CN103217446A - Embedding intersection method - Google Patents
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- CN103217446A CN103217446A CN2013101313564A CN201310131356A CN103217446A CN 103217446 A CN103217446 A CN 103217446A CN 2013101313564 A CN2013101313564 A CN 2013101313564A CN 201310131356 A CN201310131356 A CN 201310131356A CN 103217446 A CN103217446 A CN 103217446A
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Abstract
The invention discloses an embedding intersection method comprising the following steps of: observing the fracture morphology of a fracture metallographic specimen under a scanning electron microscope to determine the intersection manner of the fracture and the grinding position of the fracture surface; embedding an embedding material in the fracture surface; grinding the fracture surface according to the determined grinding position of the fracture surface to obtain a ground surface; corroding the ground surface through a metallographic corrosive; observing the tissues of the ground surface under an optical microscope to obtain tissue signatures; removing the embedding material in the fracture surface; and observing the tissue signatures of the intersection region and the morphology features of the fracture under the scanning electron microscope. The method disclosed by the invention is used for obtaining the direct relation between the information and the microstructure and morphology of the material fracture.
Description
Technical field
The present invention relates to material fracture metallographic detection range, specifically, relate to a kind of method of hand over cutting of inlaying, be used to obtain contacting directly between information on the material fracture and tissue topography.
Background technology
The fracture and the tissue of material have confidential relation, and the microstructure of material influences the fracture process of material significantly.In fracture analysis, often fracture apperance and metallographic structure feature need be connected consideration, this analysis-by-synthesis has been subjected to general attention in fracture research.Also can solve some problem though carry out fracture and metallographic examination respectively, can not be directly at the corresponding relation of determining on the micro-scale between fracture and the tissue signature.For this reason, the fracture metallographic technique have been produced.After scanning electron microscope is come out, because it has the resolution height, Masaru Ibuka, advantage such as the visual field is wide has promoted the development of fracture metallographic technique.In the fractography technology the most normal use be direct etch method, this method is that the fracture that cleans is not inlayed, sanding and polishing not, directly fracture face is carried out the method that chemistry (or galvanochemistry) is handled, the fracture of corrosion is put into scanning electron microscope to be observed, this method is simple, uses the proper image that just can obtain on the fracture apperance stack tissue morphology, but this method can't be obtained contacting directly between information on the fracture and tissue topography.
Summary of the invention
Technical matters to be solved by this invention provides a kind of method of hand over cutting of inlaying, and is used to obtain contacting directly between information on the material fracture and tissue topography.
Technical scheme of the present invention is as follows:
A kind of inlaying handed over the method for cutting, and comprising: observe the fracture apperance of fractography sample under scanning electron microscope, determine that the friendship of described fracture cuts the polishing position of mode and fracture face; Inlay described fracture face with inlay; According to the polishing position of the described fracture face of determining, the polishing fracture face obtains flour milling; Corrode described flour milling with metallographic etching agent; Under optical microscope, described flour milling is carried out structure observation and obtain tissue signature; Remove the inlay on the described fracture face; Under scanning electron microscope, observe and hand over section tissue signature in district and the shape characteristic of described fracture.
Further: under scanning electron microscope, observe before the fracture apperance of fractography sample, check described fracture face,, then clean described fracture face if described fracture face has pollution.
Further: the mode of cleaning described fracture face is for using the ultrasonic cleaning that is placed with acetone soln.
Further: remove before the inlay on the described fracture face, that observes described fractography sample friendship section district under scanning electron microscope organizes whether appear clear, if unintelligible, then the fracture face that described friendship is cut the district is polished and to corrode the organization exposure that makes described friendship cut the district clear again.
Further: the friendship mode of cutting of described fracture comprises bevel and abscissuses.
Further: the method that adopts heat to inlay is inlayed described inlay, and inlaying temperature is 150 ℃～180 ℃.
Further: described inlay comprises acryl resin and Polyvinylchloride.
Further: the angle between described flour milling and the described fracture face is 20 °～45 °.
