CN104819876A - Preparation method of transmission electron microscopy film sample for in-situ application of electric field and stress - Google Patents
Preparation method of transmission electron microscopy film sample for in-situ application of electric field and stress Download PDFInfo
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Abstract
The present invention provides a preparation method of a transmission electron microscopy film sample for in-situ application of the electric field and the stress. The preparation method comprises: (1) cutting a film to be detected and a single crystal Si substrate into a strip shape with a size of 3 mm*1 mm*0.5 mm, and adhering the film surface of the film strip and the polishing surface of the Si strip; (2) carrying out mechanical grinding and polishing on both surfaces having the film strip thickness; (3) using a nail thinning instrument to carry out nail thinning; (4) adhering a half copper ring; and (5) selecting an ion thinning instrument to carry out ion thinning, setting the ion gun voltage to 4 kV, setting the angle to 6 DEG, thinning for 20-40 min, changing the angle into 4 DEG, thinning for 15-30 min, and finally polishing for 3 min by adopting the angle of 3 DEG and the voltage of 3 kV so as to obtain the large area perforation on the adhering seam, wherein the large area adhered Si sheet is bombarded, the film is exposed, the electric field and the stress can be applied by using the probe, and the large area thin region suitable for observation by the transmission electron microscopy exists on the edge.
Description
Technical field
The invention belongs to epitaxial thin film material In situ transmission electron microscopy studying technological domain, be specifically related to a kind of sample for use in transmitted electron microscope preparation method and application being applicable to epitaxial film original position applying stress and electric field.
Background technology
The high-resolution ability of the existing transmission electron microscope of original position transmission electron microscopy, the observation of atomic scale real-time in-situ can be carried out to material structure change, also synchronously can apply outfield (as stress, electric field and light signal etc.), it is the important technical of modern material research, can be widely used in growth or the stress and deformation of nano material, electricity, magnetic field are on the research work in the fields such as the impact of material structure and performance and minimum gas detection.And directly affect observation test result for the quality of the sample for use in transmitted electron microscope of home position observation.Epitaxial thin film material widespread use in the industries such as semiconductor, photoelectron, machinery, original position transmission electron microscopy is applied to the aspects such as the failure analysis of quality, military service performance and the related device evaluating epitaxial film, greatly will improve detection efficiency, reduce production cost.
The technology of preparing of traditional transmission electron microscope film cross-sectional sample adopts two face to being fixed on after sticky on copper ring that diameter is 3mm, through mechanical wear down and ion milling, forms thin district at face to the perforation of sticky seam central area.The thin district that the method obtains is at the center of copper ring and single crystalline substrate, and the film in thin district is surrounded by annulus and single crystalline substrate, the nano-probe location that loads mechanical stress and electric signal can not be provided and mobile needed for space.The present invention adopts the one side of film sample to sticky on traditional sample making technology basis, the method that semicircular ring is fixing, makes film out exposed, for the interaction of nano-probe and film provides enough spaces, realize original position loading stress and the electric field of epitaxial film, realize in situ TEM and observe.
Summary of the invention
The object of the invention is electron microscope technique be in position applied to epitaxial film detection and in characterizing, a kind of preparation method of the epitaxial film cross-sectional sample of add in-place live field and stress on transmission electron microscope is newly provided.Sample for use in transmitted electron microscope prepared by the method can be compatible with existing business-like specimen holder well, and thin district is large, unobstructed, facilitates extra electric field and stress, is applicable to high-resolution and diffraction contrast image observation.
The object of the invention is to be achieved by the following technical measures.
