CN103792128A - Method for displaying two-phase grain boundary of duplex stainless steel - Google Patents
Method for displaying two-phase grain boundary of duplex stainless steel Download PDFInfo
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Abstract
The invention relates to a method for displaying two-phase grain boundary of duplex stainless steel. The method comprises the following steps: I, preparation of a metallographic sample, namely, (1) cutting the metallographic sample by adopting a machining saw; (2) roughly grinding the observation surface of the sample; (3) mechanically polishing the observation surface of the sample by adopting a metallographic polishing machine; (4) finely polishing the observation surface by the metallographic polishing machine; (5) cleaning the observation surface of the sample with ethyl alcohol; II, preparation of a corrosive agent, namely, preparing a mixed solution from 10-15g of copper sulfate, 50 mm <3> of nitric acid with the volume percentage being 65-68% and 100-150 mm <3> of hydrochloric acid with the volume percentage being 36-38%; III, corrosion of the metallographic sample, namely, putting the metallographic sample into a metallographic corrosive agent, taking out the duplex stainless steel when the metallographic observation surface is corroded to be deep silver gray, cleaning the sample with water, and wiping the observation surface of the metallographic sample by degreasing cotton dipped with absolute ethyl alcohol. The method for displaying two-phase grain boundary of duplex stainless steel can be used for quickly, simply and conveniently displaying the two-phase grain boundary of the duplex stainless steel.
Description
Technical field
The present invention relates to a kind of method of the two-phase crystal boundary that shows two phase stainless steel.
Background technology
Two phase stainless steel also claims ferritic-austenitic stainless steel, has many features of ferritic steel and austenitic steel concurrently, is widely used in acid-soluble oil, gas field and transportation, oil refining, petrochemical complex and oceanographic engineering field.In two phase stainless steel is produced, often need the metallographic structure of experimental material, then reach desirable performance by suitable adjusting component and production technology.When check, general 10% oxalic acid aqueous solution electrolysis, the method such as basic iron potassium cyanide solution and 40% NaOH (potassium) electrolysis of solutions heat or that boil of adopting, these methods can show the phase boundary of austenite and ferrite, carrying out mensuration and the precipitated phase of phase ratio observes, shortcoming is requirement instrumentation, time-consuming and need electricity, the two-phase crystal boundary that particularly can not show two phase stainless steel, carries out the observation of grain size.
Summary of the invention
In order to overcome the above-mentioned deficiency of method of two-phase crystal boundary of existing demonstration two phase stainless steel, the invention provides a kind of method of two-phase crystal boundary of quick, easy demonstration two phase stainless steel, profit can corrode the crystal boundary of austenite and ferrite two-phase in two phase stainless steel metallographic structure in this way in the short period of time simultaneously, observes grain size.
For achieving the above object, the present invention has taked following technical scheme.
The method of the two-phase crystal boundary of this demonstration two phase stainless steel comprises following step successively:
The preparation of I, metallographic sample
(1) metallographic specimen is got in machine work sawing, sample size will be applicable to metallographic observation, be generally the right cylinder of 15 × 20 millimeters of φ or the cube of 15 × 10 × thickness (millimeter), when sampling, must prevent that Yin Wendu from raising and causing that microstructure changes or causes plastic yield because of stressed.
(2) on abrasive machine, polish off wedge angle and the corner angle of metallographic sample, the sightingpiston of sample is roughly ground.
(3) adopt metallic phase polisher milling to carry out mechanical buffing, carry out fine grinding sightingpiston with 240#, 600# and 1000# abrasive paper for metallograph respectively, every one fine grinding all will be eliminated a procedure and stay the polishing scratch of sightingpiston, with the sightingpiston of the timely washed samples of clear water, avoid at sightingpiston kish abrasive dust simultaneously.
(4) adopt metallic phase polisher milling to carry out essence to sightingpiston and throw, use woollen cloth or velveting, adopting successively granularity is the efficient metallurgical polishing agent of 5 μ and 1 μ, controls humidity and dynamics when polishing well, after polishing the sightingpiston of sample smooth, without deformation layer, no marking.
(5) with alcohol washed samples sightingpiston, confirmation sample is treated planation surface cleanliness without any pollution.
