CN103868770A - Preparation method of granulate Fe-C compound transmission electron microscope in-situ tensile sample - Google Patents
Preparation method of granulate Fe-C compound transmission electron microscope in-situ tensile sample Download PDFInfo
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- CN103868770A CN103868770A CN201410061850.2A CN201410061850A CN103868770A CN 103868770 A CN103868770 A CN 103868770A CN 201410061850 A CN201410061850 A CN 201410061850A CN 103868770 A CN103868770 A CN 103868770A
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Abstract
The invention discloses a preparation method of a granulate Fe-C compound transmission electron microscope in-situ tensile sample. The preparation method of the granulate Fe-C compound TEM (transmission electron microscope) in-situ tensile sample mainly comprises the following steps: burying and casting Fe-C compound dispersed granules with the granule size of 5 microns-1mm into a pure nickel thin sheet of 3mm*(5-8)mm*1.5mm by an electric casting method, grinding by waterproof abrasive paper for thinning, and then carrying out electrolytic polishing, wherein the polishing time is controlled to enable concave pits to be formed on the surface of the electric casting nickel sheet without penetration; and finally, carrying out ion polishing on the polished electric casting nickel sheet on an ion polishing system until holes are formed in a sample, thereby preparing the granulate monocrystal Fe-C compound transmission electron microscope in-situ tensile sample. According to the invention, the TEM direct in-situ tensile observation of the granulate monocrystal Fe-C compound with the size of 5 microns-1mm can be realized, and an effective method can be provided for the plastic deformation and the fracture mechanism of the Fe-C compound.
Description
Technical field
The invention belongs to Materials Fracture Mechanism Study field, particularly a kind of preparation method of transmission electron microscope original position stretching sample.
Technical background
The fracture mechanism research of material is the important topic of materialogy, transmission electron microscope (TEM) home position observation (in situ observation) of Materials Fracture, can under electron microscope, directly observe the microcosmic continuous process of Materials Fracture, for fracture mechanism analysis provides microcosmic point the most direct evidence, it is the effective method of mechanism analysis.
The beginning of the eighties, first Kobayashir and Ohr etc. use transmission electron microscope original position stretching (TEM in situ tension) method, the fracture behaviour of research Mo, W, Cu, Al, under TEM, directly observe and recorded crack tip dislocation motion, form DFZ(Dislocation Free Zone), the long-pending dynamic process with micro-crack extension of the anti-plug of dislocation.After this, Pestman and Hosson have studied Ni by this method
3the interaction of slip dislocation and low angle boundary in Al crystal, finds that the distortion of the intrinsic fault of superlattice (SISF) causes forming jog on slip dislocation line, in full accord with the result of computer simulation.Zielinski, Lii and Gerberich have studied the sharp emissary dislocations that splits of Fe-2wt.%Si crystal, and finding to split the quantity of sharp emissary dislocations and DFZ length and crack tip opening displacement has definite relation.Palladium after to rapid cooling of G.wilde and researchist thereof and the deformation and fracture process of compound band thereof have been carried out TEM home position observation in recent years, result shows that nanocrystalline tension failure presents along brilliant fracture characteristic, and the distortion twin of crack tip becomes the extensions path along brilliant crackle.
The home position observation sample of TEM is due to the needs of imposed load, stock size requires at 3mm × 5mm, for the Fe-C compound discrete particles of 5 μ m-1mm magnitudes, can not carry out the home position observation directly stretching, the application that this has directly limited TEM original position stretching method, is difficult to realize the independent Plastic Deformation Mechanism research of graininess monocrystal Fe-C compound.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of preparation method of graininess Fe-C compound diaphotoscope original position stretching sample.
Preparation method of the present invention is as follows:
1, electroforming
After cleaning, dry, buries the Fe-C compound discrete particles of 5 μ m-1mm casting being of a size of 3mm × (5-8) carry out electroforming in mm × 1.5mm pure nickel thin slice, electroforming process parameter to being of a size of:
Electroforming solution composition: every liter electroforming solution is containing nickel sulfamic acid 400-450g, nickel chloride 10-20g, boric acid 35-45g.
