CN105067414A - System and method for observing hard alloy structure with scanning electron microscope - Google Patents
System and method for observing hard alloy structure with scanning electron microscope Download PDFInfo
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Abstract
The invention discloses a method for observing a hard alloy structure with a scanning electron microscope. The method is characterized by comprising the following steps: embedding a hard alloy sample and polishing the embedded hard alloy sample; putting the polished sample in a corrosive liquid for sample corrosion; after the sample corrosion is finished, observing the microscopic structure of the treated hard alloy sample with the scanning electron microscope. The internal structure of an alloy product, particularly an ultrafine grain hard alloy or an alloy containing an additive cannot be clearly observed with the conventional optical metallographic microscope, so that the scanning electron microscope is needed for the observation; an alloy corrosion method directly impacts the observation effect and the accuracy of judging whether the phase differences reach the standards or not; through the adoption of a special corrosive liquid formula and a specific corrosion process, a clear and visualized structure picture can be obtained, the sizes, morphology and distribution of various phases can be effectively observed, the impact of the third phase of corrosion can be eliminated, and the improvement of product quality, the research and development of novel products, and the promotion and utilization of alloy grades can be facilitated.
Description
Technical field
The present invention relates to a kind of System and method for of scanning electron microscopic observation Mathematical Analysis of Al-li Alloy Containing Rare Earth, it adopts wimet particular etch formula of liquid and special etching process to carry out pre-treatment, afterwards, clearly show the microstructure of wimet microstructure and each phase by scanning electron microscope, can solve alloy product particularly ultra-fine and containing third phase product observe the difficult problem of interior tissue.
Background technology
Along with the fast development of wimet, hart metal product kind gets more and more.Particularly, due to metaloscope enlargement factor limitation in prior art, for alloy, particularly the alloy of ultra-fine grain and the alloy containing third phase, adopt traditional optical metallographic microscope clearly cannot obtain alloy product internal organizational structure.Namely use scanning electron microscope to observe alloy structure, under the excellent resolution and enlargement factor condition of scanning electron microscope, make corrosion liquid formula of the prior art and etching process can not meet the detection demand of Mathematical Analysis of Al-li Alloy Containing Rare Earth observation.
A kind of technical prejudice is there is in prior art, think follow the beaten track sampling traditionally, sample preparation, observation metallurgical structure right and proper, nobody thinks and should to improve the preliminary work of sample, and be the technical matters that solve, if more nobody considers to improve or change and could improve observation effect.
Summary of the invention
The object of this invention is to provide a kind of System and method for of scanning electron microscopic observation Mathematical Analysis of Al-li Alloy Containing Rare Earth, it is by novel etchant solution formula and Special Corrosion technique, make excellent sample, can solve by scanning electron microscopic observation wimet (particularly ultra-fine cemented carbide and the wimet containing third phase) the unsharp difficult problem of tissue.
For this reason, according to an aspect of the present invention, provide a kind of method of scanning electron microscopic observation Mathematical Analysis of Al-li Alloy Containing Rare Earth, it is characterized in that, the method comprises: inlay and polishing wimet sample; Sample after polishing is put into corrosive liquid, sample is corroded; After completing sample preparation, by the microstructure of scanning electron microscopic observation Mathematical Analysis of Al-li Alloy Containing Rare Earth.
Preferably, etchant solution comprises WC phase etchant solution and Co phase etchant solution.
Preferably, WC phase etchant solution comprises potassium hydroxide or NaOH and potassium ferricyanide aqueous solution equal volume mixed liquor; The concentration of each aqueous solution between 16-19%, preferably 17.5%; The concentration of each aqueous solution WC phase relevant to the etching time of sample etchant solution comprises potassium hydroxide or NaOH and potassium ferricyanide aqueous solution equal volume mixed liquor; The concentration of each aqueous solution between 16-19%, preferably 17.5%; The concentration of each aqueous solution is relevant to the etching time of sample.
Preferably, Co phase etchant solution comprises ferric trichloride hydrochloric acid saturated solution.
Preferably, for the alloy not containing adjuvant, first the sample making minute surface is put into WC etchant solution, soak 3min10s, complete WC phase to corrode, then sample is put into Co phase corrosive liquid, (all time fluctuations allow the scope at 2 seconds to corrosion 30s, if but wide fluctuations, then need the formula coordinating corrosive liquid).
Preferably, for the alloy having adjuvant, the sample making minute surface is first corroded Co phase 20s, then corrodes WC phase 3min10s, then corrode Co phase 10s.
