CN109632852A - A kind of electron microscopic sample preparation method showing bainite structure at fracture surface - Google Patents
A kind of electron microscopic sample preparation method showing bainite structure at fracture surface Download PDFInfo
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- CN109632852A CN109632852A CN201811534604.9A CN201811534604A CN109632852A CN 109632852 A CN109632852 A CN 109632852A CN 201811534604 A CN201811534604 A CN 201811534604A CN 109632852 A CN109632852 A CN 109632852A
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- fracture
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
Abstract
The invention discloses a kind of electron microscopic sample preparation methods for showing bainite structure at fracture surface, pass through cleaning to steel material fracture, derusting, the again process that corrodes, realize that the tissue of incision position reproduces, method is simple, each solution used is prepared simple, strong to fracture apperance sensibility, the available fracture apperance tissue being perfectly clear can be used for daily fracture conventional detection.The method of the present invention realizes the structure observation of the incision position of bainitic steel, the tissue of incision position different-shape can be compared, Bainite Carbide is directly observed in the distribution of incision position and carbide size pattern, the means for enriching the measurement of bainitic steel fracture provide a kind of new morphology observation scheme.
Description
Technical field
The present invention, which relates to, belongs to metal material detection and analysis field, and in particular to one kind shows bainite structure at fracture surface
Electron microscopic sample preparation method.
Background technique
Materials microstructure and Fracture Morphology are the most basic physical features of steel material, are detected to materials microstructure normal
Based on detecting with metallographic, by the sample of detection position needed for cutting, pass through the means such as polishing, polishing, corrosion crystal boundary, Ke Yiyou
The tissue signature of effect observation various types of materials.And Fracture Profile in Metallic Materials morphology observation, mainly pass through scanning electron microscope or Stereo microscope etc.
Big depth of field detecting devices characterizes Fracture Profile in Metallic Materials pattern.
For the tissue signature of incision position, rarely has people's further investigation at present, main difficulty is fracture surface complex topography
It differs greatly with smooth surface required by metallographic sample preparation, and can not only obtain the feature of material fracture by metallographic observation.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of electron microscopic sample systems for showing bainite structure at fracture surface
Preparation Method.The invention observes its fractograph by certain means, can be used for material structure to material after material fracture
Expect the judgement of Effect on Mechanical Properties, and abundant Fracture Profile in Metallic Materials analysis means.
In order to solve the above technical problems, the technical solution used in the present invention is: one kind shows bainite at fracture surface
The electron microscopic sample preparation method of tissue, the preparation method comprises the following steps:
(1) sample size of bainite structure and height control need to not influenced to sweep by sample on the broken edge needed for preparing scanning electron microscope
In the range of retouching Electronic Speculum observation, cutting process is carried out to superelevation super large sample；
(2) physical cleaning is carried out to fracture surface, sample surfaces can be cleaned with high-speed flow, produced when removing sample fracture
Raw clast, should be avoided and collide with, and the modes such as beat, in order to avoid damage fracture；
(3) to fracture surface derusting oxide layer, the derusting time is 1~5min；
(4) fracture surface is corroded, 30~60s of etching time shows pattern tissue signature；
(5) sample on the broken edge prepared is fixed on sample platform of scanning electronic microscope, vacuumizes observation.
Step (1) sample on the broken edge of the present invention can be stretching fracture, impact fracture, fatigue fracture, compression fracture, turn round
Mouth absolutely.
Step (1) sample on the broken edge height of the present invention is less than 35mm, and fracture surface maximum gauge, that is, catercorner length is small
In 30mm.
Physical cleaning in step (2) of the present invention is cleared up in fracture gap using dehydrated alcohol ultrasonic cleaning
Impurity and dust.
Derusting in step (3) of the present invention, the derusting reagent used is the aqueous hydrochloric acid solution of volume fraction 3~5%.
After the completion of derusting process in step (3) of the present invention, sample is rinsed with dehydrated alcohol, and is blown with hair dryer
It is dry.
For fracture in step (3) of the present invention as relatively newer, the not oxidized pollution in surface can omit derusting and deoxidation
Layer process.
The corrosive liquid that corrosion uses in step (4) of the present invention is the nital of volume fraction 4%, after corrosion
It is rinsed with dehydrated alcohol, and to be measured with hair dryer drying.
