acid, ethylene glycol and ethylene glycol monobutyl ether into electrolytic polishing solution according to the volume ratio of 1:7:1-1:9:2;
(4) Sample electrolytic polishing: immersing a duplex stainless steel sample into an electrolytic polishing solution to serve as an anode, wherein a cathode material is ultrapure ferrite stainless steel, and performing anode pulse wave electrolytic polishing by using an electrochemical workstation or a pulse voltage output device; the electrolytic polishing is carried out for 1-2 s under the condition that the pulse wave voltage is 22-26V, then for 3-4 s under the condition that the pulse wave voltage is 14-18V, and continuously and alternately carrying out 10-12 cycles;
(5) Cleaning: and (3) ultrasonically cleaning the sample subjected to electrolytic polishing with ethanol for 160-180 s, and drying the surface of the sample with cold air.
The invention considers the different electrochemical characteristics of two phases in the electrolytic polishing solution, and respectively selects two groups of proper electrolytic polishing voltages for austenite and ferrite through a pulse wave process. Because the electrolytic polishing is the effect of the over-passivation area, the austenite and ferrite are simultaneously corroded and polished when the electrolytic polishing voltage of the austenite is applied, and the austenite is in a passivation state or at the junction of passivation and over-passivation when the electrolytic polishing voltage of the ferrite is applied, so that the relative corrosion rate is low. Through alternately acting for a proper period in the optimal electrolytic polishing voltage range of two phases, the acting effect of the austenite and ferrite phases of the sample is equivalent, and the EBSD sample with better polishing effect can be obtained. The method for preparing the dual-phase stainless steel EBSD sample by pulse wave electropolishing solves the problem of serious selective corrosion of the conventional electropolishing method of the dual-phase stainless steel, and provides a new thought method for preparing the EBSD sample by electropolishing the dual-phase stainless steel.
The invention has the beneficial effects that; 1. the electrolytic polishing process is unique, and the dual-phase stainless steel is polished by adopting a pulse wave mode, so that the problem that the two-phase selective corrosion is serious under the conventional single voltage is balanced. 2. The surface of the sample after electrolytic polishing is clean and has no dirt, the calibration rate of the EBSD is greatly improved, and the EBSD result is more reliable. 3. The electrolytic polishing solution is simple in configuration, can be repeatedly used for a plurality of times, and is environment-friendly and safe.
Drawings
FIG. 1 is a graph showing the results of EBSD analysis of the sample prepared in example 1.
FIG. 2 is a graph showing the results of EBSD analysis of the sample prepared in example 2.
FIG. 3 is a graph showing the results of EBSD analysis of the sample prepared in example 3.
Detailed Description
The method for preparing the dual-phase stainless steel EBSD sample by the pulse wave electropolishing of the invention is further described below by way of specific examples.
Example 1
(1) Sample preparation: the duplex stainless steel sample is processed by adopting linear cutting, the cutting specification is RD multiplied by TD multiplied by thickness=10mm multiplied by 8mm multiplied by 4mm, RD is the rolling direction, and TD is the rolling width direction;
(2) Sample embedding and section polishing treatment: fixing the wire-cut sample by adopting thermal mosaic, performing section grinding and polishing treatment on the mosaic sample, manually grinding the section of the sample by sequentially passing through No. 600, no. 800, no. 1200 and No. 2000 abrasive paper, and finally mechanically polishing the ground sample;
(3) Sample cleaning: taking out the mechanically polished sample from the thermal mosaic material, placing the sample into a small beaker containing ethanol for ultrasonic cleaning, and drying the surface of the sample by using a blower after cleaning for 180 seconds;
(4) Preparing electrolytic polishing solution: the method comprises the steps of preparing perchloric acid, ethylene glycol and ethylene glycol monobutyl ether according to a volume ratio of 1:8:1, placing the prepared solution into a self-made electrolytic tank, wherein the electrolytic tank is a small glass beaker, the cathode material is ultra-pure ferrite stainless steel, folding the cathode material in a positive Z shape, and placing the cathode material into the small beaker to form an electrolytic polishing device;
(5) Sample electrolytic polishing: immersing a sample into electrolyte, and performing anodic pulse wave electrolytic polishing by using an electrochemical workstation or a pulse voltage output device with a 32V range; the pulse wave voltage is 26V for 1s, then is 18V for 3s, and the pulse wave voltage is continuously and alternately applied for 10 periods;
(6) Sample cleaning: and (3) placing the electrolyzed sample into a small beaker containing ethanol for ultrasonic cleaning, and drying the surface of the sample by using a blower after cleaning for 180 seconds, so that the EBSD analysis can be performed on the sample by using an electron microscope.
