CN105865866A - Method for preparing ultra-thin single-crystal for transmission electron diffraction studies - Google Patents
Method for preparing ultra-thin single-crystal for transmission electron diffraction studies Download PDFInfo
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- CN105865866A CN105865866A CN201610200723.5A CN201610200723A CN105865866A CN 105865866 A CN105865866 A CN 105865866A CN 201610200723 A CN201610200723 A CN 201610200723A CN 105865866 A CN105865866 A CN 105865866A
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- thin single
- single crystalline
- ultra thin
- ultra
- contained network
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20058—Measuring diffraction of electrons, e.g. low energy electron diffraction [LEED] method or reflection high energy electron diffraction [RHEED] method
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
Abstract
The invention discloses a method for preparing an ultra-thin single-crystal sample for transmission electron diffraction studies. The method comprises the steps of: 1) placing ultra-thin single-crystal with thickness of less than 100nm on a clean substrate; 2) placing a new support grid upside down on the ultra-thin single-crystal surface to form a new support grid-ultra-thin-single-crystal-substrate structure; 3) dropwise adding an isopropyl alcohol solution into the new support grid-ultra-thin-single-crystal-substrate structure, so as to immerse isopropyl alcohol solution in an interface of the new grid and the ultra-thin single-crystal, and naturally evaporating to dryness; 4) placing the new support grid-ultra-thin-single-crystal-substrate structure from the step 3) into a solution for dissolving of the substrate structure to dissolve the substrate, separate the ultra-thin single-crystal from substrate, and adhere the ultra-thin single-crystal to the new support grid, so as to form a new support grid-ultra-thin-single-crystal structure; and 5) subjecting the new support grid-ultra-thin-single-crystal structure in the step 4) to repeated deionized water rinsing and drying in the air. The method has the advantages of simple operation, low cost and rapid sample preparation.
Description
Technical field
The invention belongs to transmission electron diffraction (TED) technical field, be specifically related to a kind of for transmitted electron
The preparation method of the ultra thin single crystalline sample of diffraction investigation.
Background technology
In technical fields such as Condensed Matter Physics, material science and large scale integrated circuits, in order to obtain
Obtain the microcosmos structure characteristic of object of study, it usually needs by means of electron diffraction technique, such as transmission
Ultramicroscope, ultrafast electronic diffraction instrument etc..Transmission electron microscopy has high spatial discrimination
Rate, can be used to the architectural characteristic of research material, it is thus achieved that the fine micro-image of sample, lattice structure
Deng important information, it it is research means indispensable in current leading basic research.With transmission electricity
Sub-microtechnique is compared, and ultrafast electric diffraction also has high time resolution characteristics, can be used to grind
Study carefully the Structural Dynamics of material, and then the regulation and control to material function can be realized, biological, chemistry,
The numerous areas such as physics and quasiconductor has important application.
Owing to the interaction between electronics and material is very strong, the mean free path of electronics is general very
Short, the penetration capacity of electron beam is the most weak, therefore in transmission electron diffraction (TED) is studied, in order to ensure
Electronic energy penetrates sample, and conventional transmission electron microscope and mental retardation ultrafast electronic diffraction instrument are to sample
The thickness of product has strict demand, it is generally required to thickness is less than the ultra-thin sample of 200nm self-supporting.
If sample is the thickest, electronics will not penetrate sample, therefore can not obtain electron diffraction pattern.
As can be seen here, in transmission electron diffraction (TED) is studied, preparing of the ultra-thin sample of self-supporting is most important.
The method being currently used for preparing the ultra-thin sample of self-supporting mainly has a following two:
At Grown thin film, the most again by substrate thinning or dissolving.Patent
CN102353687B proposes the preparation method of a kind of super thin aluminum film, first has the base of micropore
Form organic film on bottom structure, then utilize physical gas-phase deposition on organic film surface
Growth aluminum film, is derived from the aluminum film of support after being corroded by organic film the most again.But, this
Method is typically only used for preparing amorphous sample, it is impossible to prepare high-quality self-supporting ultra thin single crystalline
Sample.
