CN104236993B - A kind of method simultaneously showing bearing steel austenite grain boundary and intracrystalline martensite - Google Patents
A kind of method simultaneously showing bearing steel austenite grain boundary and intracrystalline martensite Download PDFInfo
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- CN104236993B CN104236993B CN201410482905.7A CN201410482905A CN104236993B CN 104236993 B CN104236993 B CN 104236993B CN 201410482905 A CN201410482905 A CN 201410482905A CN 104236993 B CN104236993 B CN 104236993B
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Abstract
A kind of method simultaneously showing bearing steel austenite grain boundary and intracrystalline martensite.Steel are first processed into the square sample that the length of side is 10～20mm by the present invention, are cooled to 690～730 DEG C with 0.1～0.5 DEG C/s, then Quenching Treatment after sample is inserted the heating furnace inside holding 5～20min of 1000～1100 DEG C.Secondly sample is roughly ground, fine grinding and polishing.Last configuration 2～the nital of 4% at normal temperatures, by in burnishing surface leaching people's nital of sample 10～20s, when canescence occurs in specimen surface, rinse with water, with alcoholic solution, water is washed again, with hair-dryer, specimen surface is dried up, examine under a microscope, just it is observed that clearly net carbide be distributed at beginning austenite grain boundary, the martensite of austenite crystal intragranular also is able to clearly indicate out simultaneously.The method corrosion process step is simple, it is easy to operation, and stability is strong, and the effect after erosion is clear.
Description
Technical field
The invention belongs to technical field of metallographic preparation, utilize heat treatment to prepare pro-eutectoid net carbide particularly to one
Method method that high-carbon-chromium bearing steel austenite grain boundary is carried out display process.
Background technology
Austenite grain size and uniformity coefficient have important impact for the mechanical property of steel.High-carbon-chromium bearing steel is come
Saying, tiny original austenite grains is sized to be effectively improved the mechanical property of bearing steel and fatigue life.Tiny crystal grain
More crystal boundary can be provided, owing to intercrystalline strengthening improves the intensity of bearing steel；There is uniformly fine austenite crystal grain simultaneously
Bearing steel will obtain the most even tiny lath martensite, it is possible to the effective toughness improving bearing steel.Additionally, crystal boundary
Place's atomic arrangement is irregular, and micro-crack extension to grain boundaries will consume more energy, and tiny crystal grain can effectively suppress crackle
Spreading rate.The most accurately and easily show that the austenite grain boundary of steel has great importance.Currently for austenite crystal
The display packing on boundary mainly has oxidizing process, ferrite net method, segregation of Mn method and grain boundary corrosion method, wherein grain boundary corrosion method
The more commonly used.
But, the display packing such as grain boundary corrosion method operates the most comparatively laborious, and not only the preparation of corrosive liquid is complicated, and in reality
Needing in the operating process of border to corrode the most for a long time, and to need repeatedly to polish and corrode, display effect is the most unstable, has
Time Display of Grain Boundary the most clear.Especially for the steel grade that Si comparision contents is high, such as GCr15SiMn steel, due to Si element
Existence so that austenite grain boundary is more difficult to corrode.Additionally, conventional method is only capable of displaying out single austenite grain boundary, and
Cannot demonstrate the position of martensite within austenite to the thickness with martensitic needles, these problems are to high-carbon-chromium bearing steel austenite
The analysis of the relation of the display of crystal boundary and austenite grain size and martensite brings difficulty and inconvenience.
Summary of the invention
The present invention relates to a kind of method utilizing net carbide display GCr15SiMn steel austenite grain boundary, by steel are adopted
Take specific heat treatment method so that pro-eutectoid proeutectoid carbide separates out at original austenite crystal prevention, utilize easy nitre afterwards
Acid alcoholic solution corrodes, and can clearly display the proeutectoid carbide net at austenite grain boundary, thus symbolize austenite crystal
Size.The present invention solves to study GCr15SiMn high-carbon-chromium bearing steel crystal grain long big experiment austenite grain boundary and is difficult to corrode and operate
Loaded down with trivial details problem, and simple, clearly, demonstrate austenite grain boundary accurately while, show the position of martensite to
With the thickness of martensitic needles, this is to solve the relation of martensite in austenite grain size and austenite crystal to provide convenience.