Further, the inlay of removing on the described fracture face comprises: adopt mechanical means to remove the inlay of described fracture face periphery and bottom; Dissolve described fractography sample, dissolution time is 5 hours～72 hours; Adopt the described fracture face of ultrasonic cleaning.
Further: the solution that dissolves described fractography sample comprises acetone.
Technique effect of the present invention is as follows:
The method of hand over cutting of inlaying of the present invention can solve fracture and learns and the histological problem of contacting directly, and is used to obtain contacting directly between information on the material fracture and tissue topography.
Description of drawings
Fig. 1 is a fractography sample of the present invention observation place synoptic diagram;
Fig. 2 is the metallographic structure figure of embodiments of the invention;
Fig. 3 is the fracture apperance scanning electron microscope diagram of embodiments of the invention;
Fig. 4 is the fractography scanning electron microscope diagram of embodiments of the invention.
Embodiment
Below with reference to accompanying drawing and preferred embodiment, technical scheme of the present invention is described in detail.
Of the present invention inlaying hands over the step of the method for cutting to comprise:
Step S1: the fracture face of checking the fractography sample.
With the naked eye, magnifier or microscope etc. are checked the macrostate of fractography sample.If this fracture face has pollution, then, make the fracture face cleaning with this fracture face of ultrasonic cleaning that is placed with acetone soln.
Step S2: observe the fracture apperance of fractography sample under scanning electron microscope, the friendship of determining fracture cuts the polishing position of mode (bevel and abscissus) and fracture face.For the more sample of section fluctuating, abscissusing often to obtain more friendship transversal.Because each projection all may form a little flour milling, its periphery then constitutes the friendship transversal.And bevel is toward the friendship transversal that firmly can only obtain complications.
Fractography sample after cleaning is put into scanning electron microscope carry out microscopic observation, tentatively determine the shape characteristic of fracture face to be observed, determine that according to the appearance feature of the fracture face of determining to be observed the friendship of fracture cuts the polishing position and the degree of depth of mode and fracture face.
Step S3: inlay fracture face with inlay.
The method that adopts heat to inlay is inlayed inlay on fracture face, inlaying temperature is 150 ℃～180 ℃.Strict relatively in the selection of inlay, should satisfy following requirement:
(1) hardness of inlay and steel sample hardness are approaching, Vickers hardness difference △ HV≤30.Vickers hardness differs 30 tensile strength and differs about 100MPa.Can make the fracture face good seal performance like this, be easy to obtain smooth metallographic flour milling during polishing.
(2) inlay not with the metallographic etching agent chemically reactive, suffer damage to exempt from transversal both sides metallographic and fracture apperance.
(3) inlay is wanted thoroughly to remove easily, and this is the important assurance that recovers the original pattern of fracture.
(4) inlay requires water white transparency, so that effect is inlayed in inspection, for example, has or not bubble and cracking etc., and determines to hand over cut position to put.
The general inlay of selecting is acryl resin and Polyvinylchloride.
Step S4: according to the polishing position of the fracture face of determining, the polishing fracture face obtains flour milling.
According to the polishing position of the fracture face of determining, select the angle and the degree of depth of polishing.Angle between flour milling and the fracture face to be observed is 20 °～45 °.If angle is less than 20 °, then the edge filler peels off easily; If angle greater than 45 °, then is subjected to the restriction of the depth of field of scanning electron microscope, can't be clear in imaging under the high power.For the more sample of section fluctuating, adopt the angle of abscissusing often can obtain more friendship transversal, because each projection all may form a flour milling.
Step S5: corrode flour milling with metallographic etching agent.
Because fracture always rise and fall rise and fall than tissue big many, so during with sem observation in order to obtain good stereoeffect, it is darker that the extent of corrosion of flour milling tissue corrodes when analyzing with ordinary optical microscope.Deep etch can be coordinated the contrast difference of fracture face and tissue surface, obtains the better image quality.
Step S6: under optical microscope, flour milling is carried out structure observation and obtain tissue signature.
The fractography sample is placed on carries out structure observation under the optical microscope, observe and note tissue signature.
Step S7: that observes fractography sample friendship section district under scanning electron microscope organizes whether appear clear.
