CN107014661B - A kind of caustic solution showing high nitrogen martensitic stain less steel original austenite crystal boundary - Google Patents
A kind of caustic solution showing high nitrogen martensitic stain less steel original austenite crystal boundary Download PDFInfo
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- CN107014661B CN107014661B CN201710285036.2A CN201710285036A CN107014661B CN 107014661 B CN107014661 B CN 107014661B CN 201710285036 A CN201710285036 A CN 201710285036A CN 107014661 B CN107014661 B CN 107014661B
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- 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
Abstract
The invention discloses the caustic solutions of display high nitrogen martensitic stain less steel original austenite crystal boundary.The composition range of the high nitrogen martensitic stain less steel of the invention that is applicable in are as follows: C:0.2~0.6%, Si :≤1.0%, Mn :≤1.0%, Cr:15.0~18.0%, Mo:0.5~1.5%, N:0.25~0.5%, Fe: surplus.1) caustic solution of the present invention includes the following steps: that conventionally processing obtains quenching high nitrogen martensitic stain less steel corrosion sample；2) by the polishing of sample, merging is heated in 65~75 DEG C of etchant solution one upwardly, and constant temperature 20~50min of etch takes out when the burnishing surface of sample corrodes；3) etchant solution two is dipped with cotton, is wiped repeatedly the burnishing surface through step 2) treated sample, until silver gray is presented in sample burnishing surface, cleaned, drying.Caustic solution of the present invention can clearly, completely show quenching high nitrogen martensitic stain less steel original austenite crystal boundary, reach the requirement of Measurement and evaluation crystallite dimension, formulate reasonable heat treating regime for such steel grade and provide technical support.
Description
Technical field
The invention belongs to metallographic structure observational technique fields, and in particular to a kind of original Austria of display high nitrogen martensitic stain less steel
The caustic solution of family name's body crystal boundary.
Background technique
Nitrogen is added in martensitic stain less steel as a kind of important alloying element, by with other elements (Cr, Mn etc.)
Synergistic effect, while significantly improving stainless hardness of steel, does not reduce its toughness, moreover it is possible to its wear-resisting and corrosion resistant be greatly enhanced
Corrosion energy.Therefore, high nitrogen martensitic stain less steel is as a kind of important engineering material, in Aeronautics and Astronautics, electric power, medical instrument
Have broad application prospects with fields such as cutters.
Heat treatment process can significantly affect the tissue and performance of high nitrogen martensitic stain less steel.Quenching is non-in heat treatment process
Often important link determines the quantity and distribution, residual austenite content and original austenite grains size of precipitated phase.It is original
Austenite grain size has a great impact to the mechanical property and corrosion resistance of steel, and coarse grains often reduce the impact of steel
Toughness, anti-fatigue life and corrosion resistance.Therefore, it is necessary to which the original austenite for rationally controlling high nitrogen martensitic stain less steel is brilliant
Particle size.But the addition of nitrogen makes high nitrogen martensitic stain less steel have excellent corrosion resistance, conventional martensitic is stainless
The corrosive agent of steel cannot show the original austenite crystal boundary of high nitrogen martensitic stain less steel well, be unable to measure and evaluate its crystal grain ruler
It is very little.Therefore, finding one kind can clearly show that the caustic solution of high nitrogen martensitic stain less steel original austenite crystal boundary with important
Meaning can formulate reasonable heat treating regime for such steel grade and provide foundation, so that it is big to efficiently control original austenite grains
It is small and obtain excellent tissue and performance.