A kind of method simultaneously showing bearing steel austenite grain boundary and intracrystalline martensite, by heat treatment, corase grind sample,
Fine grinding sample, polish and corrode four steps complete to have Morphology of pearlite GCr15SiMn steel original austenite crystal prevention display process,
Concrete technical step is as follows:
(1) steel are processed into the sample of regular shape, then sample is inserted the heating rising to predetermined temperature
In stove, carry out slow cooling process after the insulation scheduled time, after slow cooling to specified temp, carry out shrend；Described heating
Stove predetermined temperature is 1000～1100 DEG C, and temperature retention time is 5～20min；Slow cooling cooling rate is 0.1～0.5 DEG C/s,
Then slow cooling carries out Quenching Treatment to 690～730 DEG C；
(2) sample after heat treatment is roughly ground, fine grinding and polishing, use etching solution that sample is invaded
Erosion, after specimen surface becomes canescence, is carried out, dries up.
In step (1), the described steel a size of length of side is the square sample of 10～20mm.
In step (2), etching solution mass ratio used is: ethanol: nitric acid=1:50.
Step configures nital in (2) at normal temperatures, the burnishing surface of sample is immersed nitric acid ethanol molten
In liquid 10～20s, when canescence occurs in specimen surface, rinse with water, with alcoholic solution, water is cleaned the most again
Fall, then with hair-dryer, specimen surface is dried up, examine under a microscope, it is possible to observe reticulated carbon clearly
Compound is distributed at beginning austenite grain boundary, and the martensite of austenite crystal intragranular also is able to clearly indicate out simultaneously
Come.
The present invention be directed to GCr15SiMn high-carbon-chromium bearing steel Austenite Grain Growth experiment austenite grain boundary be difficult to corrode and grasp
Make loaded down with trivial details problem, it is provided that a kind of short-cut method that can clearly demonstrate its original austenite grain, and simultaneously by austenite
The martensite of intra-die shows.By specific heat treatment method so that pro-eutectoid proeutectoid carbide is at austenite grain boundary
Sentence netted form to separate out, coordinate nital to corrode at normal temperatures, according to proeutectoid carbide and martensitic structure to invading
The resistance to degree of corrosion of erosion liquid is different, is able to the proeutectoid carbide at by austenite grain boundary and corrodes out, and by proeutectoid carbide net
Size reflects the size of austenite crystal.This kind of method corrosion process step is simple, it is easy to operation, and stability is strong, after erosion
Effect clear, it is easy to quantitative statistics, thus grasp austenite grain growth behavior, show austenite crystal intragranular simultaneously
Martensite, can be with quantitative observation martensite and the orientation relationship of austenite and the size of statistics martensitic needles.
Accompanying drawing explanation
Fig. 1: specimen size be the GCr15SiMn steel heating-up temperature of 10mm × 10mm × 10mm be 1000 DEG C, insulation
15min, is then cooled to 690 DEG C with 0.5 DEG C/s, the grain size photo after shrend.
Fig. 2: specimen size be the GCr15SiMn steel heating-up temperature of 15mm × 15mm × 15mm be 1000 DEG C, insulation
15min, is then cooled to 710 DEG C with 0.5 DEG C/s, the grain size photo after shrend.
Fig. 3: specimen size be the GCr15SiMn steel heating-up temperature of 20mm × 20mm × 20mm be 1100 DEG C, be incubated 5min,
Then it is cooled to 710 DEG C with 0.5 DEG C/s, the grain size photo after shrend.
Detailed description of the invention
1, the square sample that the length of side is 10～20mm is cut, the setting long big experiment of crystal grain is temperature required, time parameter, will heating
Furnace temperature rises to established temperature, and then sample inserts heating furnace insulation, and insulation is cooled to 0.1～0.5 DEG C/s after terminating
690～730 DEG C, then Quenching Treatment.
2, will cut in the middle of sample, at 240#, 400#, 600#, 800#, 1000#, 1200#, (i.e. granularity is respectively 240
Mesh, 400 mesh, 600 mesh, 800 mesh, 1000 mesh, 1200 mesh) on abrasive paper for metallograph by thick to carefully roughly grinding.Change every time
Ensure before sand paper specimen surface without being perpendicular to polish direction cut, sample half-twist angle when changing sand paper, after through 1000#
Coated abrasive working.After roughly grinding, sample polished surface is on the sand paper of 1500# and 2000# (i.e. granularity is at 1500 mesh and 2000 mesh)
Carry out water mill, be polished to no marking after water mill.Polishing agent uses 2.5 μm diamond polishing cream, makees lubricant with water,
Finally polished sample is dried.