Current density: 25-30A/dm
2
PH value: 3.5-4.5
Temperature: 35-40 ℃
Described graininess monocrystalline Fe-C compound is Fe
3c, M
23c
6, M
7c
3;
2, mechanical reduction
The electroformed nickel sheet of step 1 embedding Fe-C compound is ground and carries out attenuate with waterproof abrasive paper, and thickness reaches 50 μ m, and length and width are of a size of 3mm × 5mm;
3, electropolishing
Electroformed nickel sheet to step 2 attenuate carries out electropolishing, and polishing area size reaches Φ 3mm; Polishing fluid is 7% perchloric acid acetum, polishing voltage 22～25V, electric current 85mA, room temperature; Controlling polishing time makes electroformed nickel sheet surface form pit but can not bore a hole;
4, ion milling
Electroformed nickel sheet after step 3 polishing is carried out to ion milling on Ion Beam Thinner, Ion Beam Thinner running parameter: accelerating potential 4.5kv, line 15～20mA, ion beam incident angle is successively successively decreased by 10～5～3 °, until electroformed nickel sheet occurs that hole stops attenuate, make graininess monocrystal Fe-C compound transmission electron microscope original position stretching sample.
The present invention compared with prior art tool has the following advantages:
1, can realize the directly home position observation of stretching of TEM of the graininess monocrystal Fe-C compound that is of a size of 5 μ m-1mm, for Plastic Deformation Mechanism, the fracture mechanism research of Fe-C compound provide effective ways.
2, can, according to recording Crack Extension form and measuring crack extending length, determine its toughness/brittle fracture feature.
Accompanying drawing explanation
Fig. 1 is the graininess monocrystalline Fe that be about 700 μ m × 900 μ ms of the embodiment of the present invention 1 for the preparation of TEM original position stretching sample
3the SEM figure of C.
Fig. 2 is graininess monocrystalline Fe-C compound TEM original position stretching sample prepared by the embodiment of the present invention 1.
Fig. 3 is the graininess monocrystalline Fe-C compound TEM original position stretching sample that uses the embodiment of the present invention 1 to prepare, and in H-800TEM, stretches and observes, and is recorded to the TEM figure of Fe-C compound Crack Extension.
Fig. 4 is the graininess monocrystalline Fe-C compound TEM original position stretching sample that uses the embodiment of the present invention 2 to prepare, and in H-800TEM, stretches and observes, and is recorded to the TEM figure of Fe-C compound Crack Extension.
Embodiment
Embodiment 1
To being of a size of the Fe of dispersion of 5 μ m
3after C particle (as shown in Figure 1) cleans, dries, bury casting and carry out electroforming being of a size of in 3mm × 5mm × 1.5mm pure nickel, electroforming solution composition is that every liter electroforming solution is containing nickel sulfamic acid 400g, nickel chloride 10g, boric acid 35g.Current density: 25A/dm
2, pH value: 3.5, temperature: 35 ℃.
Above-mentioned casting is embedded with to Fe
3the electroformed nickel sheet of C, grinds and carries out attenuate with waterproof abrasive paper, and thickness reaches 50 μ m, and length and width are of a size of 3mm × 5mm.The electroformed nickel sheet of above-mentioned attenuate is carried out to electropolishing, and polishing area size reaches Φ 3mm; Polishing fluid is 7% perchloric acid acetum, polishing voltage 22V, electric current 85mA, room temperature; Controlling polishing time makes electroformed nickel sheet surface form pit but can not bore a hole.Electroformed nickel sheet after polishing is carried out to ion milling, accelerating potential 4.5kv, line 15mA on Ion Beam Thinner.Ion beam incident angle is successively successively decreased by 10～5～3 °, stops attenuate until hole appears in sample, obtains graininess monocrystalline Fe-C compound TEM original position stretching sample, as shown in Figure 2.
