CN103792128B - A kind of method of the biphase crystal boundary showing two phase stainless steel - Google Patents
A kind of method of the biphase crystal boundary showing two phase stainless steel Download PDFInfo
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- CN103792128B CN103792128B CN201410059302.6A CN201410059302A CN103792128B CN 103792128 B CN103792128 B CN 103792128B CN 201410059302 A CN201410059302 A CN 201410059302A CN 103792128 B CN103792128 B CN 103792128B
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Abstract
A kind of method that the present invention relates to biphase crystal boundary showing two phase stainless steel, it includes following step；The preparation of I metallographic sample；(1) machining sawing takes metallographic specimen；(2) sightingpiston of sample is roughly ground；(3) sample sightingpiston is mechanically polished by metallic phase polisher milling；(4) metallic phase polisher milling carries out essence throwing to sightingpiston；(5) alcohol washes sample sightingpiston；Preparation of Cupric Sulfate 10g 15g joined by II caustic, takes nitric acid 50 mm that percent by volume is 65% ~ 68%3With hydrochloric acid 100 ~ 150 mm that percent by volume is 36% ~ 38%3Preparation mixed solution；Metallographic specimen is put in metallographic etching agent by III etching pit, when metallographic observation face is etched to deeper silver gray, takes out two-phase stainless steel curved beam, uses water washed samples, dip dehydrated alcohol wiped clean metallographic sample sightingpiston with absorbent cotton.The method of the biphase crystal boundary of this display two phase stainless steel can be quick, easy the biphase crystal boundary of display two phase stainless steel.
Description
Technical field
A kind of method that the present invention relates to biphase crystal boundary showing two phase stainless steel.
Background technology
Two phase stainless steel is also referred to as ferritic-austenitic stainless steel, has many features of ferritic steel and austenitic steel concurrently, extensively
General apply in acid petroleum-gas fiedl and transport, oil refining, petrochemical industry and ocean engineering field.In two phase stainless steel produces, warp
Often need the metallographic structure of experimental material, then reach preferable performance by suitable adjusting component and production technology.Inspection
Time, general employing 10% oxalic acid aqueous solution is electrolysed, hot or that boil basic iron potassium cyanide solution and 40% sodium hydroxide (potassium) are molten
The methods such as liquid electrolysis, these methods can show the phase boundary of austenite and ferrite, carries out mensuration and the precipitation of Phase Proportion
Observing mutually, shortcoming is requirement instrumentation, time-consuming and need electricity, particularly can not show the biphase crystal boundary of two phase stainless steel,
Carry out the observation of grain size.
Summary of the invention
In order to overcome the above-mentioned deficiency of the method for the biphase crystal boundary of existing display two phase stainless steel, the present invention provides a kind of fast
The method of the biphase crystal boundary of fast, easy display two phase stainless steel, profit can be invaded in this way the most simultaneously
Lose the crystal boundary that austenite and ferrite in two phase stainless steel metallographic structure are biphase, observe grain size.
For achieving the above object, this invention takes following technical scheme.
The method of the biphase crystal boundary of this display two phase stainless steel includes following step successively:
I, the preparation of metallographic sample
(1) machining sawing takes metallographic specimen, sample size metallographic observation to be suitable for, the usually circle of φ 15 × 20 millimeters
Cylinder or the cube of 15 × 10 × thickness (millimeter), must be prevented from during sampling causing microscopic structure to become because temperature raises
Change or because stress causes plastic deformation.
(2) polish off wedge angle and the corner angle of metallographic sample on abrasive machine, the sightingpiston of sample is roughly ground.
(3) use metallic phase polisher milling to mechanically polish, carry out fine grinding with 240#, 600# and 1000# abrasive paper for metallograph respectively
Sightingpiston, every one fine grinding will eliminate one procedure and stay the polishing scratch of sightingpiston, simultaneously by the timely washed samples of clear water
Sightingpiston, it is to avoid at sightingpiston kish abrasive dust.
(4) using metallic phase polisher milling that sightingpiston carries out essence throwing, use woollen cloth or velveting, using granularity successively is 5 μ
With 1 μ efficient metallurgical polishing agent, controlling humidity and dynamics during polishing well, after polishing, the sightingpiston of sample is smooth, without deformation layer, nothing
Cut.
(5) with alcohol washes sample sightingpiston, confirm that erosion surface cleanliness without any pollution treated by sample.