Preferably, complete sample preparation and also comprise: to the sample purified rinse water through excessive erosion, then be placed in absolute ethyl alcohol, carry out ultrasonic cleaning and dry up.
According to another aspect of the present invention, provide a kind of system of scanning electron microscopic observation Mathematical Analysis of Al-li Alloy Containing Rare Earth, it is characterized in that, this system comprises: sample preparation device, and it has inlaying device and the burnishing device of wimet sample; Sample processing device, it is arranged on the downstream of sample preparation device, has corrosive liquid container; Sample preparation forming apparatus, it is arranged on the downstream of sample processing device, has the device to the sample purified rinse water through excessive erosion, absolute ethyl alcohol container, ultrasonic cleaning equipment and blow-dry device; And for observing the microstructural scanning electron microscope of Mathematical Analysis of Al-li Alloy Containing Rare Earth.
Preferably, corrosive liquid container comprises the WC phase etchant solution container accommodating 17.5% potassium hydroxide aqueous solution and 17.5% potassium ferricyanide aqueous solution equal volume mixed liquor and the Co phase etchant solution container holding ferric trichloride hydrochloric acid saturated solution.
Preferably, there is the time controller sample making minute surface being soaked in WC etchant solution 3min10s, and in Co phase corrosive liquid, soak the time controller of 10s, 20s, 30s.
In order to the observation using advanced scanning electron microscope to carry out Mathematical Analysis of Al-li Alloy Containing Rare Earth, must ensure that sample meets the testing requirement of scanning electron microscope, respectively clear and definite through corrosion threshold, crystal boundary appears clear and inexcessive, does not have the interference of third phase.The present invention, by described etchant solution formula and etching process, solves a difficult problem for sample production, solves the accurate detection of the institutional framework of wimet (particularly ultra-fine cemented carbide and the wimet containing third phase).
Accompanying drawing explanation
Fig. 1 is 0.4 micron of ultra-fine cemented carbide metallograph (1000X) in prior art.
Fig. 2 A is 0.4 micron of ultra-fine cemented carbide scanning electron microscope macrograph (10000X) in prior art.
Fig. 2 B is the present invention's 0.4 micron of ultra-fine cemented carbide scanning electron microscope macrograph (10000X).
Fig. 3 A is the wimet scanning electron microscope macrograph (5000X) containing third phase in prior art.
Fig. 3 B is the wimet scanning electron microscope macrograph (5000X) that the present invention contains third phase.
Fig. 4 is the structural representation of the system according to scanning electron microscopic observation Mathematical Analysis of Al-li Alloy Containing Rare Earth of the present invention.
Embodiment
According to the present invention, need to observe by scanning electron microscope, the caustic solution of alloy directly has influence on the effect that interior tissue is observed and the judgment accuracy that respectively whether phase is qualified; By Special Corrosion formula of liquid and the particular etch technique of caustic solution of the present invention, clear and intuitive macrograph can be obtained, effectively can observe the size of each phase, pattern and distribution, contribute to that product quality is improved, the research and development of new product, the promoting the use of of alloy designations.
Etchant solution of the present invention comprises: 1) WC phase etchant solution (17.5% potassium hydroxide aqueous solution and 17.5% potassium ferricyanide aqueous solution equal volume mixed liquor); 2) Co phase etchant solution (ferric trichloride hydrochloric acid saturated solution);
Etching process of the present invention is: for the alloy not containing adjuvant, first the sample making minute surface is put into WC etchant solution, soaks 3min10s, completes WC phase and corrode, then sample is put into Co phase corrosive liquid, corrosion 30s; For the alloy having adjuvant, first corrode Co phase 20s, then corrode WC phase 3min10s, then corrode Co phase 10s.
WC phase etchant solution comprises 17.5% potassium hydroxide/sodium hydrate aqueous solution and 17.5% potassium ferricyanide aqueous solution equal volume mixed liquor.The concentration of potassium hydroxide/sodium hydrate aqueous solution and potassium ferricyanide aqueous solution, between 16-19%, changes this formula and then wants corresponding change etching time.The fluctuation of sample soak time allows the scope at 2 seconds, if need wide fluctuations, then needs the formula adjusting corrosive liquid.
