CN103868770B - The preparation method of graininess Fe-C compound transmission electron microscope original position stretching sample - Google Patents
The preparation method of graininess Fe-C compound transmission electron microscope original position stretching sample Download PDFInfo
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Abstract
A kind of preparation method of graininess Fe C compound diaphotoscope original position stretching sample, it is mainly the Fe C compound discrete particles that particle size is 5 μm～1mm, casting is buried in 3mm × (5～8) mm × 1.5mm pure nickel thin slice with electrocasting method, carry out thinning with waterproof abrasive paper grinding, carrying out electrobrightening again, control polishing time makes electroforming nickel sheet surface form pit but can not bore a hole；Finally the electroforming nickel sheet after polishing is carried out ion milling on Ion Beam Thinner, until sample occurs that hole stopping is thinning, be prepared as graininess monocrystal Fe C compound transmission electron microscope original position stretching sample.The present invention can realize the TEM direct in-situ stretching of the graininess monocrystal Fe C compound of a size of 5 μm 1mm and observe, and Plastic Deformation Mechanism, fracture mechanism research for Fe C compound provide effective ways.
Description
Technical field
The invention belongs to Materials Fracture Mechanism Study field, particularly to the preparation of a kind of transmission electron microscope original position stretching sample
Method.
Technical background
The fracture mechanism research of material is the important topic of materialogy, and the transmission electron microscope (TEM) of Materials Fracture is seen in situ
Examine (in situ observation), can the most directly observe the microcosmic continuous process of Materials Fracture, for fracture machine
Analysis processed provides the most direct evidence of microcosmic point, is mechanism analysis most efficient method.
At the beginning of the eighties, first Kobayashir and Ohr etc. use transmission electron microscope original position stretching (TEM in situ tension)
Method, research Mo, W, Cu, Al fracture behaviour, the most directly observe and have recorded crack tip dislocation motion,
Form DFZ(Dislocation Free Zone), dislocation is counter fills in the long-pending dynamic process with micro-crack extension.Hereafter, Pestman
With Hosson with this technique study Ni3In Al crystal, slip dislocation and the interaction of low angle boundary, find that superstructure is intrinsic
The deformation of fault (SISF) causes being formed jog on slip dislocation line, completely the same with the result of computer simulation.Zielinski、
What Lii and Gerberich have studied Fe-2wt.%Si crystal splits point emissary dislocations, finds to split the point quantity of emissary dislocations and DFZ length
Degree and crack tip opening displacement have the relation determined.G.wilde and researcher thereof are to the palladium after rapid cooling and compound thereof in recent years
The deformation of band and fracture process have carried out TEM home position observation, and it is special that result shows that nanocrystalline tension failure presents grain boundary fracture
Levying, the deformation twins of crack tip becomes the extensions path of Edge crystal crack.
The home position observation sample of TEM is due to the needs of imposed load, and stock size requires at 3mm × 5mm, for 5 μ
The Fe-C compound discrete particles of m-1mm magnitude, it is impossible to carrying out the home position observation of uniaxial direct tensile, it is former that this directly limit TEM
The application of position drawing process, it is difficult to realize the independent Plastic Deformation Mechanism research of graininess monocrystal Fe-C compound.
Summary of the invention
For solving above-mentioned technical problem, the invention provides the preparation of a kind of graininess Fe-C compound diaphotoscope original position stretching sample
Method.
The preparation method of the present invention is as follows:
1, electroforming
The Fe-C compound discrete particles of a size of 5 μm-1mm is carried out, dry after bury casting a size of 3mm ×
(5-8) mm × 1.5mm pure nickel thin slice carries out electroforming, electroforming process parameter:
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/dm2
PH value: 3.5-4.5
Temperature: 35-40 DEG C
Described graininess monocrystalline Fe-C compound is Fe3C、M23C6、M7C3；
2, mechanical reduction
The electroforming nickel sheet waterproof abrasive paper grinding that step 1 embeds Fe-C compound carries out thinning, and thickness reaches 50 μm, length and width chi
Very little for 3mm × 5mm；
3, electrobrightening
The electroforming nickel sheet that step 2 is thinning is carried out electrobrightening, and polishing area size reaches Φ 3mm；Polishing fluid is 7% perchloric acid vinegar
Acid solution, polishes voltage 22～25V, electric current 85mA, room temperature；Control polishing time make electroforming nickel sheet surface formed pit but not
Can perforation；
4, ion milling
Electroforming nickel sheet after step 3 being polished carries out ion milling on Ion Beam Thinner, Ion Beam Thinner running parameter: accelerate
Voltage 4.5kv, line 15～20mA, Ion beam incident angles gradually successively decreases by 10～5～3 °, until electroforming nickel sheet occurs that hole stops
The most thinning, prepare graininess monocrystal Fe-C compound transmission electron microscope original position stretching sample.