Patent CN201410255299.5 discloses the clear display 9-12%Cr heat resisting steel original austenite crystal boundary of one kind
Etching pit method, the invention use corrosive agent for the aqueous solution of nitric acid of 55-65%, and it is resistance to can extremely to clearly display 9-12%Cr
Hot steel original austenite crystal boundary.Patent CN200710193134.X discloses a kind of display GCr15 original austenite grains boundary
Etching pit method, which is made into corrosive liquid by picric acid, neopelex, iron chloride and distilled water, can
Clearly show the boundary of GCr15 bearing steel original austenite grains under quenching annealed strip.However, consulting published at present
Documents and materials and patent, the caustic solution about high nitrogen martensitic stain less steel original austenite crystal boundary are rarely reported.In addition, existing
Caustic solution, some cannot corrode high nitrogen martensitic stain less steel, some preferentially corrode lath martensitic structure, original austenite
Crystal boundary is not shown or imperfect, and the purpose of Measurement and evaluation crystallite dimension is not achieved.
Therefore, the present invention is intended to provide a kind of corruption that can clearly display high nitrogen martensitic stain less steel original austenite crystal boundary
Etching method is formulated for the Measurement and evaluation of original austenite grains size after the quenching of high nitrogen martensitic stain less steel for such steel grade
Reasonable heat treating regime provides technical support.
Summary of the invention
A kind of caustic solution showing high nitrogen martensitic stain less steel original austenite crystal boundary provided by the invention, Neng Gouqing
It is clear, completely show high nitrogen martensitic stain less steel original austenite crystal boundary, for high nitrogen martensitic stain less steel quenching after original Austria
The Measurement and evaluation of family name's body crystallite dimension formulates reasonable heat treating regime for such steel grade and provides foundation, so as to effectively
It controls the original austenite grains size of high nitrogen martensitic stain less steel and obtains excellent tissue and performance.
A kind of caustic solution showing high nitrogen martensitic stain less steel original austenite crystal boundary provided by the invention, is applicable in height
The composition range of nitrogen martensitic stain less steel are as follows: C:0.2~0.6%, Si :≤1.0%, Mn :≤1.0%, Cr:15.0~
18.0%, Mo:0.5~1.5%, N:0.25~0.5%, Fe: surplus.
A kind of caustic solution showing high nitrogen martensitic stain less steel original austenite crystal boundary, comprising the following steps:
(1) prepared by metallographic specimen:
Sample is cut on high nitrogen martensitic stain less steel using wire cutting machine, after quenching, by the detection of sample to be tested
Face conventional method corase grinding, fine grinding, polishing, after making the defects of its detection faces light is without any scratch, pit and stain, with nothing
Water-ethanol is rinsed and is dried up.
(2) corrosive agent is prepared:
The used caustic solution of the present invention includes two kinds of etchant solutions, specific as follows:
(i) etchant solution one: including distilled water, ferric sulfate, potassium permanganate and sulfuric acid；Wherein the mass fraction of ferric sulfate is
0.5~1.5%, the mass fraction of potassium permanganate is 2.5~4.5%, and the mass fraction of sulfuric acid is 7.5~12.5%, and surplus is
Distilled water.
(ii) etchant solution two: including distilled water, citric acid and oxalic acid；Wherein the mass fraction of citric acid is 4~8%,
The mass fraction of oxalic acid is 6~10%, and surplus is distilled water.
(3) etching pit:
Caustic solution of the present invention is divided into two steps, specific as follows:
(i) container equipped with etchant solution one is put into 65~75 DEG C of water-baths and is heated；By step after temperature is uniform
(1) polishing of treated sample to be tested is placed in upwardly etchant solution one, constant temperature 20~50min of etch, the throwing of sample to be tested
It takes out when smooth surface is corroded, is rinsed with circulating water；
(ii) etchant solution two is dipped with clean cotton, gently wipes the polishing of sample to be tested after first step corrosion treatment
Face, and rinsed with circulating water；Wiping is repeated, until silver gray is presented in the burnishing surface of test specimens, is washed later with dehydrated alcohol
Net drying；Original austenite grains observation is finally carried out under metallographic microscope.