FIG. 1 is a graph showing the results of EBSD analysis of the sample prepared in this example, and the two-phase morphology and distribution of the duplex stainless steel can be seen clearly, and the calibration rate reaches 98%.
Example 2
(1) Sample preparation: the duplex stainless steel casting blank sample is processed by adopting linear cutting, the cutting specification is RD multiplied by TD multiplied by thickness=10mm multiplied by 8mm, RD is the rolling direction, and TD is the rolling width direction;
(2) Sample embedding and section polishing treatment: fixing the wire-cut sample by adopting thermal mosaic, performing section grinding and polishing treatment on the mosaic sample, manually grinding the section of the sample by sequentially passing through No. 600, no. 800, no. 1200 and No. 2000 abrasive paper, and finally mechanically polishing the ground sample;
(3) Sample cleaning: taking out the mechanically polished sample from the thermal mosaic material, placing the sample into a small beaker containing ethanol for ultrasonic cleaning, and drying the surface of the sample by using a blower after cleaning for 180 seconds;
(4) Preparing electrolytic polishing solution: the method comprises the steps of preparing perchloric acid, ethylene glycol and ethylene glycol monobutyl ether according to a volume ratio of 1:8:2, placing the prepared solution into a self-made electrolytic tank, wherein the electrolytic tank is a small glass beaker, the cathode material is ultra-pure ferrite stainless steel, folding the cathode material in a positive Z shape, and placing the cathode material into the small beaker to form an electrolytic polishing device;
(5) Sample electrolytic polishing: immersing a sample into electrolyte, and performing anodic pulse wave electrolytic polishing by using an electrochemical workstation or a pulse voltage output device with a 32V range; the pulse wave voltage is applied for 1.5s at 24V, then applied for 3.5s at 16V, and continuously and alternately applied for 11 periods;
(6) Sample cleaning: placing the electrolyzed sample into a small beaker containing ethanol for ultrasonic cleaning, and drying the surface of the sample by using a blower after cleaning for 180 seconds, so that an electron microscope can be used for carrying out EBSD analysis on the sample;
FIG. 2 is a graph showing the results of EBSD analysis of the sample prepared in this example, wherein the calibration rate is 97% as clearly seen from the two-phase morphology and distribution of the duplex stainless steel.
Example 3
(1) Sample preparation: the duplex stainless steel casting blank sample is processed by adopting linear cutting, the cutting specification is RD multiplied by TD multiplied by thickness=10mm multiplied by 8mm multiplied by 12mm, RD is the rolling direction, and TD is the rolling width direction;
(2) Sample embedding and section polishing treatment: fixing the wire-cut sample by adopting thermal mosaic, performing section grinding and polishing treatment on the mosaic sample, manually grinding the section of the sample by sequentially passing through No. 600, no. 800, no. 1200 and No. 2000 abrasive paper, and finally mechanically polishing the ground sample;
(3) Sample cleaning: taking out the mechanically polished sample from the thermal mosaic material, placing the sample into a small beaker containing ethanol for ultrasonic cleaning, and drying the surface of the sample by using a blower after cleaning for 180 seconds;
(4) Preparing electrolytic polishing solution: perchloric acid, ethylene glycol and ethylene glycol monobutyl ether are configured according to the volume ratio of 1:9:1, the prepared solution is put into a self-made electrolytic tank, the electrolytic tank is a small glass beaker, the cathode material is ultra-pure ferrite stainless steel, the cathode material is folded into a positive Z shape and is put into the small beaker, and an electrolytic polishing device is formed;
(5) Sample electrolytic polishing: immersing a sample into electrolyte, and performing anodic pulse wave electrolytic polishing by using an electrochemical workstation or a pulse voltage output device with a 32V range; the pulse wave voltage is applied for 2s at 22V, then applied for 4s at 14V, and continuously and alternately applied for 12 periods;
(6) Sample cleaning: placing the electrolyzed sample into a small beaker containing ethanol for ultrasonic cleaning, and drying the surface of the sample by using a blower after cleaning for 180 seconds, so that an electron microscope can be used for carrying out EBSD analysis on the sample;
FIG. 3 is a graph showing the results of EBSD analysis of the sample prepared in this example, wherein the calibration rate is 97% as clearly seen from the two-phase morphology and distribution of the duplex stainless steel.