II, caustic preparation
Caustic preparation to be carried out in draughty fume hood, and balance weighs copper sulfate 10g-15g, divides with graduated cylinder
Do not measure nitric acid 50 mm that percent by volume is 65% ~ 68%3With hydrochloric acid 100 ~ 150 mm that percent by volume is 36% ~ 38%3Join
Mixed solution processed, measures 1 ~ 2 mm with dropper3Fluohydric acid. join in mixed solution, then with Glass rod, the solution prepared is stirred
Mix uniformly, can use after standing.
III, etching pit
With bamboo clip or tweezers, the metallographic specimen prepared is put in the metallographic etching agent prepared, make sightingpiston
Being completely immersed in etchant, sightingpiston upwards, observes the color change of specimen surface simultaneously.Treat that metallographic observation face is etched to relatively
During deep silver gray, taking out two-phase stainless steel curved beam with bamboo clip or tweezers, the water with the flowing of flowing is the most clear at once
Wash sample, finally dip dehydrated alcohol wiped clean metallographic sample sightingpiston with absorbent cotton, use hot blast drying.
Owing to using technique scheme, the present invention has a prominent technique effect:
1, two-phase structure's ferrite of two phase stainless steel and the crystal boundary of austenite can clearly show simultaneously, optical microscope
Lower observation erosion effect is splendid.
2, the pollution that the non-corrosive product of sightingpiston corroded through this caustic brings, it is thus achieved that good microscopic structure is seen
Examine effect.
3, the caustic that the present invention uses simultaneously has certain chemical polishing effect, can eat away sample sightingpiston relatively
Thin cut to a certain degree can reach the effect of chemical polishing.
4, the corrosion method of the present invention can be used to observe two phase stainless steel ferrite after different solution annealing temperature
Growing up situation with the Recovery and recrystallization of austenite two-phase structure and crystal grain, the common corrosion method of this point does not reaches.
Accompanying drawing explanation
Fig. 1 is the metallographic structure photo of super-duplex stainless steel 2906 rolled, after the key character of tissue is thermal deformation
Ferrite and austenite two-phase structure are threadiness along rolling direction.
Fig. 2-6 is the super-duplex stainless steel 2906 of rolled ferrite and Austria after different solution annealing respectively
The Recovery and recrystallization of Shi Ti two-phase structure and crystal grain are grown up the metallographic structure photo of situation, along with the liter of solution annealing temperature
, preferentially there is recovery and recrystallization such as Fig. 2 at 950 DEG C of ferritic phases in height, austenite phase occurs recrystallization 1000 DEG C of left back beginnings
Such as Fig. 3, to 1050 DEG C of ferrites and austenite biphase generation perfect recrystallization such as Fig. 4；Along with the continuation of temperature raises, ferrite
The crystal grain biphase with austenite all can be grown up in various degree, but ferritic grain size austenite crystal to be significantly greater than is such as
Fig. 5,6, Fig. 5 is 1150 DEG C of solid solutions, and Fig. 6 is 1200 DEG C of solid solutions.
Detailed description of the invention
Below in conjunction with example, the invention will be further described, but the concrete of the present invention is suitable for two-phase stainless Steel material not only
It is limited only to the steel grade chosen in Examples below.
Embodiment
The material chosen is super-duplex stainless steel material 2906 sheet material, 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 rolled
With through different solid solubility temperature annealing, metallurgical analysis apparatus model is Lei DM4000.
The concrete operation step of the present embodiment is as follows:
I, the preparation of metallographic sample
(1) machining sawing takes metallographic specimen, sample size metallographic observation to be suitable for, the usually circle of φ 15 × 20 millimeters
Cylinder (or cube of 15 × 10 × 20 millimeters), must be prevented from during sampling causing microscopic structure to change because temperature raises
Or because stress causes plastic deformation.
(2) the unwanted wedge angle of metallographic sample and corner angle are polished off on abrasive machine, the sightingpiston 120# metallographic to sample
Sand paper is roughly ground.
(3) use metallic phase polisher milling to mechanically polish, carry out fine grinding with 240#, 600# and 1000# abrasive paper for metallograph respectively
Sightingpiston, every one fine grinding will eliminate the polishing scratch that one procedure stays, simultaneously with the sightingpiston of the timely washed samples of clear water,
Avoid at sightingpiston kish abrasive dust.