Electron microscopic sample preparation method of the present invention is that analysis is pure, and water is pure water using reagent.
The beneficial effects of adopting the technical scheme are that 1, the method for the present invention realizes the fracture of bainitic steel
Locate structure observation, the tissue of incision position different-shape can be compared, to Bainite Carbide incision position distribution with
And carbide size pattern is directly observed, and the means of bainitic steel fracture measurement are enriched, and provides a kind of new pattern sight
Examine scheme.2, the cleaning of the invention by steel material fracture, derusting, the process corroded again, realize the tissue of incision position again
Existing, method is simple, and each solution used prepares simple, the available fracture apperance that is perfectly clear strong to fracture apperance sensibility
Tissue, can be used for daily fracture conventional detection.
Detailed description of the invention
Fig. 1 is bainite structure shape appearance figure at 40CrMnMoVA steel impact fracture in embodiment 1；
Fig. 2 is bainite structure shape appearance figure at SX780CF steel stretching fracture in embodiment 2；
Fig. 3 is bainite structure shape appearance figure at 14Cr1MoR steel fatigue fracture in embodiment 3；
Fig. 4 is that 30CrMoA steel compresses incision position bainite structure shape appearance figure in embodiment 4；
Fig. 5 is that 20Cr2MoNiA steel twists off incision position bainite structure shape appearance figure in embodiment 5；
Fig. 6 is bainite structure shape appearance figure at 30Ni2CrMnMoVA steel stretching fracture in embodiment 6；
Fig. 7 is bainite structure shape appearance figure at WSD690E steel impact fracture in embodiment 7；
Fig. 8 is 20CrMoA steel incision position bainite structure shape appearance figure in embodiment 8.
Specific embodiment
The present invention is described in further detail in the following with reference to the drawings and specific embodiments.
Embodiment 1
The observation of bainite structure pattern, mainly comprises the steps that at the present embodiment 40CrMnMoVA steel impact fracture
(1) taking 40CrMnMoVA steel impact fracture is sample to be tested, sample to be seen is cut, by impact fracture sample
Height is switched to as 3mm, carries out grinding process to impact sample burr；
(2) dehydrated alcohol ultrasonic cleaning is used, impurity and dust in fracture gap are cleared up；
(3) rusty scale of fracture surface is cleaned using the aqueous hydrochloric acid solution of volume fraction 3%, by fracture surface in hydrochloric acid water
It is stirred in solution, removes fracture surface oxide, derust time 2min, after the completion of the process that derusts, is rinsed, is used in combination with dehydrated alcohol
Hair dryer drying；
(4) by the fracture surface for the sample that derusted, corrosion treatment is carried out to sample with 4% nital of volume fraction, is corroded
Time 45s, is rinsed after corrosion with dehydrated alcohol, and is dried up with hair dryer；
(5) sample on the broken edge prepared is fixed on sample platform of scanning electronic microscope, is vacuumized, fracture is observed using secondary electron image
Surface.
Bainite structure shape appearance figure is shown in Fig. 1 at the present embodiment 40CrMnMoVA steel impact fracture, available as shown in Figure 1
Bainite Morphology tissue at the 40CrMnMoVA steel impact fracture being perfectly clear.
Embodiment 2
The observation of bainite structure pattern, mainly comprises the steps that at the present embodiment SX780CF steel stretching fracture
(1) take SX780CF steel stretching fracture be sample to be tested, by stretch sample carry out being cut to length along its length be
2.5mm carries out grinding process to sample burr is stretched；
(2) dehydrated alcohol ultrasonic cleaning is used, impurity and dust in fracture gap are cleared up；
(3) rusty scale of fracture surface is cleaned using the aqueous hydrochloric acid solution of volume fraction 4%, by fracture surface in hydrochloric acid water
It is stirred in solution, removes fracture surface oxide, derust time 4min, after the completion of the process that derusts, is rinsed, is used in combination with dehydrated alcohol
Hair dryer drying；
(4) by the fracture surface for the sample that derusted, corrosion treatment is carried out to sample with 4% nital of volume fraction, is corroded
Time 60s, is rinsed after corrosion with dehydrated alcohol, and is dried up with hair dryer；
(5) sample on the broken edge prepared is fixed on sample platform of scanning electronic microscope, is vacuumized, fracture is observed using secondary electron image
Surface.