With the thinning sample of the technique of focused-ion-beam lithography.US 2013/0143412A1 proposes
A kind of focused-ion-beam lithography technique is utilized to realize method prepared by transmission electron diffraction (TED) sample.This
The advantage of the method for kind is that degree of accuracy is high, and the thickness of sample is controlled, and sample preparation speed is fast, and yield rate is high,
It it is most-often used method.But, focused ion beam equipment is expensive, and sample preparation cost is high, and by
Then use the thinning sample of method of high-energy ion bombardment sample surfaces, easily sample is caused damage
Wound, makes sample produce defect, even can make the doping of paired samples time serious, change sample
Structure and characteristic, limit its range of application.
It can be seen that the method for existing preparation self-supporting ultra-thin transmission electron diffraction (TED) sample exists not
The preparation of ultra thin single crystalline sample can be realized, easily sample caused damage, prepare sample cost height
The shortcoming such as high, is badly in need of a kind of new sample preparation methods.
Summary of the invention
For the shortcoming overcoming above prior art to exist, the present invention provides a kind of for transmission electricity
The preparation method of the ultra-thin sample of self-supporting of sub-diffraction investigation, the method has simple to operate, system
The sample time is short, low cost and the advantage little to sample damage, especially can realize high-quality from
The preparation of support ultra thin single crystalline sample.
The present invention provides following technical scheme:
The preparation method of a kind of ultra thin single crystalline sample for transmission electron diffraction (TED) research, it is special
Part is, comprises the following steps:
1) ultra thin single crystalline is placed on the substrate of cleaning；Wherein, the thickness of ultra thin single crystalline is less than
100nm；
2) new contained network is inverted in ultra thin single crystalline surface, forms new contained network-ultra thin single crystalline-substrate
Structure；
Described new contained network includes porous carbon support membrane and standard transmission electron microscopy contained network, its
In, porous carbon support membrane is placed in standard transmission electron microscopy contained network；
New contained network is inverted in ultra thin single crystalline surface and refers to that the one side of porous carbon support membrane is just to ultra-thin
Single-crystal surface；
3) on new contained network-ultra thin single crystalline-substrat structure, instill aqueous isopropanol, make isopropanol
It is dry with the separating surface of ultra thin single crystalline natural evaporation that solution immerses new contained network；Now exist due to solvent
Surface tension in evaporation process makes new contained network and ultra thin single crystalline thin slice combine；
4) by through step 3) new contained network-ultra thin single crystalline-substrat structure put into for dissolving lining
In the solution at the end, making substrate dissolve, ultra thin single crystalline departs from substrate, is attached in new contained network,
Form new contained network-ultra thin single crystalline structure；
5) by through step 4) new contained network-ultra thin single crystalline structure of being formed carries out repeatedly deionization
Water rinses, and naturally dries afterwards, i.e. can be used for testing.
Step 1) in ultra thin single crystalline be stratified material, specially graphite, topological insulator or
High-temperature superconductor.
In order to make the adhesion between new contained network and ultra thin single crystalline further enhance；Step 3) in
Aqueous isopropanol natural evaporation dry after, newer contained network-ultra thin single crystalline-substrat structure is positioned over
Heating on hot plate, about 5 minutes heat time heating times, temperature controls within 200 degree.
Step 1) in substrate be to have silica membrane thick for 300nm in superficial growth
Silicon substrate.
Step 4) in be strong base solution for dissolving the solution of substrate, the concentration of solution is
25%-35%.
Step 4) in be potassium hydroxide solution or sodium hydroxide solution for dissolving the solution of substrate.
Step 1) in ultra thin single crystalline be prepared by the technique utilizing adhesive tape to peel off.
Step 2) in porous carbon support membrane thickness be 8-20nm, aperture 1 μm-6 μm.