Distilled water is solvent in the present invention, and potassium permanganate and ferric sulfate are cathodic depolarization agent, can promote crystal boundary Cr depletion zone
Electrochemical reaction.Sulfuric acid can dissolve corrosion product and eliminate the passivating film in high nitrogen martensitic stainless steel face, reduce its corrosion resistant
Corrosion energy.Further, since high nitrogen martensitic stain less steel has very strong corrosion resistance, it is resistance to that raising temperature and reduction pH value can weaken its
Corrosion energy, but the excessively high passivation tendency that can improve high nitrogen martensitic stain less steel of sulfuric acid concentration, and temperature is excessively high can make corrosive agent
Volatilization is serious, it is therefore desirable to by sulfuric acid concentration and temperature control in zone of reasonableness.Ferric sulfate can inhibit stainless steel in acid solution
In homogeneous corrosion acid can be inhibited to the corrosion in crystal grain by adjusting the composition of ferric sulfate and sulfuric acid, and only corrode crystal boundary
Cr depletion zone.Citric acid and oxalic acid are reducing agents, can effectively remove the corrosion product and deposit of specimen surface.With the use of two
Kind etchant solution can achieve clear display high nitrogen martensitic stain less steel original austenite crystal boundary but not show lath martensite group
The purpose knitted.
The invention has the benefit that the two-step method provided shows the corruption of high nitrogen martensitic stain less steel original austenite crystal boundary
Etching method can clearly show high nitrogen martensitic stain less steel original austenite crystal boundary under as-quenched, and for Measurement and evaluation, it is brilliant
Particle size formulates reasonable heat treating regime for such steel grade and provides technical support.
Detailed description of the invention
Fig. 1 is embodiment 1 using the invention shows go out through 1000 DEG C of quenched high nitrogen martensitic stain less steels
30Cr15Mo1N original austenite grains figure.
Fig. 2 is embodiment 1 using the invention shows go out through 1020 DEG C of quenched high nitrogen martensitic stain less steels
30Cr15Mo1N original austenite grains figure.
Fig. 3 is embodiment 1 using the invention shows go out through 1050 DEG C of quenched high nitrogen martensitic stain less steels
30Cr15Mo1N original austenite grains figure.
Fig. 4 is embodiment 1 using the invention shows go out through 1100 DEG C of quenched high nitrogen martensitic stain less steels
30Cr15Mo1N original austenite grains figure.
Fig. 5 is the original austenite grains of high nitrogen martensitic stain less steel 30Cr15Mo1N under 1 different quenching of embodiment
Change in size tendency chart.
Fig. 6 is that comparative example 1 is stainless using picric acid, iron chloride, hydrochloric acid, alcoholic solution corrosion gained high nitrogen martensite
The metallographic microscope of steel 30Cr15Mo1N (1050 DEG C of hardening heat).
Fig. 7 is that comparative example 1 (is quenched using 60% nitric acid solution corrosion gained high nitrogen martensitic stain less steel 30Cr15Mo1N
1050 DEG C of fiery temperature) metallographic microscope.
Fig. 8 is using former through 1020 DEG C of quenched high nitrogen martensitic stain less steel 55Cr18Mo1VN the invention shows what is gone out
Beginning austenite grain figure.
Fig. 9 is embodiment 2 using the invention shows go out through 1060 DEG C of quenched high nitrogen martensitic stain less steels
55Cr18Mo1VN original austenite grains figure.
Figure 10 is embodiment 3 using the invention shows go out through 1060 DEG C of quenched high nitrogen martensitic stain less steels
55Cr18Mo1VN original austenite grains figure
Figure 11 is embodiment 4 using the invention shows go out through 1060 DEG C of quenched high nitrogen martensitic stain less steels
55Cr18Mo1VN original austenite grains figure
Specific embodiment
It is for a more detailed description to the present invention according to specific embodiment, but use scope of the present invention is not limited to following reality
It applies in example.
Embodiment 1
The chemical component of high nitrogen martensitic stain less steel 30Cr15Mo1N sample is shown in Table 1 in this example.