Bainite structure shape appearance figure is shown in Fig. 2 at the present embodiment SX780CF steel stretching fracture, available non-as shown in Figure 2
Often Bainite Morphology tissue at clear SX780CF steel stretching fracture.
Embodiment 3
The observation of bainite structure pattern, mainly comprises the steps that at the present embodiment 14Cr1MoR steel fatigue fracture
(1) take 14Cr1MoR steel fatigue fracture for sample to be tested, fatigue fracture height of specimen 15mm, surface maximum length 10mm,
Grinding process is carried out to the fatigue samples burr；
(2) dehydrated alcohol ultrasonic cleaning is used, impurity and dust in fracture gap are cleared up；
(3) rusty scale of fracture surface is cleaned using the aqueous hydrochloric acid solution of volume fraction 5%, by fracture surface in hydrochloric acid water
It is stirred in solution, removes fracture surface oxide, derust time 3min, after the completion of the process that derusts, is rinsed, is used in combination with dehydrated alcohol
Hair dryer drying；
(4) by the fracture surface for the sample that derusted, corrosion treatment is carried out to sample with 4% nital of volume fraction, is corroded
Time 35s, is rinsed after corrosion with dehydrated alcohol, and is dried up with hair dryer；
(5) sample on the broken edge prepared is fixed on sample platform of scanning electronic microscope, is vacuumized, fracture is observed using secondary electron image
Surface.
Bainite structure shape appearance figure is shown in Fig. 3 at the present embodiment 14Cr1MoR steel fatigue fracture, available non-as shown in Figure 3
Often Bainite Morphology tissue at clear 14Cr1MoR steel fatigue fracture.
Embodiment 4
The present embodiment 30CrMoA steel compresses the observation of incision position bainite structure pattern, mainly comprises the steps that
(1) taking 30CrMoA steel compression fracture is sample to be tested, compression sample height is cut to 12mm, to compression sample burr
Carry out grinding process；
(2) dehydrated alcohol ultrasonic cleaning is used, impurity and dust in fracture gap are cleared up；
(3) rusty scale of fracture surface is cleaned using the aqueous hydrochloric acid solution of volume fraction 3.5%, by fracture surface in hydrochloric acid
It is stirred in aqueous solution, removes fracture surface oxide, derust time 1min, after the completion of the process that derusts, rinsed with dehydrated alcohol, and
It is dried up with hair dryer；
(4) by the fracture surface for the sample that derusted, corrosion treatment is carried out to sample with 4% nital of volume fraction, is corroded
Time 40s, is rinsed after corrosion with dehydrated alcohol, and is dried up with hair dryer；
(5) sample on the broken edge prepared is fixed on sample platform of scanning electronic microscope, is vacuumized, fracture is observed using secondary electron image
Surface.
The present embodiment 30CrMoA steel compression incision position bainite structure shape appearance figure is shown in Fig. 4, available non-as shown in Figure 4
Often clearly 30CrMoA steel compresses incision position Bainite Morphology tissue.
Embodiment 5
The present embodiment 20Cr2MoNiA steel twists off the observation of incision position bainite structure pattern, mainly comprises the steps that
(1) taking 20Cr2MoNiA steel to twist off fracture is sample to be tested, the height of specimen 20mm, surface diameter 8mm, to twisting off sample
Burr carries out grinding process；
(2) dehydrated alcohol ultrasonic cleaning is used, impurity and dust in fracture gap are cleared up；
(3) rusty scale of fracture surface is cleaned using the aqueous hydrochloric acid solution of volume fraction 4.5%, by fracture surface in hydrochloric acid
It is stirred in aqueous solution, removes fracture surface oxide, derust time 5min, after the completion of the process that derusts, rinsed with dehydrated alcohol, and
It is dried up with hair dryer；
(4) by the fracture surface for the sample that derusted, corrosion treatment is carried out to sample with 4% nital of volume fraction, is corroded
Time 30s, is rinsed after corrosion with dehydrated alcohol, and is dried up with hair dryer；
(5) sample on the broken edge prepared is fixed on sample platform of scanning electronic microscope, is vacuumized, fracture is observed using secondary electron image
Surface.