3, nital is configured under room temperature, by burnishing surface leaching people's nital of sample 10～20s, when sample table
There is canescence in face, rinses with water, is washed by water with alcoholic solution, then dried up by specimen surface with hair-dryer,
Basis of microscopic observation, it is possible to observe that net carbide is distributed at beginning austenite grain boundary clearly, austenite crystal intragranular simultaneously
Martensite also be able to clearly indicate out.
Agent prescription: nitric acid: ethanol :=1:50.
Preparation of reagents method: take clean beaker, adds 20ml alcoholic solution, is subsequently adding 0.4ml salpeter solution, and mixing is all
Even.
Embodiment 1:
Selecting have the GCr15SiMn steel stocking of Morphology of pearlite as sample, described GCr15SiMn steel is that chemical composition is:
C:1.02%, Si:0.55%, Mn:1.07%, Cr:1.49%, processing method comprises the following steps:
1, cut 10mm × 10mm × 10mm bulk sample, the heating-up temperature of long for crystal grain big experiment be set as 1000 DEG C,
Insulation 15min, is then cooled to 690 DEG C with 0.5 DEG C/s, then Quenching Treatment.
2, will cut in the middle of sample, at 240#, 400#, 600#, 800#, 1000#, 1200#, (i.e. granularity is respectively 240
Mesh, 400 mesh, 600 mesh, 800 mesh, 1000 mesh, 1200 mesh) on abrasive paper for metallograph by thick to carefully roughly grinding.Change every time
Ensure before sand paper specimen surface without being perpendicular to polish direction cut, sample half-twist angle when changing sand paper, after through 1000#
Coated abrasive working.After roughly grinding, sample polished surface is on the sand paper of 1500# and 2000# (i.e. granularity is at 1500 mesh and 2000 mesh)
Carry out water mill, be polished to no marking after water mill.Polishing agent uses 2.5 μm diamond polishing cream, makees lubricant with water,
Finally polished sample is dried.
3, nital is configured under room temperature, by burnishing surface leaching people's nital of sample 10～20s, when sample table
There is canescence in face, rinses with water, is washed by water with alcoholic solution, then dried up by specimen surface with hair-dryer,
Basis of microscopic observation, it is possible to observe that net carbide is distributed at beginning austenite grain boundary clearly, austenite crystal intragranular simultaneously
Martensite also be able to clearly indicate out.
Agent prescription: nitric acid: ethanol :=1:50～2:50.
Preparation of reagents method: take clean beaker, adds 20ml alcoholic solution, is subsequently adding 0.4～0.8ml salpeter solution, mixed
Close uniformly.
Embodiment 2:
Selecting have the GCr15SiMn steel stocking of Morphology of pearlite as sample, described GCr15SiMn steel is that chemical composition is:
C:1.02%, Si:0.55%, Mn:1.07%, Cr:1.49%, processing method comprises the following steps:
1, cut 15mm × 15mm × 15mm bulk sample, the heating-up temperature of long for crystal grain big experiment be set as 1000 DEG C,
Insulation 15min, is then cooled to 710 DEG C with 0.5 DEG C/s, then Quenching Treatment.
2, will cut in the middle of sample, at 240#, 400#, 600#, 800#, 1000#, 1200#, (i.e. granularity is respectively 240
Mesh, 400 mesh, 600 mesh, 800 mesh, 1000 mesh, 1200 mesh) on abrasive paper for metallograph by thick to carefully roughly grinding.Change every time
Ensure before sand paper specimen surface without being perpendicular to polish direction cut, sample half-twist angle when changing sand paper, after through 1000#
Coated abrasive working.After roughly grinding, sample polished surface is on the sand paper of 1500# and 2000# (i.e. granularity is at 1500 mesh and 2000 mesh)
Carry out water mill, be polished to no marking after water mill.Polishing agent uses 2.5 μm diamond polishing cream, makees lubricant with water,
Finally polished sample is dried.
3, nital is configured under room temperature, by burnishing surface leaching people's nital of sample 10～20s, when sample table
There is canescence in face, rinses with water, is washed by water with alcoholic solution, then dried up by specimen surface with hair-dryer,
Basis of microscopic observation, it is possible to observe that net carbide is distributed at beginning austenite grain boundary clearly, austenite crystal intragranular simultaneously
Martensite also be able to clearly indicate out.