Claims (5)
1. A method for preparing a duplex stainless steel EBSD sample by pulse wave electropolishing, comprising the steps of:
(1) Sample pretreatment: adopting linear cutting to treat a duplex stainless steel sample, fixing the linear cut sample by adopting thermal mosaic, grinding the fixed sample, and mechanically polishing after grinding;
(2) Preparing electrolytic polishing solution: preparing perchloric acid, ethylene glycol and ethylene glycol monobutyl ether into electrolytic polishing solution according to the volume ratio of 1:7:1-1:9:2;
(3) Sample electrolytic polishing: immersing a duplex stainless steel sample into an electrolytic polishing solution to serve as an anode, wherein a cathode material is ultrapure ferrite stainless steel, and performing anode pulse wave electrolytic polishing by using an electrochemical workstation or a pulse voltage output device; the electrolytic polishing is performed for 1-2 s under the condition that the pulse wave voltage is 22-26V, then for 3-4 s under the condition that the pulse wave voltage is 14-18V, and continuously and alternately performing 10-12 cycles.
2. The method for preparing the duplex stainless steel EBSD sample by pulse wave electropolishing according to claim 1, wherein the method comprises the steps of: and the method further comprises a cleaning step after mechanical polishing, wherein after the mechanical polishing, the mechanically polished sample is taken out of the thermal mosaic material, is put into ethanol for ultrasonic cleaning, and is dried on the surface of the sample by cold air after 160-180 s of cleaning.
3. The method for preparing the duplex stainless steel EBSD sample by pulse wave electropolishing according to claim 1, wherein the method comprises the steps of: the method further comprises a cleaning step after electrolytic polishing, wherein the sample after electrolytic polishing is subjected to ultrasonic cleaning by ethanol, and the surface of the sample is dried by cold air after 160-180 s of cleaning.
4. The method for preparing the duplex stainless steel EBSD sample by pulse wave electropolishing according to claim 1, wherein the method comprises the steps of: in the step (1), the cutting specification is RD×TD×thickness=8 to 12mm×6 to 10mm×0.1 to 20mm, RD is the rolling direction, and TD is the rolling width direction.
5. The method for preparing the duplex stainless steel EBSD sample by pulse wave electropolishing according to claim 1, wherein the method comprises the steps of: and (3) manually grinding the section of the sample by sequentially passing through No. 600, no. 800, no. 1200 and No. 2000 abrasive paper in the step (1).
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102721715A (en) * | 2012-06-07 | 2012-10-10 | 山西太钢不锈钢股份有限公司 | Dual-phase stainless steel crystalline grain structure display method |
| CN106896009A (en) * | 2017-04-21 | 2017-06-27 | 桂林电子科技大学 | The preparation method of shaping ring sample is rolled in 42CrMo steel casting for EBSD tests |
| CN107976459A (en) * | 2017-11-16 | 2018-05-01 | 北京科技大学 | The analyzing detecting method of two-phase proportion in a kind of two phase stainless steel as-cast structure |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102721715A (en) * | 2012-06-07 | 2012-10-10 | 山西太钢不锈钢股份有限公司 | Dual-phase stainless steel crystalline grain structure display method |
| CN106896009A (en) * | 2017-04-21 | 2017-06-27 | 桂林电子科技大学 | The preparation method of shaping ring sample is rolled in 42CrMo steel casting for EBSD tests |
| CN107976459A (en) * | 2017-11-16 | 2018-05-01 | 北京科技大学 | The analyzing detecting method of two-phase proportion in a kind of two phase stainless steel as-cast structure |
Non-Patent Citations (1)
| Title |
|---|
| "A STUDY ON SMALL SCALE MECHANICAL BEHAVIOR FOR DEFORMATION ANALYSIS OF DUPLEX STAINLESS STEEL";金永民;《首尔国立大学研究生院博士论文》;20150831;第59-60页 * |
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