II, mordant preparation
Mordant preparation will be carried out in draughty fuming cupboard, and balance takes copper sulphate 10g-15g, and measuring respectively percent by volume with graduated cylinder is 65% ~ 68% nitric acid 50 mm
3with percent by volume hydrochloric acid 100 ~ 150 mm that are 36% ~ 38%
3preparation mixed solution, measures 1 ~ 2 mm with dropper
3hydrofluorite join in mixed solution, then the solution preparing is stirred with glass bar, after leaving standstill, can use.
III, etching pit
The metallographic specimen preparing is put into the metallographic etching agent preparing with bamboo clip or tweezers, sightingpiston is immersed in etchant completely, sightingpiston upwards, is observed the change color of specimen surface simultaneously.In the time that metallographic observation face is etched to darker silver gray, with bamboo clip or tweezers taking-up two phase stainless steel sample, by the abundant washed samples of mobile water flowing, finally dip absolute ethyl alcohol wiped clean metallographic sample sightingpiston with absorbent cotton at once, use hot blast drying.
Owing to adopting technique scheme, the present invention has outstanding technique effect:
1, two-phase structure's ferrite of two phase stainless steel and austenitic crystal boundary clear demonstration simultaneously, optical microphotograph Microscopic observation erosion effect is splendid.
2, the pollution that the non-corrosive product of sightingpiston corroding through this mordant brings, has obtained good microstructure observation's effect.
3, the mordant that simultaneously the present invention adopts has certain chemical polishing effect, can eat away cut that sample sightingpiston is thinner and to a certain degree can reach the effect of chemical polishing.
4, corrosion method of the present invention can be used for observing Recovery and recrystallization and the grain growth situation of two phase stainless steel ferrite and austenite two-phase structure after different solution annealing temperature, and the common corrosion method of this point does not reach.
Accompanying drawing explanation
Fig. 1 is the metallographic structure photo of super-duplex stainless steel 2906 As rolleds, and the key character of tissue is that after thermal deformation, ferrite and austenite two-phase structure are fibrous along rolling direction.
Fig. 2-6 are respectively super-duplex stainless steel 2906 ferrite and the Recovery and recrystallization of austenite two-phase structure and metallographic structure photos of grain growth situation after different solution annealing of As rolled, along with the rising of solution annealing temperature, preferentially there is recovery and recrystallization as Fig. 2 at 950 ℃ of ferritic phases, austenite left backly starts to occur recrystallization as Fig. 3 at 1000 ℃, to 1050 ℃ of ferrites and austenite two-phase generation perfect recrystallization as Fig. 4; Along with the continuation of temperature raises, the crystal grain of ferrite and austenite two-phase all can be grown up in various degree, but ferritic grain size will obviously be greater than austenite crystal as Fig. 5,6, and Fig. 5 is 1150 ℃ of solid solutions, and Fig. 6 is 1200 ℃ of solid solutions.
Embodiment
Below in conjunction with example, the invention will be further described, but the two-phase stainless Steel material that is specifically suitable for of the present invention is not only confined to the steel grade of choosing in example below.
Embodiment
The material of choosing is super-duplex stainless steel material 2906 sheet materials, and specific chemical composition (mass percent %) is:
C 0.018, Si 0.56, Mn 0.96, Cr 29.38,
Ni 6.62, Mo 2.2, N 0.34,
Surplus is Fe and inevitable impurity.
Steel plate gauge thickness is 15 millimeters, and metallographic specimen size is the square of 15 × 10 × 15 millimeters, and state is As rolled solid solubility temperatures annealing different from process, and metallurgical analysis apparatus model is Lei DM4000.
The concrete operation step of the present embodiment is as follows:
The preparation of I, metallographic sample
(1) metallographic specimen is got in machine work sawing, sample size will be applicable to metallographic observation, be generally the right cylinder (or cube of 15 × 10 × 20 millimeters) of 15 × 20 millimeters of φ, when sampling, must prevent that Yin Wendu from raising and causing that microstructure changes or causes plastic yield because of stressed.
(2) on abrasive machine, polish off the unwanted wedge angle of metallographic sample and corner angle, the sightingpiston of sample is roughly ground with 120# abrasive paper for metallograph.
(3) adopt metallic phase polisher milling to carry out mechanical buffing, carry out fine grinding sightingpiston with 240#, 600# and 1000# abrasive paper for metallograph respectively, every one fine grinding all will be eliminated the polishing scratch that a procedure stays, and simultaneously with the sightingpiston of the timely washed samples of clear water, avoids at sightingpiston kish abrasive dust.