(4) using metallic phase polisher milling that sightingpiston carries out essence throwing, use woollen cloth or velveting, using granularity successively is 5 μ
With 1 μ efficient metallurgical polishing agent, controlling humidity and dynamics during polishing well, after polishing, the sightingpiston of sample is smooth, without deformation layer, nothing
Cut.
(5) use alcohol washes specimen surface, confirm to be seen cleanliness without any pollution of sample.
II, caustic preparation
Caustic preparation to be carried out in draughty fume hood, weighs in the balance and takes copper sulfate 10g, measures respectively with graduated cylinder
Take 50 milliliters of the nitric acid that percent by volume is 65% and the hydrochloric acid 100 milliliters that percent by volume is 36% preparation mixed solution, with dripping
Pipe measures the Fluohydric acid. of 1 ~ 2 milliliter and joins in mixed solution, then with Glass rod by uniform for the solution stirring prepared, after standing i.e.
Can use.
III, etching pit
With bamboo clip or tweezers, the metallographic specimen prepared is put in the metallographic etching agent prepared, make sightingpiston
Being completely immersed in etchant, sightingpiston upwards, observes the color change of specimen surface simultaneously.Treat that metallographic observation face is etched to relatively
During deep silver gray, take out two-phase stainless steel curved beam with bamboo clip or tweezers, at once by the abundant washed samples of water of flowing,
Finally dip dehydrated alcohol wiped clean metallographic sample sightingpiston with absorbent cotton, use hot blast drying.
Claims (1)
1. the method showing the biphase crystal boundary of two phase stainless steel, it includes following step successively:
The preparation of I metallographic sample
(1) machining sawing takes metallographic specimen, and sample size metallographic observation to be suitable for, sample is (φ 15 ± 1 millimeters2) × (20 ±
1 millimeter) cylinder or (15 ± 1 millimeters2) × (10 ± 1 millimeters) cube；
Must be prevented from during sampling causing microscopic structure change because temperature raises or because stress causes plastic deformation；
(2) polish off wedge angle and the corner angle of metallographic sample on abrasive machine, the sightingpiston of sample is roughly ground；
(3) metallic phase polisher milling is used to mechanically polish, respectively with 240#, 600# and 1000# abrasive paper for metallograph fine grinding sightingpiston, often
One fine grinding will eliminate one procedure and stay the polishing scratch of sightingpiston, simultaneously with the sightingpiston of the timely washed samples of clear water, keeps away
Exempt from sightingpiston kish abrasive dust；
(4) using metallic phase polisher milling that sightingpiston carries out essence throwing, use woollen cloth or velveting, using granularity successively is 5 μm and 1
The efficient metallurgical polishing agent of μm, controls humidity and dynamics well during polishing, after polishing, the sightingpiston of sample is smooth, without deformation layer, nothing
Cut；
(5) with alcohol washes sample sightingpiston, confirm that erosion surface cleanliness without any pollution treated by sample；
II caustic preparation
Caustic is formulated in draughty fume hood and carries out, and balance weighs copper sulfate 10g-15g, measures respectively with graduated cylinder
Percent by volume is nitric acid 50 mm of 65% ~ 68%3With hydrochloric acid 100 ~ 150 mm that percent by volume is 36% ~ 38%3Preparation mixing
Solution, measures 1 ~ 2 mm with dropper3Fluohydric acid. join in mixed solution, then with Glass rod by equal for the solution stirring prepared
Even, can use after standing；
III etching pit
With bamboo clip or tweezers, the metallographic specimen prepared is put in the metallographic etching agent prepared, make sightingpiston complete
Immersing in etchant, sightingpiston upwards, is observed the color change of specimen surface simultaneously, is treated that metallographic observation face is etched to deeper
During silver gray, take out two-phase stainless steel curved beam with bamboo clip or tweezers, at once by the abundant washed samples of water of flowing, with de-
Fat cotton dips dehydrated alcohol wiped clean metallographic sample sightingpiston, uses hot blast drying.
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| CN104233301B (en) * | 2014-09-24 | 2017-02-22 | 西安交通大学 | Metallographic etchant used for HR-2 antihydrogen steel, and preparation method and corrosion method of metallographic etchant |
| CN106092710B (en) * | 2016-06-22 | 2018-08-10 | 东方电气集团东方锅炉股份有限公司 | The display methods of austenite and ferrite dissimilar steel joint metallographic structure |
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| CN114808095A (en) * | 2022-04-06 | 2022-07-29 | 长春工业大学 | Electrolytic etching method for displaying two-phase structure and grain boundary of duplex stainless steel |
| 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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