The chemical component (wt%) of 1 high nitrogen martensitic stain less steel 30Cr15Mo1N sample of table
High nitrogen martensitic stain less steel 30Cr15Mo1N described in this example is by 25kg pressurization induction furnace melting preparation.First will
Ingot casting is forged into the pole that diameter is 80mm in 1050~1150 DEG C, and furnace cooling is to room after keeping the temperature 6 hours at 800 DEG C later
Temperature.
(1) prepared by metallographic specimen:
Cut on high nitrogen martensitic stain less steel 30Cr15Mo1N pole using wire cutting machine having a size of 10mm × 10mm ×
The sample to be tested of 5mm, by different temperatures quenching and oil it is cold after (hardening heat be respectively 1000 DEG C, 1020 DEG C, 1050 DEG C and
1100 DEG C, keep the temperature 55~60min), by sample to be tested detection faces through corase grinding, fine grinding, polishing, make detection faces light without any stroke
After the defects of trace, pit and stain, is rinsed and dried up with dehydrated alcohol.
(2) corrosive agent is prepared:
The used caustic solution of the present invention includes two kinds of etchant solutions, specific as follows:
(i) etchant solution one: 0.8g ferric sulfate and 3.5g potassium permanganate are added in 94mL distilled water, and not with glass bar
Disconnected stirring is until be completely dissolved；Later, in the aqueous solution of ferric sulfate and potassium permanganate be added 6mL mass fraction be 98% it is dense
Sulfuric acid is stirred evenly with glass bar；Wherein the mass fraction of ferric sulfate is 0.73%, the mass fraction of potassium permanganate is 3.2%,
The mass fraction of sulfuric acid is 10.1%；
(ii) etchant solution two: 5g citric acid and 10g oxalic acid are added in 100mL distilled water, and is constantly stirred with glass bar
It mixes up to being completely dissolved, is configured to the solution that lemon acid mass fraction is 4.3%, oxalic acid mass fraction is 8.7%.
(3) etching pit:
Caustic solution of the present invention is divided into two steps, specific as follows:
(i) container equipped with etchant solution one is put into 70 DEG C of water-baths and is heated；Step (1) is handled after temperature is uniform
The polishing of sample to be tested afterwards is placed in upwardly etchant solution one, constant temperature etch 40min, and polished face is taken out when corroding,
It is rinsed with circulating water；
(ii) etchant solution two is dipped with clean cotton, gently wipes the throwing of the sample to be tested after first step corrosion treatment
Smooth surface, and rinsed with circulating water；Wiping is repeated, until test specimens burnishing surface present silver gray, after washed with dehydrated alcohol
Net drying；Original austenite grains observation is finally carried out under Olympus DSX510 metallographic microscope.
Fig. 1, Fig. 2, Fig. 3 and Fig. 4 are respectively high nitrogen martensitic stain less steel 30Cr15Mo1N by different temperatures quenching and oil
The original austenite of (hardening heat is respectively 1000 DEG C, 1020 DEG C, 1050 DEG C and 1100 DEG C, keeps the temperature 55~60min) is brilliant after cold
Grain figure.As seen from the figure, test specimens crystal boundary complete display reaches the requirement of Measurement and evaluation crystallite dimension, can formulate for the steel grade
Reasonable heat treating regime provides foundation.Fig. 5 is the original of high nitrogen martensitic stain less steel 30Cr15Mo1N under different quenching
Austenite grain size trend chart.
Comparative example 1 is using the solution of picric acid, iron chloride, hydrochloric acid and alcohol as corrosive liquid
(1) prepared by metallographic specimen:
Cut on high nitrogen martensitic stain less steel 30Cr15Mo1N pole using wire cutting machine having a size of 10mm × 10mm ×
The sample to be tested of 5mm, after simultaneously oil is cold by quenching (hardening heat is 1050 DEG C, keeps the temperature 55~60min), by the inspection of sample to be tested
Survey face is through corase grinding, fine grinding, polishing, after making the defects of sample to be tested detection faces light is without any scratch, pit and stain, with nothing
Water-ethanol is rinsed and is dried up.