A kind of preparation method that can be used for the cross-sectional sample of the epitaxial film of transmission electron microscope add in-place electric field and stress provided by the invention, it specifically comprises the following steps:
(1) cutting of film and Si one side are to sticky
Film to be detected and single crystal Si substrate are cut into the elongate in shape being of a size of 3mm × 1mm × 0.5mm.By Si bar and film tape face acetone and alcohol washes clean, bar shaped Si sheet polished surface is evenly coated with last layer AB glue, is pasted onto on silicon chip by film tape face, compress, be placed in 130 DEG C of thermal station 1 ~ 2h, make AB adhesive curing, sample is firmly bonding;
(2) mechanical lapping and polishing
In thermal station, using the sample glued in (1) step two side reusable heats melt paraffin be stained with 2 3mm × 1mm × 0.5mm silicon chip as grinding accompany sheet, sample paraffin is bonded in grinding holder, the holder of thin film planar vertical lapping, on the silicon carbide paper of No. 1000, No. 2000, No. 3000 and No. 5000, be ground to thickness about 0.4 ~ 0.5mm by the sample glued respectively, be polished to till flour milling can't see cut; Melted paraffin wax is taken off sample by thermal station, and be bonded in grinding holder with paraffin again after turn-over, grinding another side, until film thickness is 50 ~ 80 μm of taking-ups, removes and accompanies sheet, cleans paraffin preparation nail thin;
(3) follow closely thin
The sample paraffin processed in (2) step is bonded in the thin holder of nail, selecting Gatan 656 to follow closely thin instrument, to carry out nail thin, following closely thin load is 20g, following closely thin depth-set is 20 μm, follow closely thin wheel and select rag wheel, following closely the thin time is 30 ~ 60min, takes out and can see the slightly saturating ruddiness of silicon chip under through the optical microscope of pattern; Reducing the thin load of nail is 15g, and following closely thin depth-set is 15 μm, and follow closely thin wheel and still use rag wheel, polishing time is about 15 ~ 20min, can make the slightly saturating gold-tinted of silicon chip, follow closely thin completing;
(4) bonding half copper ring
Acetone is put in thin for the nail being stained with sample holder together soak, until sample comes off from sample carrier, clean with acetone, alcohol rinse, dry, the copper ring of to be 3mm interior diameter by overall diameter be 1.5mm thickness 100 μm is cut into two halves, cleaned with acetone, with AB glue, the sample of the thin mistake of nail is bonded in this semicircular ring, 130 DEG C ~ 150 DEG C solidification 45 ~ 60min;
(5) ion milling
Select Gatan 691 type Ion Beam Thinner, be placed on sample stage by the sample gluing half copper ring, and add cooled with liquid nitrogen sample stage, ion gun voltage sets is 4kV, and adopt upper and lower two ion guns simultaneously thinning, angle initialization is 6 °, thinning 20 ~ 40min; Be 4 ° by the thinning angle initialization of two ion guns, thinning 15 ~ 30min, finally adopts 3kV, and angle is 3 °, and namely polishing 3min obtains occurring that large area is bored a hole to sticky seam place, and there is the thin district of the large area being applicable to electron microscopic observation at edge.What is more important, because the thinning speed of Si is greater than oxide monocrystal substrate, makes to have been fallen by Ions Bombardment sticky Si sheet large area, exposes film.Reduce the angle of ion gun in the thinning later stage, protection is not struck off to the film sample near sticky seam on the one hand, and the Si away from cemented side seam also can be made also to be removed.The more important thing is the support adopting semicircle copper ring as sample, for the probe loading external force and electric field provides operating space, and electric field and stress can be loaded to it.
Common transmission electron microscope cross-sectional sample preparation method adopts sample of the same race to sticky, because their thinning speed is identical, ion beam can make thinner boring a hole very soon to sticky seam, obtains thin district, but the substrate around hole is still very thick, block the contact of probe and film.The present invention adopts Si and sample to sticky, utilizes the thinning speed of Si to be greater than oxide monocrystal, thus makes Si come off very soon and to expose film.In addition, reduce the angle of ion gun in the thinning later stage, protective film sample is not struck off on the one hand, and the Si away from cemented side seam also can be made also to remove smoothly.The more important thing is the support adopting semicircle copper ring as sample, for the probe loading external force and electric field provides operating space.
In sum, adopt said method can obtain loading electric field and stress, thin district is large, unobstructed, can with the thin film transmission electron microscope sample of commercial TEM sample bar compatibility, be easy to high-resolution and diffraction contrast image is observed.