Agent prescription: nitric acid: ethanol :=1:50～2:50.
Preparation of reagents method: take clean beaker, adds 20ml alcoholic solution, is subsequently adding 0.4～0.8ml salpeter solution, mixed
Close uniformly.
Embodiment 3:
Selecting have the GCr15SiMn steel stocking of Morphology of pearlite as sample, described GCr15SiMn steel is that chemical composition is:
C:1.02%, Si:0.55%, Mn:1.07%, Cr:1.49%, processing method comprises the following steps:
1, cut 20mm × 20mm × 20mm bulk sample, the heating-up temperature of long for crystal grain big experiment be set as 1100 DEG C,
Insulation 15min, is then cooled to 710 DEG C with 0.5 DEG C/s, then Quenching Treatment.
2, will cut in the middle of sample, at 240#, 400#, 600#, 800#, 1000#, 1200#, (i.e. granularity is respectively 240
Mesh, 400 mesh, 600 mesh, 800 mesh, 1000 mesh, 1200 mesh) on abrasive paper for metallograph by thick to carefully roughly grinding.Change every time
Ensure before sand paper specimen surface without being perpendicular to polish direction cut, sample half-twist angle when changing sand paper, after through 1000#
Coated abrasive working.After roughly grinding, sample polished surface is on the sand paper of 1500# and 2000# (i.e. granularity is at 1500 mesh and 2000 mesh)
Carry out water mill, be polished to no marking after water mill.Polishing agent uses 2.5 μm diamond polishing cream, makees lubricant with water,
Finally polished sample is dried.
3, nital is configured under room temperature, by burnishing surface leaching people's nital of sample 10～20s, when sample table
There is canescence in face, rinses with water, is washed by water with alcoholic solution, then dried up by specimen surface with hair-dryer,
Basis of microscopic observation, it is possible to observe that net carbide is distributed at beginning austenite grain boundary clearly, austenite crystal intragranular simultaneously
Martensite also be able to clearly indicate out.
Agent prescription: nitric acid: ethanol :=1:50～2:50.
Preparation of reagents method: take clean beaker, adds 20ml alcoholic solution, is subsequently adding 0.4～0.8ml salpeter solution, mixed
Close uniformly.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, it is possible to understand that
Without departing from these embodiments being carried out multiple change in the case of the principle of the present invention and spirit, revise, replace and modification,
The scope of the present invention is limited by claims and equivalent thereof.
Claims (3)
1. the method simultaneously showing bearing steel austenite grain boundary and intracrystalline martensite, it is characterised in that comprise the following steps:
(1) steel are processed into the sample of regular shape, then sample are inserted in the heating furnace rising to predetermined temperature, insulation
Carry out slow cooling process after the scheduled time, after slow cooling to specified temp, carry out shrend；Described heating furnace predetermined temperature is
1000～1100 DEG C, temperature retention time is 5～20min；Slow cooling cooling rate is 0.1～0.5 DEG C/s, and then slow cooling to 690～730 DEG C is carried out
Quenching Treatment；
(2) sample after heat treatment is roughly ground, fine grinding and polishing, use etching solution that sample is eroded, treat sample
After surface becomes canescence, it is carried out, dries up；Etching solution mass ratio used is ethanol: nitric acid=1:50.
A kind of method simultaneously showing bearing steel austenite grain boundary and intracrystalline martensite, its feature exists
In: in step (1), the described steel a size of length of side is the square sample of 10～20mm.
A kind of method simultaneously showing bearing steel austenite grain boundary and intracrystalline martensite, its feature exists
In: step configures nital in (2) at normal temperatures, by the burnishing surface immersion nital of sample 10～20s,
When canescence occurs in specimen surface, rinse with water, with alcoholic solution, water is washed the most again, then with hair-dryer by specimen surface
Dry up, examine under a microscope, it is possible to observe that net carbide is distributed at beginning austenite grain boundary clearly, Ovshinsky simultaneously
Martensite in body crystal grain also is able to clearly indicate out.
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| CN114184613A (en) * | 2021-12-07 | 2022-03-15 | 江苏天鼎检测科技有限公司 | Method capable of clearly displaying carbide |
| CN114324081B (en) * | 2021-12-30 | 2024-04-02 | 中国航空工业集团公司金城南京机电液压工程研究中心 | Martensitic stainless steel grain forming and displaying method |
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