(2) corrosive agent is prepared:
1g picric acid and 5g iron chloride are added in the concentrated hydrochloric acid that 25mL mass fraction is 36~38%, it is continuous with glass bar
Stirring, until picric acid and iron chloride all dissolve；Then it is anhydrous that 50mL is added in the hydrochloric acid solution of picric acid and iron chloride
Ethyl alcohol is stirred evenly with glass bar.
(3) etching pit:
The polishing of step (1) treated sample to be tested is placed in upwardly etchant solution, room temperature etch 15s, test specimens
Burnishing surface present silver gray when take out, rinsed with circulating water, after with dehydrated alcohol clean drying；Finally in Olympus
Original austenite grains observation is carried out under DSX510 metallographic microscope, the metallographic microscope of sample viewing surface is as shown in Fig. 6.
The original austenite crystal boundary of test specimens does not show that presentation is lath martensite tissue, and Measurement and evaluation crystalline substance is not achieved
The requirement of particle size.
Comparative example 1 is using 60% aqueous solution of nitric acid as corrosive liquid
(1) prepared by metallographic specimen:
Cut on high nitrogen martensitic stain less steel 30Cr15Mo1N pole using wire cutting machine having a size of 10mm × 10mm ×
The sample to be tested of 5mm, after simultaneously oil is cold by quenching (hardening heat is 1050 DEG C, keeps the temperature 55~60min), by the inspection of sample to be tested
Survey face is through corase grinding, fine grinding, polishing, after making the defects of sample to be tested detection faces light is without any scratch, pit and stain, with nothing
Water-ethanol is rinsed and is dried up.
(2) corrosive agent is prepared:
60mL concentrated nitric acid is added in 40mL distilled water, is stirred evenly with glass bar；
(3) etching pit:
The polishing of step (1) treated sample to be tested is placed in upwardly etchant solution, is taken after room temperature etch 10min
Out, rinsed with circulating water, after with dehydrated alcohol clean drying；It is finally carried out under Olympus DSX510 metallographic microscope original
Austenite grain observation, the metallographic microscope of sample viewing surface are as shown in Fig. 7.
The field trash in tapping is only shown in picture, lath martensite tissue and original austenite crystal boundary does not occur.Institute
With such corrosive agent cannot corrode the high nitrogen martensitic stain less steel of excellent anti-corrosion performance, and Measurement and evaluation crystallite dimension is not achieved
Purpose.
Embodiment 2
The chemical component of high nitrogen martensitic stain less steel 55Cr18Mo1VN sample is shown in Table 2 in this example.
The chemical component (wt%) of 2 high nitrogen martensitic stain less steel 55Cr18Mo1VN sample of table
High nitrogen martensitic stain less steel 55Cr18Mo1VN described in this example is by 25kg pressurization induction furnace melting preparation.First
Ingot casting is forged into the pole that diameter is 80mm in 1060~1160 DEG C, furnace cooling is arrived after keeping the temperature 6 hours at 800 DEG C later
Room temperature.
(1) prepared by metallographic specimen:
Cut on high nitrogen martensitic stain less steel 55Cr18Mo1V pole using wire cutting machine having a size of 10mm × 10mm ×
The sample to be tested of 5mm, by different temperatures quenching and oil it is cold after (hardening heat is respectively 1020 DEG C, 1060 DEG C, heat preservation 55~
60min), make detection faces light without any scratch, pit and stain through corase grinding, fine grinding, polishing the detection faces of sample to be tested
The defects of after, rinsed and dried up with dehydrated alcohol.