Accompanying drawing explanation
Fig. 1 is preparation method's structural representation of the present invention;
Fig. 2 is the structural representation of sample after wear down polishing after sticky half copper ring;
Fig. 3 is the transmission electron microscope cross-sectional sample structural representation obtained after ion milling;
Fig. 4 is the cross sectional view of Fig. 3;
The BiFeO that Fig. 5 successfully obtains
3the tem observation figure of film add in-place stress.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
As shown in Figure 1, the present embodiment provides a kind of film sections sample preparation methods for transmission electron microscope add in-place electric field and stress, the speed utilizing Si material ions thinning is much larger than this characteristic of monocrystalline oxide, select Si sheet and membraneous material to sticky, Si sheet is destroyed by argon ion prior to film and substrate, thus epitaxial film is exposed, be conducive to applying electric field and stress by probe.It specifically comprises the following steps:
(1) cutting of film and Si one side are to sticky
BiFeO will be grown
3the GdScO of film
3oxide monocrystal and single crystalline Si cut into the elongate in shape being of a size of 3mm × 1mm × 0.5mm.By Si bar polished surface and BiFeO
3face acetone and alcohol washes totally, bar shaped Si sheet polished surface are evenly coated with last layer AB glue, by BiFeO
3face face is pasted onto on silicon chip, and compress, be placed in 130 DEG C of thermal station 1 ~ 2h, make AB adhesive curing, sample is firmly bonding;
(2) mechanical lapping and polishing
In thermal station, using the sample glued in (1) step two side reusable heats melt paraffin be stained with 2 3mm × 1mm × 0.5mm silicon chip as grinding accompany sheet, by GdScO
3monocrystalline and Si monocrystalline adhesive strip are bonded in grinding holder along film thickness direction paraffin, on the silicon carbide paper of No. 1000, No. 2000, No. 3000 and No. 5000, be ground to thickness 0.4 ~ 0.5mm by the sample glued respectively, be polished to till flour milling can't see cut; Melted paraffin wax is taken off sample by thermal station, and be bonded in grinding holder with paraffin again after turn-over, grinding another side, until film thickness is 50 ~ 80 μm of taking-ups, removes and accompanies sheet, cleans paraffin preparation nail thin;
(3) follow closely thin
The sample paraffin processed in (2) step is bonded in the thin holder of nail, selecting Gatan 656 to follow closely thin instrument, to carry out nail thin, following closely thin load is 20g, following closely thin depth-set is 20 μm, follow closely thin wheel and select rag wheel, following closely the thin time is 30 ~ 60min, takes out and can see the slightly saturating ruddiness of silicon chip under through the optical microscope of pattern; Reducing the thin load of nail is 15g, and following closely thin depth-set is 15 μm, and follow closely thin wheel and still use rag wheel, polishing time is about 15 ~ 20min, can make the slightly saturating gold-tinted of silicon chip, follow closely thin completing;
(4) bonding half copper ring
Acetone is put in thin for the nail being stained with sample holder together soak, until sample comes off from sample carrier, clean with acetone, alcohol rinse, dry, the copper ring of to be 3mm interior diameter by overall diameter be 1.5mm thickness 100 μm is cut into two halves, cleaned with acetone, with AB glue, the sample of the thin mistake of nail is bonded in this semicircular ring, 130 DEG C ~ 150 DEG C solidification 45 ~ 60min;
(5) ion milling
Select Gatan 691 type Ion Beam Thinner, be placed on sample stage by the sample gluing half copper ring, and add cooled with liquid nitrogen sample stage, ion gun voltage sets is 4kV, and adopt upper and lower two ion guns simultaneously thinning, angle initialization is 6 °, thinning 20 ~ 40min; Be 4 ° by the thinning angle initialization of two ion guns, thinning 15 ~ 30min, finally adopts 3kV, and namely 3 ° of polishing 3min obtain occurring that large area is bored a hole to sticky seam place, and there is the thin district of the large area being applicable to electron microscopic observation at edge.What is more important, because the thinning speed of Si is greater than GdScO
3single crystalline substrate, makes to have been fallen by Ions Bombardment sticky Si sheet large area, exposes film.Reduce the angle of ion gun in the thinning later stage, protection is not struck off to the film sample near sticky seam on the one hand, and the Si away from cemented side seam also can be made also to be removed.The more important thing is the support adopting semicircle copper ring as sample, for the probe loading external force and electric field provides operating space, and electric field and stress can be loaded to it.Thinning complete after obtained sample schematic diagram as shown in Figure 3.