(4) adopt metallic phase polisher milling to carry out essence to sightingpiston and throw, use woollen cloth or velveting, adopting successively granularity is the efficient metallurgical polishing agent of 5 μ and 1 μ, controls humidity and dynamics when polishing well, after polishing the sightingpiston of sample smooth, without deformation layer, no marking.
(5), with alcohol washed samples surface, confirm to be seen cleanliness without any pollution of sample.
II, mordant preparation
Mordant preparation will be carried out in draughty fuming cupboard, weigh in the balance and get copper sulphate 10g, measuring respectively percent by volume with graduated cylinder is 100 milliliters of preparation mixed solutions of hydrochloric acid that 50 milliliters, 65% nitric acid and percent by volume are 36%, the hydrofluorite that measures 1 ~ 2 milliliter with dropper joins in mixed solution, with glass bar, the solution preparing is stirred again, after leaving standstill, can use.
III, etching pit
The metallographic specimen preparing is put into the metallographic etching agent preparing with bamboo clip or tweezers, sightingpiston is immersed in etchant completely, sightingpiston upwards, is observed the change color of specimen surface simultaneously.In the time that metallographic observation face is etched to darker silver gray, take out two phase stainless steel sample with bamboo clip or tweezers, use at once the abundant washed samples of mobile water, finally dip absolute ethyl alcohol wiped clean metallographic sample sightingpiston with absorbent cotton, use hot blast drying.
Claims (2)
1. show a method for the two-phase crystal boundary of two phase stainless steel, it comprises following step successively:
The preparation of I metallographic sample
(1) metallographic specimen is got in machine work sawing, and sample size will be applicable to metallographic observation, must prevent that Yin Wendu from raising and cause that microstructure changes or cause plastic yield because of stressed when sampling;
(2) on abrasive machine, polish off wedge angle and the corner angle of metallographic sample, the sightingpiston of sample is roughly ground;
(3) adopt metallic phase polisher milling to carry out mechanical buffing, carry out fine grinding sightingpiston with 240#, 600# and 1000# abrasive paper for metallograph respectively, every one fine grinding all will be eliminated a procedure and stay the polishing scratch of sightingpiston, with the sightingpiston of the timely washed samples of clear water, avoid at sightingpiston kish abrasive dust simultaneously;
(4) adopt metallic phase polisher milling to carry out essence to sightingpiston and throw, use woollen cloth or velveting, adopting successively granularity is the efficient metallurgical polishing agent of 5 μ and 1 μ, controls humidity and dynamics when polishing well, after polishing the sightingpiston of sample smooth, without deformation layer, no marking;
(5) with alcohol washed samples sightingpiston, confirmation sample is treated planation surface cleanliness without any pollution;
The preparation of II mordant
Mordant is formulated in draughty fuming cupboard and carries out, and balance takes copper sulphate 10g-15g, and measuring respectively percent by volume with graduated cylinder is 65% ~ 68% nitric acid 50 mm
3with percent by volume hydrochloric acid 100 ~ 150 mm that are 36% ~ 38%
3preparation mixed solution, measures 1 ~ 2 mm with dropper
3hydrofluorite join in mixed solution, then the solution preparing is stirred with glass bar, after leaving standstill, can use;
III etching pit
The metallographic specimen preparing is put into the metallographic etching agent preparing with bamboo clip or tweezers, sightingpiston is immersed in etchant completely, sightingpiston upwards, is observed the change color of specimen surface simultaneously;
in the time that metallographic observation face is etched to darker silver gray, with bamboo clip or tweezers taking-up two phase stainless steel sample, by the abundant washed samples of mobile water flowing, dip absolute ethyl alcohol wiped clean metallographic sample sightingpiston with absorbent cotton at once, use hot blast drying.
2. the method for the two-phase crystal boundary of demonstration two phase stainless steel according to claim 1, is characterized in that: in the time of the preparation of step I metallographic sample, sample is (15 ± 1 millimeters of φ
220 ± 1 millimeters of) × () right cylinder or (15 ± 1 millimeters
210 ± 1 millimeters of) × () cube.
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CN104233301A (en) * | 2014-09-24 | 2014-12-24 | 西安交通大学 | Metallographic etchant used for HR-2 antihydrogen steel, and preparation method and corrosion method of metallographic etchant |
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CN115323378B (en) * | 2022-08-18 | 2024-04-26 | 西安热工研究院有限公司 | Metallographic corrosive agent for displaying sliding band of austenitic material, and preparation method and use method thereof |
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