(2) corrosive agent is prepared:
The used caustic solution of the present invention includes two kinds of etchant solutions, specific as follows:
(i) etchant solution one: 1g ferric sulfate and 4.5g potassium permanganate are added in 93mL distilled water, and continuous with glass bar
Stirring is until be completely dissolved；Later, the dense sulphur that 7mL mass fraction is 98% is added in the aqueous solution of ferric sulfate and potassium permanganate
Acid is stirred evenly with glass bar；Wherein the mass fraction of ferric sulfate is 0.9%, the mass fraction of potassium permanganate is 4%, sulfuric acid
Mass fraction be 11.5%；
(ii) etchant solution two: 6g citric acid and 9g oxalic acid are added in 100mL distilled water, and is stirred continuously with glass bar
Until being completely dissolved, it is configured to the solution that lemon acid mass fraction is 5.2%, oxalic acid mass fraction is 7.8%.
(3) etching pit:
Caustic solution of the present invention is divided into two steps, specific as follows:
(i) container equipped with etchant solution one is put into 70 DEG C of water-baths and is heated；Step (1) is handled after temperature is uniform
The polishing of sample to be tested afterwards is placed in upwardly etchant solution one, constant temperature etch 35min, and polished face is taken out when corroding,
It is rinsed with circulating water；
(ii) etchant solution two is dipped with clean cotton, gently wipes the throwing of the sample to be tested after first step corrosion treatment
Smooth surface, and rinsed with circulating water；Wiping is repeated, until test specimens burnishing surface present silver gray, after washed with dehydrated alcohol
Net drying；Original austenite grains observation is finally carried out under Olympus DSX510 metallographic microscope.
Fig. 8 and Fig. 9 is respectively high nitrogen martensitic stain less steel 55Cr18Mo1V (quenching after different temperatures quenches and oil is cold
Temperature is respectively 1020 DEG C and 1060 DEG C, keeps the temperature 55~60min) original austenite grains figure.As seen from the figure, the crystalline substance of test specimens
Boundary's complete display reaches the requirement of Measurement and evaluation crystallite dimension, can be formulated for the steel grade reasonable heat treating regime provide according to
According to.
Embodiment 3
The chemical component of high nitrogen martensitic stain less steel 55Cr18Mo1VN sample is shown in Table 2 in this example.
The chemical component (wt%) of 2 high nitrogen martensitic stain less steel 55Cr18Mo1VN sample of table
High nitrogen martensitic stain less steel 55Cr18Mo1VN described in this example is by 25kg pressurization induction furnace melting preparation.First
Ingot casting is forged into the pole that diameter is 80mm in 1060~1160 DEG C, furnace cooling is arrived after keeping the temperature 6 hours at 800 DEG C later
Room temperature.
(1) prepared by metallographic specimen:
Cut on high nitrogen martensitic stain less steel 55Cr18Mo1V pole using wire cutting machine having a size of 10mm × 10mm ×
The sample to be tested of 5mm, after simultaneously oil is cold by quenching (hardening heat is 1060 DEG C, keeps the temperature 55~60min), by the inspection of sample to be tested
Survey face is rushed after making the defects of detection faces light is without any scratch, pit and stain with dehydrated alcohol through corase grinding, fine grinding, polishing
It washes and dries up.
(2) corrosive agent is prepared:
The used caustic solution of the present invention includes two kinds of etchant solutions, specific as follows:
(i) etchant solution one: 0.5g ferric sulfate and 2.5g potassium permanganate are added in 88mL distilled water, and not with glass bar
Disconnected stirring is until be completely dissolved；Later, it is 98% that 4.1mL mass fraction is added in the aqueous solution of ferric sulfate and potassium permanganate
The concentrated sulfuric acid is stirred evenly with glass bar；Wherein the mass fraction of ferric sulfate is 0.51%, the mass fraction of potassium permanganate is
2.5%, the mass fraction of sulfuric acid is 7.6%；
(ii) etchant solution two: 4g citric acid and 6g oxalic acid are added in 90mL distilled water, and is stirred continuously with glass bar
Until being completely dissolved, it is configured to the solution that lemon acid mass fraction is 4%, oxalic acid mass fraction is 6%.