According to the present invention, comprise by the method for scanning electron microscopic observation Mathematical Analysis of Al-li Alloy Containing Rare Earth: choose wimet sample and carry out sample preparation, comprise inlay, polishing; Sample after polishing is put into the corrosive liquid of special formulation, corroded by specific etching process; Then use purified rinse water, then sample is placed in absolute ethyl alcohol and carries out ultrasonic cleaning and dry up, finally by scanning electron microscopic observation Mathematical Analysis of Al-li Alloy Containing Rare Earth microstructure.
As shown in Figure 4, the system of scanning electron microscopic observation Mathematical Analysis of Al-li Alloy Containing Rare Earth of the present invention comprises: sample preparation device 10, and it has inlaying device 11 and the burnishing device 12 of wimet sample 5; Sample processing device 20, it is arranged on the downstream of sample preparation device 10, has corrosive liquid container; Sample preparation forming apparatus 30, it is arranged on the downstream of sample processing device 20, has the device 31 to the sample purified rinse water through excessive erosion, absolute ethyl alcohol container 32, ultrasonic cleaning equipment 33 and blow-dry device 34; And for observing the microstructural scanning electron microscope 40 of Mathematical Analysis of Al-li Alloy Containing Rare Earth.
Preferably, corrosive liquid container comprises the WC phase etchant solution container 21 accommodating 17.5% potassium hydroxide aqueous solution and 17.5% potassium ferricyanide aqueous solution equal volume mixed liquor and the Co phase etchant solution container 22 holding ferric trichloride hydrochloric acid saturated solution.
Preferably, there is the time controller 23 sample making minute surface being soaked in WC etchant solution 3min10s, and in Co phase corrosive liquid, soak the time controller 24 of 10s, 20s, 30s.
Embodiment: Fig. 1, Fig. 2 A, Fig. 3 A is the macrograph after sample adopts the caustic solution corrosion of prior art.Fig. 1 is 0.4 micron of ultra-fine cemented carbide metallograph (1000X), wherein, due to the limited resolution of metaloscope, therefore cannot observe out the tissue topography of alloy, size and distribution.Fig. 2 A is 0.4 micron of ultra-fine cemented carbide scanning electron microscope macrograph (10000X), due to the caustic solution not for scanning electron microscope in prior art, continue to use etching pit method, the stereoscan photograph tissue contrast obtained is not obvious, and crystal boundary is not given prominence to.Fig. 3 A is the wimet scanning electron microscope macrograph (5000X) containing third phase, adopts the caustic solution of prior art to see that third phase has interference, hidden portion of tissue pattern and boundary, and the pattern of third phase is unintelligible.Fig. 2 B and Fig. 3 B is that sample is according to the electromicroscopic photograph after caustic solution corrosion of the present invention.Fig. 2 B is 0.4 micron of ultra-fine cemented carbide scanning electron microscope macrograph (10000X), the tissue that caustic solution according to the present invention corrodes is adopted to have phase and grain boundary clearly, and strong color contrast, very clearly can find out the distribution of each phase of alloy, size and pattern.Fig. 3 B is containing the wimet scanning electron microscope macrograph (5000X) of third phase, the tissue that caustic solution according to the present invention corrodes is adopted to have phase and grain boundary clearly, and strong color contrast, eliminate the interference of third phase, very clearly can find out the distribution of each phase of alloy, size and pattern.
Compared with prior art, adopt corrosive liquid of the present invention and etching process, clear and intuitive macrograph can be obtained, effectively can observe the size of each phase, pattern and distribution, contribute to the improvement of product quality, the research and development of new product, the promoting the use of of alloy designations.
Claims (10)
1. by a method for scanning electron microscopic observation Mathematical Analysis of Al-li Alloy Containing Rare Earth, it is characterized in that, the method comprises: inlay and polishing wimet sample; Sample after polishing is put into corrosive liquid, sample is corroded; After completing sample preparation, by the microstructure of scanning electron microscopic observation Mathematical Analysis of Al-li Alloy Containing Rare Earth.
2. the method for claim 1, is characterized in that, etchant solution comprises WC phase etchant solution and Co phase etchant solution.
3. method as claimed in claim 2, is characterized in that, WC phase etchant solution comprises potassium hydroxide or NaOH and potassium ferricyanide aqueous solution equal volume mixed liquor; The concentration of each aqueous solution between 16-19%, preferably 17.5%; The concentration of each aqueous solution is relevant to the etching time of sample.
4. method as claimed in claim 2, it is characterized in that, Co phase etchant solution comprises ferric trichloride hydrochloric acid saturated solution.