Step 2) a diameter of 3mm of Plays transmission electron microscopy contained network, mesh number is more than 200；
Step 1) in the concrete preparation process of ultra thin single crystalline be:
A, from bulky single crystal, cut out fritter monocrystalline thin slice, then this fritter monocrystalline thin slice is glued
It is attached to adhesive tape front；Wherein, the size of fritter monocrystalline thin slice is more than 1mm × 1mm × 0.2mm；
B, by fritter monocrystalline thin slice in the front of another piece of tape and step a residing for adhesive tape
Position is pasted together, and so, fritter monocrystalline thin slice is just sandwiched between two panels adhesive tape；
C, the adhesive tape of fritter monocrystalline thin slice side is opened；
D, repetition step b-c；
E, examine under a microscope the monocrystalline above each adhesive tape, select that area is relatively big, thickness
Little and smooth monocrystalline, is placed in above substrate by the front of the adhesive tape belonging to this monocrystalline, Qi Zhongsuo
The region at menu crystalline substance place is positioned at the central authorities of substrate, is removed lightly by adhesive tape, make from substrate
Ultra thin single crystalline falls within substrate, by Van der Waals between atom between these monocrystalline and substrates
Combine；
F, optical microscope and atomic force microscope is utilized to select ultra thin single crystalline, ultra thin single crystalline
Area is the bigger the better.
Advantages of the present invention:
The such scheme of the present invention compared with prior art has simple to operate, low cost and can be real
The advantage of existing rapid prototyping.Additionally, the present invention realizes super by using strong base solution to dissolve substrate
Thin single crystal material separates with substrate and note is in contained network, can farthest reduce solution pair
The damage of material, it is achieved the high-quality studied for transmission electron microscopy and ultrafast electric diffraction from
Support the preparation of ultra thin single crystalline sample.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of the present invention
1 is silicon substrate, and 2 is silica membrane, and 3 is ultra thin single crystalline, and 4 is porous carbon film,
5 is standard contained network (i.e. standard transmission electron microscopy contained network), and 6 is isopropanol dropper, 7
For potassium hydroxide solution.
Detailed description of the invention
Below in conjunction with the accompanying drawings invention is described further.
Fig. 1 is the preparation flow schematic diagram of the present invention.
First, substrate is cleaned.Substrate used is to have dioxy thick for 300nm in superficial growth
The silicon substrate of SiClx thin film.Silicon dioxide thick for 300nm can be to the position of ultra thin single crystalline and thickness
Degree differentiates the optical contrast providing best, beneficially the carrying out of subsequent step.Cleaning method be
In acetone, ethanol and deionized water each ultrasonic 5-10 minute, and dry up with nitrogen.
Then, the technique utilizing adhesive tape to peel off on substrate prepares ultra thin single crystalline.Used is ultra-thin
Monocrystalline is stratified material, and such as materials such as graphite, topological insulator, high-temperature superconductors, they have
The highest anisotropy, available adhesive tape is had to dissociate thinning easily.The process of implementing is:
(I) cutting out fritter monocrystalline thin slice from bulky single crystal, size is more than 1mm × 1
mm×0.2mm.Then, lightly this monocrystalline thin slice is placed in a piece of adhesive tape with tweezers
Front, monocrystalline is adhered to tape surface.
(II) position in the front of another piece of tape with monocrystalline thin slice place is pasted together,
So, monocrystalline thin slice is just sandwiched between two panels adhesive tape.
(III) after the adhesive tape of monocrystalline thin slice side being opened, due to the anisotropy that monocrystalline is strong,
Being easy to dissociate, will all leave monocrystalline thin slice on two panels adhesive tape, now thin slice will division
Becoming some small pieces, the thickness of these small pieces also can be thinner much than original thin slice.
(IV) repeat this adhesive tape peel off technique after, will on adhesive tape remnants the most non-
The least and thin monocrystalline, the size of these monocrystalline from several microns to hundreds of micron, thickness
It is generally less than hundreds of nanometer.Examine the monocrystalline above these adhesive tapes under the microscope, pass through
Optical contrast finds the monocrystalline of thinner thickness.Generally monocrystalline is the thinnest, and color is the most shallow, the thinnest
The color of monocrystalline close with the color of adhesive tape.Select area compared with big, thickness is little and flat
Whole monocrystalline, the monocrystalline that best monocrystalline edge is the thickest.