(3) etching pit:
Caustic solution of the present invention is divided into two steps, specific as follows:
(i) container equipped with etchant solution one is put into 65 DEG C of water-baths and is heated；Step (1) is handled after temperature is uniform
The polishing of sample to be tested afterwards is placed in upwardly etchant solution one, constant temperature etch 20min, and polished face is taken out when corroding,
It is rinsed with circulating water；
(ii) etchant solution two is dipped with clean cotton, gently wipes the throwing of the sample to be tested after first step corrosion treatment
Smooth surface, and rinsed with circulating water；Wiping is repeated, until test specimens burnishing surface present silver gray, after washed with dehydrated alcohol
Net drying；Original austenite grains observation is finally carried out under Olympus DSX510 metallographic microscope.
Figure 10 is that (hardening heat is 1060 DEG C to high nitrogen martensitic stain less steel 55Cr18Mo1V, is protected after quenching and oil is cold
55~60min of temperature) original austenite grains figure.As seen from the figure, the crystal boundary complete display of test specimens, reaches Measurement and evaluation crystal grain
The requirement of size can formulate reasonable heat treating regime for the steel grade and provide foundation.
Embodiment 4
The chemical component of high nitrogen martensitic stain less steel 55Cr18Mo1VN sample is shown in Table 2 in this example.
The chemical component (wt%) of 2 high nitrogen martensitic stain less steel 55Cr18Mo1VN sample of table
High nitrogen martensitic stain less steel 55Cr18Mo1VN described in this example is by 25kg pressurization induction furnace melting preparation.First
Ingot casting is forged into the pole that diameter is 80mm in 1060~1160 DEG C, furnace cooling is arrived after keeping the temperature 6 hours at 800 DEG C later
Room temperature.
(1) prepared by metallographic specimen:
Cut on high nitrogen martensitic stain less steel 55Cr18Mo1V pole using wire cutting machine having a size of 10mm × 10mm ×
The sample to be tested of 5mm detects sample to be tested after by quenching, simultaneously oil is cold (hardening heat is 1060 DEG C, keeps the temperature 55~60min)
Face is rinsed after making the defects of detection faces light is without any scratch, pit and stain with dehydrated alcohol through corase grinding, fine grinding, polishing
And it dries up.
(2) corrosive agent is prepared:
The used caustic solution of the present invention includes two kinds of etchant solutions, specific as follows:
(i) etchant solution one: 1.5g ferric sulfate and 4.5g potassium permanganate are added in 82mL distilled water, and not with glass bar
Disconnected stirring is until be completely dissolved；Later, it is 98% that 6.8mL mass fraction is added in the aqueous solution of ferric sulfate and potassium permanganate
The concentrated sulfuric acid is stirred evenly with glass bar；Wherein the mass fraction of ferric sulfate is 1.5%, the mass fraction of potassium permanganate is
4.5%, the mass fraction of sulfuric acid is 12.4%；
(ii) etchant solution two: 8g citric acid and 10g oxalic acid are added in 82mL distilled water, and is stirred continuously with glass bar
Until being completely dissolved, it is configured to the solution that lemon acid mass fraction is 8%, oxalic acid mass fraction is 10%.
(3) etching pit:
Caustic solution of the present invention is divided into two steps, specific as follows:
(i) container equipped with etchant solution one is put into 75 DEG C of water-baths and is heated；Step (1) is handled after temperature is uniform
The polishing of sample to be tested afterwards is placed in upwardly etchant solution one, constant temperature etch 50min, and polished face is taken out when corroding,
It is rinsed with circulating water；
(ii) etchant solution two is dipped with clean cotton, gently wipes the throwing of the sample to be tested after first step corrosion treatment
Smooth surface, and rinsed with circulating water；Wiping is repeated, until test specimens burnishing surface present silver gray, after washed with dehydrated alcohol
Net drying；Original austenite grains observation is finally carried out under Olympus DSX510 metallographic microscope.