Fractography sample after will under optical microscope, observing put under the scanning electron microscope observe hand over cut the district organize whether appear clear.If do not reach the requirement of sharpness, then hand over the organization exposure that cuts the district clear to handing over the fracture face that cuts the district to polish again and corrode to make.
Step S8: remove the inlay on the fracture face.
Adopt mechanical means to remove the inlay of fracture face periphery and bottom.With acetone solution fractography sample, make organic inlay dissolving, dissolution time is 5 hours～72 hours.Inlay is generally organic inlay, therefore adopts organic solvent not clean and the metallographic structure of corrosion can be destroyed.To often change acetone solvent in the course of dissolution.When finishing, adopt the ultrasonic cleaning fracture face near dissolving.
Step S9: under scanning electron microscope, observe and hand over section tissue signature in district and the shape characteristic of fracture.
Adopt sem observation to hand over section tissue signature in district and the shape characteristic of fracture.Because the fluctuating of fracture is greater than the fluctuating of tissue, the signal of scanning electron microscope should adopt nonlinear system.Because the mean flow rate of fracture and metallographic structure also there are differences, so should will hand over transversal parallel with the sample stage of scanning electron microscope, be fracture visual field and metallographic visual field with respect to the detecting device of scanning electron microscope be front and back position, reach and hand over the transversal purpose parallel with sample stage by regulating position, θ angle.The θ angle can tilt to realize by sample stage.As shown in Figure 1, be the synoptic diagram of the relative detector location in sample visual field.Sample 1 comprises fracture face 2 and metallographic face 3.When using sem observation, electron beam 4 is penetrated on sample 1.
Embodiment 1
With bainitic steel brittle fracture fracture is that embodiment illustrates that the present invention is used for inlaying of fractography technology and hands over the method for cutting.
At first with the naked eye check the macrostate of fractography sample, adopt the ultrasound wave that is placed with acetone soln to clean.
The macroscopic observation fracture, nothing that fracture face is straight rises and falls, and is typical brittle fracture.
After the cleaning fractography sample is put into scanning electron microscope and carry out microscopic observation, determine that fracture is characterized as intergranular fracture.Because it is obviously concavo-convex that fracture face does not have, so adopt the bevel mode and polish.
The employing Polyvinylchloride is an inlay, uses hot pointing machine that the whole fracture face of being materialsed is inlayed.Design temperature is 160 ℃, inlay is melted and the covering fracture face.When finish inlay after, hot pointing machine takes out sample after naturally cooling to room temperature.
Determine to cover the polishing position of the fracture sample of inlay, select the angle and the degree of depth of polishing, flour milling is 30 ° with angle between the fracture face that needs observation.Polishing sample process is followed successively by corase grind, correct grinding, polishing.The nital of the sample flour milling immersion 4% after the polishing corrodes.It is dark when flour milling organizes extent of corrosion to analyze than ordinary optical microscope.
Sample after the corrosion carries out structure observation under optical microscope.As shown in Figure 2, be the metallographic structure figure of embodiments of the invention.This flour milling is organized as the bainite+martensitic stucture that adopts the corrosion of 4% nitric acid alcohol.
Fractography sample after will observing under optical microscope is put into to observe under the scanning electron microscope and is handed over the tissue that cuts the district, and it is clear that this district organizes.
From scanning electron microscope, take out the fractography sample, at first adopt mechanical means that the inlay of periphery and bottom is removed.Again the fractography sample is put into acetone soln and dissolve, course of dissolution is 24 hours.Three replacing acetone solvents in the course of dissolution.When finishing, adopt ultrasound wave to clean, make the fracture cleaning near dissolving.The cleaning process of Polyvinylchloride still keeps intact metallographic structure.