5. the method for claim 1, it is characterized in that, for the alloy not containing adjuvant, first the sample making minute surface is put into WC etchant solution, soak 3min10s, complete WC phase and corrode, sample is put into Co phase corrosive liquid again, corrosion 30s (if all time fluctuations allow the scope at 2 seconds, but wide fluctuations, then need the formula coordinating corrosive liquid).
6. the method for claim 1, is characterized in that, for the alloy having adjuvant, the sample making minute surface is first corroded Co phase 20s, then corrodes WC phase 3min10s, then corrode Co phase 10s.
7. the method for claim 1, is characterized in that, completes sample preparation and also comprises: to the sample purified rinse water through excessive erosion, then be placed in absolute ethyl alcohol, carry out ultrasonic cleaning and dry up.
8. by a system for scanning electron microscopic observation Mathematical Analysis of Al-li Alloy Containing Rare Earth, it is characterized in that, this system comprises: sample preparation device, and it has inlaying device and the burnishing device of wimet sample; Sample processing device, it is arranged on the downstream of sample preparation device, has corrosive liquid container; Sample preparation forming apparatus, it is arranged on the downstream of sample processing device, has the device to the sample purified rinse water through excessive erosion, absolute ethyl alcohol container, ultrasonic cleaning equipment and blow-dry device; And for observing the microstructural scanning electron microscope of Mathematical Analysis of Al-li Alloy Containing Rare Earth.
9. the system as claimed in claim 1, it is characterized in that, corrosive liquid container comprises the WC phase etchant solution container accommodating 17.5% potassium hydroxide aqueous solution and 17.5% potassium ferricyanide aqueous solution equal volume mixed liquor and the Co phase etchant solution container holding ferric trichloride hydrochloric acid saturated solution.
10. system as claimed in claim 9, is characterized in that having the time controller sample making minute surface being soaked in WC etchant solution 3min10s, and in Co phase corrosive liquid, soak the time controller of 10s, 20s, 30s.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107643204A (en) * | 2017-08-09 | 2018-01-30 | 中北大学 | A kind of cochrome etchant and the method using its acquisition metallographic structure |
| CN108181240A (en) * | 2017-12-11 | 2018-06-19 | 崇义章源钨业股份有限公司 | The metallurgical structure exposure method of hard alloy |
| CN109576710A (en) * | 2018-12-07 | 2019-04-05 | 郑州航空工业管理学院 | A kind of chemical corrosion method removing carbide surface hard phase |
| CN109632852A (en) * | 2018-12-14 | 2019-04-16 | 河钢股份有限公司 | A kind of electron microscopic sample preparation method showing bainite structure at fracture surface |
| CN110554066A (en) * | 2019-09-20 | 2019-12-10 | 晋城鸿刃科技有限公司 | alloy metal surface treatment method for grain structure metallographic analysis |
| CN111999326A (en) * | 2020-09-04 | 2020-11-27 | 江西江钨硬质合金有限公司 | Method for measuring uniformity of nanocrystalline hard alloy |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107643204A (en) * | 2017-08-09 | 2018-01-30 | 中北大学 | A kind of cochrome etchant and the method using its acquisition metallographic structure |
| CN108181240A (en) * | 2017-12-11 | 2018-06-19 | 崇义章源钨业股份有限公司 | The metallurgical structure exposure method of hard alloy |
| CN109576710A (en) * | 2018-12-07 | 2019-04-05 | 郑州航空工业管理学院 | A kind of chemical corrosion method removing carbide surface hard phase |
| CN109576710B (en) * | 2018-12-07 | 2020-10-27 | 郑州航空工业管理学院 | Chemical corrosion method for removing hard phase on surface of hard alloy |
| CN109632852A (en) * | 2018-12-14 | 2019-04-16 | 河钢股份有限公司 | A kind of electron microscopic sample preparation method showing bainite structure at fracture surface |
| CN110554066A (en) * | 2019-09-20 | 2019-12-10 | 晋城鸿刃科技有限公司 | alloy metal surface treatment method for grain structure metallographic analysis |
| CN110554066B (en) * | 2019-09-20 | 2022-02-22 | 晋城鸿刃科技有限公司 | Alloy metal surface treatment method for grain structure metallographic analysis |
| CN111999326A (en) * | 2020-09-04 | 2020-11-27 | 江西江钨硬质合金有限公司 | Method for measuring uniformity of nanocrystalline hard alloy |
| CN111999326B (en) * | 2020-09-04 | 2023-11-03 | 江西江钨硬质合金有限公司 | Method for measuring uniformity of nanocrystalline hard alloy |
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