The TEM original position stretching sample of the above-mentioned Fe-C compound preparing is loaded on H-800TEM drawing stand, TEM accelerating potential 200KV, enlargement factor 5k～200k is adjustable continuously.First start loading stepper motor and load to sample, make sample keep permanent displacement state, draw speed 2～5 μ m/s, load maximum load 1kg.Sample stretches and forms the continuous crackle of toughness, Crack blunting, and direction of crack propagation is vertical with load, and crackle forms rear maintenance makes it stable for approximately 2 minutes, takes the first width TEM picture, as shown in Fig. 3-1.Then discontinuous loading, makes the passivation of crackle front end and forms newly to split point the expansion of crackle toughness.After Crack Extension forms steady state (SS), take the second width TEM picture, the relatively feature of two width crackle pictures, measurements and calculations crack extending length is about 65nm, as shown in Fig. 3-2.
To being of a size of the Fe of dispersion of 1mm
3after C particle cleans, dries, bury casting and carry out electroforming being of a size of in 3mm × 8mm × 1.5mm pure nickel, electroforming solution composition is that every liter electroforming solution is containing nickel sulfamic acid 450g, nickel chloride 20g, boric acid 45g.Current density: 30A/dm
2, pH value: 4.5, temperature: 40 ℃.
Above-mentioned casting is embedded with to Fe
3the electroformed nickel sheet of C, grinds and carries out attenuate with waterproof abrasive paper, and thickness reaches 50 μ m, and length and width are of a size of 3mm × 5mm.The electroformed nickel sheet of above-mentioned attenuate is carried out to electropolishing, and polishing area size reaches Φ 3mm; Polishing fluid is 7% perchloric acid acetum, polishing voltage 25V, electric current 85mA, room temperature; Controlling polishing time makes electroformed nickel sheet surface form pit but can not bore a hole.Electroformed nickel sheet after polishing is carried out to ion milling, accelerating potential 4.5kv, line 20mA on Ion Beam Thinner.Ion beam incident angle is successively successively decreased by 10 °～5 °～3 °, stops attenuate until hole appears in sample, obtains graininess monocrystalline Fe-C compound TEM original position stretching sample.
The TEM original position stretching sample of the above-mentioned Fe-C compound preparing is loaded on H-800TEM drawing stand, TEM accelerating potential 200KV, adjustable continuously under enlargement factor 5k～200k.First start and load stepper motor loading sample, make sample keep permanent displacement state, draw speed 1～3 μ m/s, loads maximum load 1kg.Fe-C compound stretches and forms step-like crackle, and crack edge is straight presents fragility, and direction of crack propagation and load are into about 45° angle; Crackle forms rear maintenance makes it stable for approximately 2 minutes, takes the first width TEM picture, as shown in Fig. 4-1.Then discontinuous loading, Fe-C compound crackle is fragility expansion, and it is straight that crack edge keeps.After crackle forms steady state (SS), take the second width TEM picture, the relatively feature of two width crackle pictures, measurements and calculations crack extending length, the extension width of main crackle increases about 70nm, and crack tip is expanded about 130nm, as shown in Fig. 4-2.
Claims (3)
1. a preparation method for graininess Fe-C compound diaphotoscope original position stretching sample, is characterized in that:
(1) bury casting after Fe-C compound discrete particles is cleaned, dried and carry out electroforming, electroforming solution composition being of a size of in 3mm × 5-8mm × 1.5mm pure nickel thin slice: every liter electroforming solution is containing nickel sulfamic acid 400-450g, nickel chloride 10-20g, boric acid 35-45g, current density: 25-30A/dm
2, pH value: 3.5-4.5, temperature: 35-40 ℃;
(2) the electroformed nickel sheet of step (1) embedding Fe-C compound is ground and carries out attenuate with waterproof abrasive paper, thickness reaches 50 μ m, and length and width are of a size of 3mm × 5mm;
(3) the electroformed nickel sheet of step (2) attenuate is carried out to electropolishing, polishing area size reaches Φ 3mm; Polishing fluid is 7% perchloric acid acetum, polishing voltage 22～25V, electric current 85mA, room temperature; Controlling polishing time makes electroformed nickel sheet surface form pit but can not bore a hole;
(4) the electroformed nickel sheet after step (3) polishing is carried out to ion milling, Ion Beam Thinner running parameter on Ion Beam Thinner: accelerating potential 4.5kv, line 15～20mA.Ion beam incident angle is successively successively decreased by 10～5～3 °, stops attenuate until hole appears in sample.