At first adopt the sem observation fracture face.The signal of scanning electron microscope should adopt nonlinear system.Reach the friendship transversal purpose parallel by regulating position, θ angle with the sample stage of scanning electron microscope.The position of regulating the θ angle tilts to realize by sample stage.As shown in Figure 3, be the fracture apperance scanning electron microscope diagram of embodiments of the invention.The fracture apperance of this sample is the intergranular fracture that has secondary cracks.Observe again and hand over the tissue signature and the fracture apperance feature of cutting the district.As shown in Figure 4, be the fractography scanning electron microscope diagram of embodiments of the invention.As can be seen from Figure 4, inlay friendship and cut the fluctuating of the fluctuating of the fracture under the method greater than tissue.The secondary cracks that can clearly be seen that fracture upper edge crystalline substance among the figure ftractures along the crystal boundary in the metallographic structure, and crackle is arranged essentially parallel to martensitic needles.
Can solve fracture and learn and the histological problem of contacting directly by the method for hand over cutting of inlaying of the present invention, can obtain contacting directly between information on the material fracture and tissue topography.
Claims (10)
1. inlay a friendship section method for one kind, comprising:
Under scanning electron microscope, observe the fracture apperance of fractography sample, determine that the friendship of described fracture cuts the polishing position of mode and fracture face;
Inlay described fracture face with inlay;
According to the polishing position of the described fracture face of determining, the polishing fracture face obtains flour milling;
Corrode described flour milling with metallographic etching agent;
Under optical microscope, described flour milling is carried out structure observation and obtain tissue signature;
Remove the inlay on the described fracture face;
Under scanning electron microscope, observe and hand over section tissue signature in district and the shape characteristic of described fracture.
2. as claimed in claim 1 inlaying handed over the method for cutting, and it is characterized in that: observe before the fracture apperance of fractography sample under scanning electron microscope, check described fracture face, if described fracture face has pollution, then clean described fracture face.
3. as claimed in claim 2 inlaying handed over the method for cutting, and it is characterized in that: the mode of cleaning described fracture face is for using the ultrasonic cleaning that is placed with acetone soln.
4. the method for cutting of handing over of inlaying as claimed in claim 1, it is characterized in that: remove before the inlay on the described fracture face, that observes described fractography sample friendship section district under scanning electron microscope organizes whether appear clear, if unintelligible, then the fracture face that described friendship is cut the district is polished and to corrode the organization exposure that makes described friendship cut the district clear again.
5. as claimed in claim 1 inlaying handed over the method for cutting, and it is characterized in that: the friendship mode of cutting of described fracture comprises bevel and abscissuses.
6. as claimed in claim 1 inlaying handed over the method for cutting, and it is characterized in that: the method that adopts heat to inlay is inlayed described inlay, and inlaying temperature is 150 ℃～180 ℃.
7. as claimed in claim 6 inlaying handed over the method for cutting, and it is characterized in that: described inlay comprises acryl resin and Polyvinylchloride.
8. as claimed in claim 1 inlaying handed over the method for cutting, and it is characterized in that: the angle between described flour milling and the described fracture face is 20 °～45 °.
9. as claimed in claim 1 inlaying handed over the method for cutting, and it is characterized in that the inlay of removing on the described fracture face comprises: adopt mechanical means to remove the inlay of described fracture face periphery and bottom; Dissolve described fractography sample, dissolution time is 5 hours～72 hours; Adopt the described fracture face of ultrasonic cleaning.
10. as claimed in claim 9 inlaying handed over the method for cutting, and it is characterized in that: the solution that dissolves described fractography sample comprises acetone.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013101313564A CN103217446A (en) | 2013-04-16 | 2013-04-16 | Embedding intersection method |
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| CN2013101313564A CN103217446A (en) | 2013-04-16 | 2013-04-16 | Embedding intersection method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109632851A (en) * | 2018-11-15 | 2019-04-16 | 包头钢铁（集团）有限责任公司 | A kind of analysis method that Fracture Profile in Metallic Materials is combined with metallographic structure |
| CN111982642A (en) * | 2020-06-07 | 2020-11-24 | 首钢集团有限公司 | Preparation method of EBSD sample of fracture sample section |
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Cited By (2)
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| CN111982642A (en) * | 2020-06-07 | 2020-11-24 | 首钢集团有限公司 | Preparation method of EBSD sample of fracture sample section |
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Application publication date: 20130724 |