Adopt method provided by the invention to prepare and grown at GdScO
3biFeO in single crystalline substrate
3the cross-sectional Transmission electron microscopic sample of epitaxial film, as shown in Figure 5, BiFeO
3film large area has been exposed, and thin district is large, can do diffraction contrast image and high resolution picture, gives BiFeO in figure
3the film change of ferroelectric domain under effect of stress outside.
Claims (1)
1., for a film sample preparation method for transmission electron microscope add in-place electric field and stress, it is characterized in that specifically comprising the following steps:
(1) cutting of film and Si one side are to sticky
Film to be detected and single crystal Si substrate are cut into the elongate in shape being of a size of 3mm × 1mm × 0.5mm.By Si bar polished surface and film tape face acetone and alcohol washes clean, bar shaped Si sheet polished surface is evenly coated with last layer AB glue, is pasted onto on silicon chip by film tape face, compress, be placed in 130 DEG C of thermal station 1 ~ 2h, make AB adhesive curing, sample is firmly bonding.
(2) mechanical lapping and polishing
In thermal station, using the sample glued in (1) step two side reusable heats melt paraffin be stained with 2 3mm × 1mm × 0.5mm silicon chip as grinding accompany sheet, sample paraffin is bonded in grinding holder, the holder of thin film planar vertical lapping, on the silicon carbide paper of No. 1000, No. 2000, No. 3000 and No. 5000, be ground to thickness 0.4 ~ 0.5mm by the sample glued respectively, be polished to till flour milling can't see cut; Melted paraffin wax is taken off sample by thermal station, and be bonded in grinding holder with paraffin again after turn-over, grinding another side, until film thickness is 50 ~ 80 μm of taking-ups, removes and accompanies sheet, cleans paraffin preparation nail thin.
(3) follow closely thin
The sample paraffin processed in (2) step is bonded in the thin holder of nail, selecting Gatan 656 to follow closely thin instrument, to carry out nail thin, following closely thin load is 20g, following closely thin depth-set is 20 μm, follow closely thin wheel and select rag wheel, following closely the thin time is 30 ~ 60min, takes out and can see the slightly saturating ruddiness of silicon chip under through the optical microscope of pattern; Reducing the thin load of nail is 15g, and following closely thin depth-set is 15 μm, and follow closely thin wheel and still use rag wheel, polishing time is about 15 ~ 20min, can make the slightly saturating gold-tinted of silicon chip, follow closely thin completing.
(4) bonding half copper ring
Acetone is put in thin for the nail being stained with sample holder together soak, until sample comes off from sample carrier, clean with acetone, alcohol rinse, dry, the copper ring of to be 3mm interior diameter by overall diameter be 1.5mm thickness 100 μm is cut into two halves, cleaned with acetone, with AB glue, the sample of the thin mistake of nail is bonded in this semicircular ring, 130 DEG C ~ 150 DEG C solidification 45 ~ 60min.