The present invention compared with prior art has the advantage that
1, the home position observation of the TEM uniaxial direct tensile of the graininess monocrystal Fe-C compound of a size of 5 μm-1mm can be realized,
Plastic Deformation Mechanism, fracture mechanism research for Fe-C compound provide effective ways.
2, according to recording Crack Extension form and crack extending length can be measured, determine its toughness/brittle fracture feature.
Accompanying drawing explanation
Fig. 1 is that the embodiment of the present invention 1 is for preparing the graininess monocrystalline being about 700 μ m 900 μm of TEM original position stretching sample
Fe3The SEM figure of C.
Fig. 2 is the graininess monocrystalline Fe-C compound TEM original position stretching sample of the embodiment of the present invention 1 preparation.
Fig. 3 is the graininess monocrystalline Fe-C compound TEM original position stretching sample using the embodiment of the present invention 1 preparation,
In H-800TEM, stretching is observed, and recorded the TEM figure of Fe-C compound Crack Extension.
Fig. 4 is the graininess monocrystalline Fe-C compound TEM original position stretching sample using the embodiment of the present invention 2 preparation,
In H-800TEM, stretching is observed, and recorded the TEM figure of Fe-C compound Crack Extension.
Detailed description of the invention
Embodiment 1
Scattered Fe to a size of 5 μm3C particle (as shown in Figure 1) is carried out, dry after, bury casting at a size of 3mm
Carrying out electroforming in × 5mm × 1.5mm pure nickel, electroforming solution composition is that every liter electroforming solution is containing nickel sulfamic acid 400g, chlorination
Nickel 10g, boric acid 35g.Current density: 25A/dm2, pH value: 3.5, temperature: 35 DEG C.
Above-mentioned casting is embedded with Fe3The electroforming nickel sheet of C, carries out thinning with waterproof abrasive paper grinding, and thickness reaches 50 μm, and length and width are a size of
3mm×5mm.Above-mentioned thinning electroforming nickel sheet is carried out electrobrightening, and polishing area size reaches Φ 3mm；Polishing fluid is 7%
Perchloric acid acetum, polishes voltage 22V, electric current 85mA, room temperature；Controlling polishing time makes electroforming nickel sheet surface be formed recessed
Cheat but can not bore a hole.Electroforming nickel sheet after polishing is carried out ion milling, accelerating potential 4.5kv, line on Ion Beam Thinner
15mA.Ion beam incident angles gradually successively decreases by 10～5～3 °, until sample occurs that hole stopping is thinning, i.e. obtains graininess list
Brilliant Fe-C compound TEM original position stretching sample, as shown in Figure 2.
Being loaded by the TEM original position stretching sample of the above-mentioned Fe-C compound prepared on H-800TEM drawing stand, TEM accelerates
Voltage 200KV, multiplication factor 5k～200k continuously adjustabe.First start loading stepper motor to load to sample, make sample keep
Permanent displacement state, draw speed 2～5 μm/s, load maximum load 1kg.The sample stretching formation continuous crackle of toughness, Crack blunting,
Direction of crack propagation is vertical with load, and crackle keeps after being formed about 2 minutes stabilizing it, and takes the first width TEM picture, such as figure
Shown in 3-1.The most discontinuous loading, makes crackle front end be passivated and be formed and newly splits point, and crackle toughness extends.Treat that Crack Extension is formed
After stable state, take the second width TEM picture, compare the feature of two width crackle pictures, measure and calculate crack extending length and be about
65nm, as shown in figure 3-2.
Embodiment 2
Scattered Fe to a size of 1mm3C particle is carried out, dry after, bury casting at a size of 3mm × 8mm × 1.5mm
Carrying out electroforming in 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/dm2, pH value: 4.5, temperature: 40 DEG C.
Above-mentioned casting is embedded with Fe3The electroforming nickel sheet of C, carries out thinning with waterproof abrasive paper grinding, and thickness reaches 50 μm, and length and width are a size of
3mm×5mm.Above-mentioned thinning electroforming nickel sheet is carried out electrobrightening, and polishing area size reaches Φ 3mm；Polishing fluid is 7%
Perchloric acid acetum, polishes voltage 25V, electric current 85mA, room temperature；Controlling polishing time makes electroforming nickel sheet surface be formed recessed
Cheat but can not bore a hole.Electroforming nickel sheet after polishing is carried out ion milling, accelerating potential 4.5kv, line on Ion Beam Thinner
20mA.Ion beam incident angles gradually successively decreases by 10 °～5 °～3 °, until sample occurs that hole stopping is thinning, i.e. obtains particle
Shape monocrystalline Fe-C compound TEM original position stretching sample.