Figure 11 is respectively high nitrogen martensitic stain less steel 55Cr18Mo1V (hardening heat 1060 after quenching and oil is cold
DEG C, keep the temperature 55~60min) original austenite grains figure.As seen from the figure, the crystal boundary complete display of test specimens, reaches measurement and comments
Determine the requirement of crystallite dimension, foundation can be provided for reasonable heat treating regime.
Claims (1)
1. a kind of caustic solution for showing high nitrogen martensitic stain less steel original austenite crystal boundary, which is characterized in that the high nitrogen
The composition range of martensitic stain less steel be C:0.2~0.6%, Si :≤1.0%, Mn :≤1.0%, Cr:15.0~18.0%,
Mo:0.5~1.5%, N:0.25~0.5%, Fe: surplus；The following steps are included:
(1) prepared by metallographic specimen:
Sample is cut on high nitrogen martensitic stain less steel, after quenching, by the detection faces corase grinding of sample to be tested, fine grinding, polishing,
Make its detection faces light without any defect after, rinsed and dried up with dehydrated alcohol；
(2) corrosive agent is prepared:
1. etchant solution one: including distilled water, ferric sulfate, potassium permanganate and sulfuric acid；Wherein the mass fraction of ferric sulfate be 0.5~
1.5%, the mass fraction of potassium permanganate is 2.5~4.5%, and the mass fraction of sulfuric acid is 7.5~12.5%, and surplus is distillation
Water；
2. etchant solution two: including distilled water, citric acid and oxalic acid；Wherein the mass fraction of citric acid is 4~8%, oxalic acid
Mass fraction is 6~10%, and surplus is distilled water；
(3) etching pit:
(i) container equipped with etchant solution one is put into 65~75 DEG C of water-baths and is heated；It will be at step (1) after temperature is uniform
The polishing of sample to be tested after reason is placed in etchant solution one upwardly, constant temperature 20~50min of etch, the burnishing surface of sample to be tested
It takes out when corroding, is rinsed with circulating water；
(ii) etchant solution two is dipped with clean cotton, gently wipes the burnishing surface of sample to be tested after the corrosion treatment of (i) step,
And it is rinsed with circulating water；Wiping is repeated, until silver gray is presented in the burnishing surface of test specimens, is cleaned blow with dehydrated alcohol later
It is dry；Original austenite grains observation is finally carried out under metallographic microscope.
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| CN201710285036.2A CN107014661B (en) | 2017-04-27 | 2017-04-27 | A kind of caustic solution showing high nitrogen martensitic stain less steel original austenite crystal boundary |
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| CN109022698B (en) * | 2018-10-10 | 2020-07-10 | 北京科技大学 | Original austenite grain boundary display method of medium alloy martensite wear-resistant cast steel |
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| CN112304733A (en) * | 2020-10-27 | 2021-02-02 | 上海交通大学 | Corrosive agent for displaying austenite grain boundary of martensitic stainless steel and display method |
| CN112548094B (en) * | 2020-12-04 | 2023-04-18 | 东北大学 | 30Cr15MoY alloy steel powder for laser additive manufacturing or remanufacturing and using method thereof |
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| CN113218736A (en) * | 2021-05-07 | 2021-08-06 | 大唐锅炉压力容器检验中心有限公司 | Original austenite grain boundary corrosion method of martensitic stainless steel for steam turbine bolt |
| CN113358646B (en) * | 2021-05-12 | 2023-01-31 | 东南大学 | Corrosive agent for testing 16MnCr5 steel austenite grain boundary and testing method thereof |
| CN114397166B (en) * | 2021-12-09 | 2023-07-28 | 阳江合金材料实验室 | Application of potassium permanganate etchant in metallographic corrosion of high-carbon martensitic stainless steel |
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