(V), after choosing suitable monocrystalline, the front of the adhesive tape belonging to monocrystalline is placed in substrate
Above, wherein the region at selected monocrystalline place should be in the central authorities of substrate.By adhesive tape lightly from
After removing on substrate, just have the ultra thin single crystalline being invisible to the naked eye and fall within substrate, these monocrystalline
And combined by Van der Waals between atom between substrate.
(VI) utilize optical microscope and atomic force microscope find area compared with big, thickness is moderate
Ultra thin single crystalline.
It should be noted that the ultra thin single crystalline owing to utilizing mechanical stripping technique to prepare is to take
From in high-quality bulky single crystal, the quality of the ultra thin single crystalline obtained is also inevitable the highest, and defect is few,
Monocrystalline is the most smooth, does not haves the situation of crystal grain and crystal boundary, simultaneously mechanical stripping technological operation
Simply, it is not necessary to large-scale instrument, cost is the lowest, and therefore the application advantage in scientific research is very
Substantially.
Secondly, get out the standard contained network of transmission electron diffraction (TED), a diameter of 3mm of contained network,
Mesh number is more than 200, is attached with porous carbon film, the thickness 8nm-20 of porous carbon film in contained network
Nm, aperture 1 μm-6 μm.The size of the ultra thin single crystalline obtained due to mechanical stripping is less,
Therefore the existence of porous carbon film has beneficially ultra thin single crystalline to adhere better in contained network.Standard contained network
New contained network will be formed with porous carbon film.
Again, new contained network is being inverted in ultra thin single crystalline sample surfaces, the i.e. one side of porous carbon film just
To ultra thin single crystalline surface, form new contained network-ultra thin single crystalline-substrat structure；From the limit of ultra thin single crystalline
Drip several aqueous isopropanols at Yan, make solution penetrate into new contained network and the separating surface of ultra thin single crystalline, etc.
After solution natural evaporation, due to capillary effect, ultra thin single crystalline will be combined with new contained network；
In order to further increase the adhesion between ultra thin single crystalline and new contained network, by new contained network-super
Thin single crystal-substrat structure is positioned on hot plate heating；About 5 minutes heat time heating times, temperature controls
Within 200 degree；After this step, the strongest by having between ultra thin single crystalline and new contained network
Interaction force.
Finally, new contained network-ultra thin single crystalline-substrat structure is put into potassium hydroxide solution or hydroxide
In the highly basic such as sodium, concentration 25%-35% of solution.Strong base solution will corrode silicon dioxide, when
After silicon dioxide is corroded, new contained network-ultra thin single crystalline will be disengaged from substrate, and now ultra thin single crystalline is
Through being attached in new contained network, for new contained network-ultra thin single crystalline structure.
New contained network-ultra thin single crystalline structure is pulled out from solution, and carries out repeatedly deionized water punching
Wash, remove the pollutant on ultra thin single crystalline surface, after naturally drying, i.e. can be used for transmission electron diffraction (TED)
Experiment.
Utilize said method prepare self-supporting ultra thin single crystalline have simple and quick, low cost,
Success rate advantages of higher, is especially suitable for preparing the ultra thin single crystalline with high anisotropy.