The present embodiment 20Cr2MoNiA steel twists off incision position bainite structure shape appearance figure and sees Fig. 5, available as shown in Figure 5
The 20Cr2MoNiA steel being perfectly clear twists off incision position Bainite Morphology tissue.
Embodiment 6
The observation of bainite structure pattern, mainly comprises the steps that at the present embodiment 30Ni2CrMnMoVA stretching fracture
(1) taking 30Ni2CrMnMoVA stretching fracture is sample to be tested, and it is 10mm, surface that 30Ni2CrMnMoVA, which stretches height of specimen,
Diameter 8.5mm stretches sample burr to 30Ni2CrMnMoVA and carries out grinding process；
(2) dehydrated alcohol ultrasonic cleaning is used, impurity and dust in fracture gap are cleared up；
(3) rusty scale of fracture surface is cleaned using the aqueous hydrochloric acid solution of volume fraction 3.8%, by fracture surface in hydrochloric acid
It is stirred in aqueous solution, removes fracture surface oxide, derust time 4.5min, after the completion of the process that derusts, rinsed with dehydrated alcohol,
And it is dried up with hair dryer；
(4) by the fracture surface for the sample that derusted, corrosion treatment is carried out to sample with 4% nital of volume fraction, is corroded
Time 43s, is rinsed after corrosion with dehydrated alcohol, and is dried up with hair dryer；
(5) sample on the broken edge prepared is fixed on sample platform of scanning electronic microscope, is vacuumized, fracture is observed using secondary electron image
Surface.
Bainite structure shape appearance figure is shown in Fig. 6 at the present embodiment 30Ni2CrMnMoVA stretching fracture, can obtain as shown in Figure 6
The Bainite Morphology tissue at the 30Ni2CrMnMoVA stretching fracture being perfectly clear.
Embodiment 7
The observation of bainite structure pattern, mainly comprises the steps that at the present embodiment WSD690E impact fracture
(1) taking WSD690E impact fracture is sample to be tested, which is 22.5mm, width 10mm, to WSD690E
It impacts sample burr and carries out grinding process；
(2) dehydrated alcohol ultrasonic cleaning is used, impurity and dust in fracture gap are cleared up；
(3) rusty scale of fracture surface is cleaned using the aqueous hydrochloric acid solution of volume fraction 4.7%, by fracture surface in hydrochloric acid
It is stirred in aqueous solution, removes fracture surface oxide, derust time 2.5min, after the completion of the process that derusts, rinsed with dehydrated alcohol,
And it is dried up with hair dryer；
(4) by the fracture surface for the sample that derusted, corrosion treatment is carried out to sample with 4% nital of volume fraction, is corroded
Time 55s, is rinsed after corrosion with dehydrated alcohol, and is dried up with hair dryer；
(5) sample on the broken edge prepared is fixed on sample platform of scanning electronic microscope, is vacuumized, fracture is observed using secondary electron image
Surface.
Bainite structure shape appearance figure is shown in Fig. 7 at the present embodiment WSD690E impact fracture, as shown in Figure 7 it is available very
Bainite Morphology tissue at clear WSD690E impact fracture.
Embodiment 8
The observation of the present embodiment 20CrMoA incision position bainite structure pattern, mainly comprises the steps that
(1) taking 20CrMoA fracture is sample to be tested, the height of specimen 11mm, surface diameter 6.5mm, to 20CrMoA sample burr
Carry out grinding process；
(2) dehydrated alcohol ultrasonic cleaning is used, impurity and dust in fracture gap are cleared up；
(3) rusty scale of fracture surface is cleaned using the aqueous hydrochloric acid solution of volume fraction 4.2%, by fracture surface in hydrochloric acid
It is stirred in aqueous solution, removes fracture surface oxide, derust time 3.5min, after the completion of the process that derusts, rinsed with dehydrated alcohol,
And it is dried up with hair dryer；
(4) by the fracture surface for the sample that derusted, corrosion treatment is carried out to sample with 4% nital of volume fraction, is corroded
Time 50s, is rinsed after corrosion with dehydrated alcohol, and is dried up with hair dryer；
(5) sample on the broken edge prepared is fixed on sample platform of scanning electronic microscope, is vacuumized, fracture is observed using secondary electron image
Surface.