Being loaded by the TEM original position stretching sample of the above-mentioned Fe-C compound prepared on H-800TEM drawing stand, TEM accelerates
Continuously adjustabe under voltage 200KV, multiplication factor 5k～200k.First start loading stepper motor and load sample, make sample keep
Permanent displacement state, draw speed 1～3 μm/s, load maximum load 1kg.The stretching of Fe-C compound forms step-like crackle, splits
Line border is straight presents fragility, and direction of crack propagation becomes about 45° angle with load；Crackle keeps after being formed about 2 minutes stabilizing it,
Take the first width TEM picture, as shown in Fig. 4-1.The most discontinuous loading, Fe-C compound crackle is fragility extension, crackle
Border keeps straight.After crackle forms stable state, take the second width TEM picture, compare the feature of two width crackle pictures, measure
With calculating crack extending length, the extension width increase about 70nm of lead crack, crack tip extends about 130nm, such as Fig. 4-2 institute
Show.
Claims (3)
1. the preparation method of a graininess Fe-C compound diaphotoscope original position stretching sample, it is characterised in that:
(1) casting is buried after Fe-C compound discrete particles being carried out, dried pure at a size of 3mm × 5-8mm × 1.5mm
Nickel thin slice carries out electroforming, electroforming solution composition: every liter electroforming solution containing nickel sulfamic acid 400-450g, nickel chloride 10-20g,
Boric acid 35-45g, current density: 25-30A/dm2, P H value: 3.5-4.5, temperature: 35-40 DEG C；
(2) the electroforming nickel sheet waterproof abrasive paper grinding to step (1) embedding Fe-C compound carries out thinning, and thickness reaches 50 μm,
Length and width a size of 3mm × 5mm；
(3) the electroforming nickel sheet that step (2) is thinning being carried out electrobrightening, polishing area size reaches Φ 3mm；Polishing fluid is 7% height
Chloric acid acetum, polishes voltage 22～25V, electric current 85mA, room temperature；Controlling polishing time makes electroforming nickel sheet surface be formed recessed
Cheat but can not bore a hole；
(4) the electroforming nickel sheet after step (3) being polished carries out ion milling on Ion Beam Thinner, Ion Beam Thinner running parameter:
Accelerating potential 4.5kv, line 15～20mA, Ion beam incident angles gradually successively decreases by 10～5～3 °, until sample occurs that hole stops
The most thinning.
The preparation method of graininess Fe-C compound diaphotoscope original position stretching sample the most according to claim 1, its feature
It is: the size of described graininess Fe-C compound is 5 μm～1mm.
The preparation method of graininess Fe-C compound diaphotoscope original position stretching sample the most according to claim 1 and 2, its
It is characterised by: described graininess Fe-C compound is Fe3C、M23C6、M7C3。
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| 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 |
| CN107082428B (en) * | 2017-04-28 | 2019-03-26 | 苏州大学 | A method of cementite is prepared using more metal sulfate slags |
| 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 |
| 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 |
| CN110323457B (en) * | 2019-06-28 | 2020-11-17 | 浙江大学 | Method for in-situ preparation of nano particles by transmission 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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| CN1420349A (en) * | 2002-07-12 | 2003-05-28 | 北京科技大学 | Method for making sample of chemical deposited nickel fixed alloy powder for transmission electron microscope observing |
| CN102304748A (en) * | 2011-09-14 | 2012-01-04 | 哈尔滨工业大学 | Preparation method of transmission electron microscope film sample through rapidly solidifying aluminum alloy powder |
| CN102841005A (en) * | 2012-09-20 | 2012-12-26 | 东南大学 | Preparation method for thin steel wire transmission electron microscope sample |
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| JP2006329743A (en) * | 2005-04-26 | 2006-12-07 | Sumika Chemical Analysis Service Ltd | Sample preparing method for transmission electron microscope |
| JP2008083033A (en) * | 2006-08-31 | 2008-04-10 | Jeol Ltd | Sample preparation method |
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| CN1420349A (en) * | 2002-07-12 | 2003-05-28 | 北京科技大学 | Method for making sample of chemical deposited nickel fixed alloy powder for transmission electron microscope observing |
| CN102304748A (en) * | 2011-09-14 | 2012-01-04 | 哈尔滨工业大学 | Preparation method of transmission electron microscope film sample through rapidly solidifying aluminum alloy powder |
| CN102841005A (en) * | 2012-09-20 | 2012-12-26 | 东南大学 | Preparation method for thin steel wire transmission electron microscope sample |
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| 金属塑性变形与断裂的TEM/SEM原位研究;张静武;《中国优秀博硕士学位论文全文数据库（博士） 工程科技I辑》;20021215(第2期);第15-16页 * |
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