(5) ion milling
Select Gatan 691 type Ion Beam Thinner, be placed on sample stage by the sample gluing half copper ring, and add cooled with liquid nitrogen sample stage, ion gun voltage sets is 4kV, and adopt upper and lower two ion guns simultaneously thinning, angle initialization is 6 °, thinning 20 ~ 40min; Be 4 ° by the thinning angle initialization of two ion guns, thinning 15 ~ 30min, finally adopts 3kV, and namely 3 ° of polishing 3min obtain occurring that large area is bored a hole to sticky seam place, and there is the thin district of the large area being applicable to electron microscopic observation at edge.What is more important, because the thinning speed of Si is greater than oxide monocrystal substrate, makes to have been fallen by Ions Bombardment sticky Si sheet large area, exposes film.Reduce the angle of ion gun in the thinning later stage, protection is not struck off to the film sample near sticky seam on the one hand, and the Si away from cemented side seam also can be made also to be removed.The more important thing is the support adopting semicircle copper ring as sample, for the probe loading external force and electric field provides operating space, and electric field and stress can be loaded to it.
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Cited By (10)
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| CN105486566A (en) * | 2015-11-18 | 2016-04-13 | 大连交通大学 | Preparation method for metallographic sample used for scanning electron microscopy |
| CN105652040A (en) * | 2016-01-08 | 2016-06-08 | 西北工业大学 | TEM sample preparation method |
| CN105973674A (en) * | 2016-07-01 | 2016-09-28 | 中国科学院地质与地球物理研究所 | Preparation method of transmission electron microscope sample with large area of thin region |
| CN107576541A (en) * | 2017-07-22 | 2018-01-12 | 复旦大学 | The preparation method of power-up indium arsenide/gallium antimonide superlattice semiconductor sample in situ of transmission electron microscope |
| CN108731993A (en) * | 2018-04-18 | 2018-11-02 | 厦门大学 | Weak bond strength brittleness is bonded sample in cross section transmission electron microscope preparation method |
| CN108918211A (en) * | 2018-05-08 | 2018-11-30 | 西京学院 | A kind of metallic film/amorphous alloy cross-sectional Transmission sample preparation methods |
| CN109870336A (en) * | 2019-01-31 | 2019-06-11 | 长江存储科技有限责任公司 | Semiconductor test system and its test method |
| CN110702717A (en) * | 2019-10-15 | 2020-01-17 | 重庆大学 | Preparation method for transmission electron microscope slicing sample and slicing transfer device |
| CN113020612A (en) * | 2021-02-22 | 2021-06-25 | 上海理工大学 | Preparation method of copper nano-spherulites with continuously adjustable size |
| CN117213951A (en) * | 2023-11-07 | 2023-12-12 | 矿冶科技集团有限公司 | Preparation method of coal combustion fly ash transmission electron microscope sample |
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| CN107576541A (en) * | 2017-07-22 | 2018-01-12 | 复旦大学 | The preparation method of power-up indium arsenide/gallium antimonide superlattice semiconductor sample in situ of transmission electron microscope |
| CN107576541B (en) * | 2017-07-22 | 2020-05-12 | 复旦大学 | Method for preparing in-situ power-up indium arsenide/gallium antimonide superlattice semiconductor sample of transmission electron microscope |
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| CN108918211A (en) * | 2018-05-08 | 2018-11-30 | 西京学院 | A kind of metallic film/amorphous alloy cross-sectional Transmission sample preparation methods |
| CN109870336A (en) * | 2019-01-31 | 2019-06-11 | 长江存储科技有限责任公司 | Semiconductor test system and its test method |
| CN110702717A (en) * | 2019-10-15 | 2020-01-17 | 重庆大学 | Preparation method for transmission electron microscope slicing sample and slicing transfer device |
| CN110702717B (en) * | 2019-10-15 | 2022-05-10 | 重庆大学 | Preparation method for transmission electron microscope slicing sample and slicing transfer device |
| CN113020612A (en) * | 2021-02-22 | 2021-06-25 | 上海理工大学 | Preparation method of copper nano-spherulites with continuously adjustable size |
| CN117213951A (en) * | 2023-11-07 | 2023-12-12 | 矿冶科技集团有限公司 | Preparation method of coal combustion fly ash transmission electron microscope sample |
| CN117213951B (en) * | 2023-11-07 | 2024-02-02 | 矿冶科技集团有限公司 | Preparation method of coal combustion fly ash transmission electron microscope sample |
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