The present embodiment 20CrMoA incision position bainite structure shape appearance figure is shown in Fig. 8, available as shown in Figure 8 to be perfectly clear
20CrMoA incision position Bainite Morphology tissue.
Above-described embodiment shows that the present invention by cleaning to steel material fracture, derusting, the again process that corrodes, realizes
The tissue of incision position reproduces, and method is simple, each solution used prepare it is simple, it is strong to fracture apperance sensibility, it is available very
Clear fracture apperance tissue, can be used for daily fracture conventional detection；The tissue of incision position different-shape can be carried out simultaneously
Compare, Bainite Carbide is directly observed in the distribution of incision position and carbide size pattern, enriches bainite
The means of steel fracture measurement provide a kind of new morphology observation scheme.
The above embodiments are only used to illustrate and not limit the technical solutions of the present invention, although referring to above-described embodiment to this hair
It is bright to be described in detail, those skilled in the art should understand that: still the present invention can be modified or be waited
With replacement, without departing from the spirit or scope of the invention, or any substitutions, should all cover in power of the invention
In sharp claimed range.
Claims (9)
1. a kind of electron microscopic sample preparation method for showing bainite structure at fracture surface, which is characterized in that the preparation method
The following steps are included:
(1) sample size of bainite structure and height control need to not influenced to sweep by sample on the broken edge needed for preparing scanning electron microscope
In the range of retouching Electronic Speculum observation, cutting process is carried out to superelevation super large sample；
(2) physical cleaning is carried out to fracture surface, sample surfaces can be cleaned with high-speed flow, produced when removing sample fracture
Raw clast, should be avoided and collide with, and the modes such as beat, in order to avoid damage fracture；
(3) to fracture surface derusting oxide layer, the derusting time is 1~5min；
(4) fracture surface is corroded, 30~60s of etching time shows pattern tissue signature；
(5) sample on the broken edge prepared is fixed on sample platform of scanning electronic microscope, vacuumizes observation.
2. a kind of electron microscopic sample preparation method for showing bainite structure at fracture surface according to claim 1, special
Sign is that step (1) sample on the broken edge can be stretching fracture, impact fracture, fatigue fracture, compress fracture, twists off fracture.
3. a kind of electron microscopic sample preparation method for showing bainite structure at fracture surface according to claim 1, special
Sign is that step (1) the sample on the broken edge height is less than 35mm, and fracture surface maximum gauge, that is, catercorner length is less than 30mm.
4. a kind of electron microscopic sample preparation method for showing bainite structure at fracture surface according to claim 1, special
Sign is, the physical cleaning in the step (2), using dehydrated alcohol ultrasonic cleaning, clear up impurity in fracture gap and
Dust.
5. a kind of electron microscopic sample preparation for showing bainite structure at fracture surface according to any one of claims 1-4
Method, which is characterized in that the derusting in the step (3), the derusting reagent used are water-soluble for the hydrochloric acid of volume fraction 3~5%
Liquid.
6. a kind of electron microscopic sample preparation for showing bainite structure at fracture surface according to any one of claims 1-4
Method, which is characterized in that after the completion of the derusting process in the step (3), sample is rinsed with dehydrated alcohol, and is blown with hair dryer
It is dry.
7. a kind of electron microscopic sample preparation for showing bainite structure at fracture surface according to any one of claims 1-4
Method, which is characterized in that for the fracture in the step (3) as relatively newer, the not oxidized pollution in surface can omit derusting and deoxidation
Change layer process.
8. a kind of electron microscopic sample preparation for showing bainite structure at fracture surface according to any one of claims 1-4
Method, which is characterized in that the corrosive liquid that corrosion uses in the step (4) is the nital of volume fraction 4%, corrosion
It is rinsed afterwards with dehydrated alcohol, and to be measured with hair dryer drying.
9. a kind of electron microscopic sample preparation for showing bainite structure at fracture surface according to any one of claims 1-4
Method, which is characterized in that the electron microscopic sample preparation method is that analysis is pure, and water is pure water using reagent.
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Cited By (1)
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| CN111076993A (en) * | 2019-12-12 | 2020-04-28 | 重庆市城投路桥管理有限公司 | Sample fracture treatment method |
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