2. the preparation method of graininess Fe-C compound diaphotoscope original position stretching sample according to claim 1, is characterized in that: described graininess monocrystalline Fe-C compound is of a size of 5 μ m～1mm.
3. the preparation method of graininess Fe-C compound diaphotoscope original position stretching sample according to claim 1 and 2, is characterized in that: described graininess monocrystalline Fe-C compound is Fe
3c, M
23c
6, M
7c
3.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107082428A (en) * | 2017-04-28 | 2017-08-22 | 苏州大学 | A kind of method that cementite is prepared using many metal sulfate slags |
| CN107121316A (en) * | 2017-03-22 | 2017-09-01 | 华南理工大学 | A kind of preparation method of micron order Ni-base Superalloy Powder transmission electron microscope film sample |
| CN109668765A (en) * | 2019-01-18 | 2019-04-23 | 南京理工大学 | A kind of more orientations Jie's sight stretching sample preparation methods based on femtosecond laser processing |
| CN110018189A (en) * | 2019-03-21 | 2019-07-16 | 浙江大学 | A kind of in situ TEM method for studying copper alloy with high strength and high conductivity strengthening mechanism |
| CN110208168A (en) * | 2019-06-28 | 2019-09-06 | 浙江大学 | A kind of transmission electron microscopy of on-spot study nanoparticle three-dimensional distributed architecture |
| CN110323457A (en) * | 2019-06-28 | 2019-10-11 | 浙江大学 | A kind of method that nano particle is prepared in situ in transmission electron microscope |
| CN113899919A (en) * | 2021-10-08 | 2022-01-07 | 长沙理工大学 | Method for observing dislocation glide trace of magnesium alloy containing LPSO phase by using scanning electron microscope |
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Cited By (12)
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|---|---|---|---|---|
| CN107121316A (en) * | 2017-03-22 | 2017-09-01 | 华南理工大学 | A kind of preparation method of micron order Ni-base Superalloy Powder transmission electron microscope film sample |
| CN107121316B (en) * | 2017-03-22 | 2021-12-21 | 华南理工大学 | Preparation method of micron-sized nickel-based superalloy powder transmission electron microscope film sample |
| CN107082428A (en) * | 2017-04-28 | 2017-08-22 | 苏州大学 | A kind of method that cementite is prepared using many metal sulfate slags |
| CN107082428B (en) * | 2017-04-28 | 2019-03-26 | 苏州大学 | A method of cementite is prepared using more metal sulfate slags |
| CN109668765A (en) * | 2019-01-18 | 2019-04-23 | 南京理工大学 | A kind of more orientations Jie's sight stretching sample preparation methods based on femtosecond laser processing |
| CN109668765B (en) * | 2019-01-18 | 2021-11-09 | 南京理工大学 | Method for preparing multi-orientation mesoscopic stretching sample based on femtosecond laser processing |
| CN110018189A (en) * | 2019-03-21 | 2019-07-16 | 浙江大学 | A kind of in situ TEM method for studying copper alloy with high strength and high conductivity strengthening mechanism |
| CN110208168A (en) * | 2019-06-28 | 2019-09-06 | 浙江大学 | A kind of transmission electron microscopy of on-spot study nanoparticle three-dimensional distributed architecture |
| CN110323457A (en) * | 2019-06-28 | 2019-10-11 | 浙江大学 | A kind of method that nano particle is prepared in situ in transmission electron microscope |
| CN110208168B (en) * | 2019-06-28 | 2020-06-16 | 浙江大学 | Transmission electron microscope technology for in-situ research of three-dimensional distribution structure of nanoparticles |
| CN113899919A (en) * | 2021-10-08 | 2022-01-07 | 长沙理工大学 | Method for observing dislocation glide trace of magnesium alloy containing LPSO phase by using scanning electron microscope |
| CN113899919B (en) * | 2021-10-08 | 2024-04-12 | 长沙理工大学 | Method for observing dislocation slip trace of magnesium alloy containing LPSO phase by using scanning electron microscope |
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