Claims (9)
1. a preparation method for the ultra thin single crystalline sample studied for transmission electron diffraction (TED), its
It is characterised by, comprises the following steps:
1) ultra thin single crystalline is placed on the substrate of cleaning；Wherein, the thickness of ultra thin single crystalline is less than
100nm；
2) new contained network is inverted in ultra thin single crystalline surface, forms new contained network-ultra thin single crystalline-substrate
Structure；
Described new contained network includes porous carbon support membrane and standard transmission electron microscopy contained network, its
In, porous carbon support membrane is placed in standard transmission electron microscopy contained network；
New contained network is inverted in ultra thin single crystalline surface and refers to that the one side of porous carbon support membrane is just to ultra-thin
Single-crystal surface；
3) on new contained network-ultra thin single crystalline-substrat structure, instill aqueous isopropanol, make isopropanol
It is dry with the separating surface of ultra thin single crystalline natural evaporation that solution immerses new contained network；
4) by through step 3) new contained network-ultra thin single crystalline-substrat structure put into for dissolving lining
In the solution at the end, making substrate dissolve, ultra thin single crystalline departs from substrate, is attached in new contained network,
Form new contained network-ultra thin single crystalline structure；
5) by through step 4) new contained network-ultra thin single crystalline structure of being formed carries out repeatedly deionization
Water rinses, and naturally dries afterwards.
Preparation method the most according to claim 1, it is characterised in that step 1) in
Ultra thin single crystalline be stratified material, specially graphite, topological insulator or high-temperature superconductor.
Preparation method the most according to claim 2, it is characterised in that step 3) in
Aqueous isopropanol natural evaporation after, newer contained network-ultra thin single crystalline-substrat structure is positioned over heat
Heating on plate, about 5 minutes heat time heating times, temperature controls within 200 degree.
Preparation method the most according to claim 3, it is characterised in that step 1) in
Substrate be the silicon substrate that superficial growth has silica membrane thick for 300nm.
5. according to the preparation method described in claim 1 or 2 or 3 or 4, it is characterised in that
Step 4) in be strong base solution for dissolving the solution of substrate, the concentration of solution is 25%-35%.
Preparation method the most according to claim 5, it is characterised in that step 4) in
It is potassium hydroxide solution or sodium hydroxide solution for dissolving the solution of substrate.
Preparation method the most according to claim 6, it is characterised in that step 1) in
Ultra thin single crystalline be prepared by the technique utilizing adhesive tape to peel off.
Preparation method the most according to claim 7, it is characterised in that step 2) in
Porous carbon support membrane thickness is 8-20nm, aperture 1 μm-6 μm.
Preparation method the most according to claim 8, it is characterised in that step 2) in
The a diameter of 3mm of standard transmission electron microscopy contained network, mesh number is more than 200.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108663387A (en) * | 2018-05-16 | 2018-10-16 | 国家纳米科学中心 | A kind of method that wet etching prepares nano particle TEM sample |
| CN109254025A (en) * | 2018-11-02 | 2019-01-22 | 内蒙古工业大学 | A kind of device and method for pasting annular support grid for transmission electron microscope sample |
| CN111537529A (en) * | 2020-04-09 | 2020-08-14 | 中国科学院微电子研究所 | Silicon mesh for attaching transmission electron microscope sample and preparation method thereof |
| CN113130376A (en) * | 2021-04-13 | 2021-07-16 | 中国科学院上海微系统与信息技术研究所 | Preparation method of multilayer heterogeneous single crystal thin film substrate |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108663387A (en) * | 2018-05-16 | 2018-10-16 | 国家纳米科学中心 | A kind of method that wet etching prepares nano particle TEM sample |
| CN109254025A (en) * | 2018-11-02 | 2019-01-22 | 内蒙古工业大学 | A kind of device and method for pasting annular support grid for transmission electron microscope sample |
| CN109254025B (en) * | 2018-11-02 | 2023-09-22 | 内蒙古工业大学 | Device and method for sticking annular carrier net to transmission electron microscope sample |
| CN111537529A (en) * | 2020-04-09 | 2020-08-14 | 中国科学院微电子研究所 | Silicon mesh for attaching transmission electron microscope sample and preparation method thereof |
| CN113130376A (en) * | 2021-04-13 | 2021-07-16 | 中国科学院上海微系统与信息技术研究所 | Preparation method of multilayer heterogeneous single crystal thin film substrate |
| CN113130376B (en) * | 2021-04-13 | 2024-04-09 | 中国科学院上海微系统与信息技术研究所 | Preparation method of multilayer heterogeneous monocrystalline film substrate |
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