CN108871890A - A method of TEM sample is prepared using graphene as protective layer - Google Patents
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The invention discloses a kind of using transfer or the graphene directly grown using chemical vapor deposition as the method for protective layer preparation TEM sample, it is mainly characterized by transferring graphene to or directly growing into the material surface for needing to prepare TEM sample, damage and pollution caused by the material of observation is in sample preparation procedure needed for being avoided using graphene, and obtain the TEM sample containing graphene protective layer, if this protective layer does not influence Germicidal efficacy, transmission electron microscope observing can be directly placed into, if wanting to remove this layer of protective layer, then (550 DEG C) calcining a period of times (2h) are removed at high temperature.The present invention is of great significance for the production of structural integrity, zero damage TEM sample.
Description
Technical field
The invention belongs to Material Fields, and in particular to a method of TEM sample is prepared using graphene protective layer.
Background technique
Any material has the surface contacted with the external world, compared with its inside body, either in structure or is changing
Learning on composition has apparent difference, and the most important means in research material surface are STM at present, but the principle based on STM, this
Method is only limitted to the research to nonisulated body material surface, for some insulating materials for having major application prospect nothing in a helpless situation
Plan.And transmission electron microscope (TEM) can solve this problem, no matter insulate or non-insulating material, Wo Mendou
Its property can be probed by TEM, more intuitive associated materials can be regulated and controled on an atomic scale.But it is making
During TEM sample, sample surfaces are easy to contaminated and damage, so that sample loses its intrinsic crystal structure, to us
The structure-activity relationship for further looking at and constructing material, which generates, inevitably to be influenced.Graphene is by carbon atom with sp2 hydridization shape
At hexagon cellular shape planar ultrathin film material, outside proton free, atom etc. cannot be penetrated, can be in thinning process
When protecting sample surfaces structure well, make it not by the destruction of other foreign particles, and applying external force to sample, graphene
The meeting bending deformation of carbon atom face carrys out the power that relaxation is subject to；In addition, calcining graphene at high temperature, it can be made to be oxidized to CO2 gas
Body vapors away.We are ultra-thin, flexible using graphene, can shield foreign particles and characteristic that high temperature can remove, by metal liner
Protective layer is made on the surface of observation material needed for the graphene grown on bottom is shifted or directly grown into, and sample is protected in sample making course
Product surface, and then structural integrity, zero damage TEM sample are obtained, this probes into material properties for us, developing research method has
Irreplaceable role.
Summary of the invention
It can subtract in ion for some technical problems in current TEM sample preparation process, such as surface of all product in section
The pollution that the actual conditions, sample surfaces that lead to not judge the sample surfaces are broken during thin (has in sample making course
The phenomenon that impurity element is to Segregation at interface) and sample surfaces the problems such as generating stress, the present invention provide it is a kind of using transfer or
The graphene directly grown using chemical vapor deposition is as the method for protective layer preparation TEM sample.
Specifically, transfer step is as follows：
(1) continuous graphite alkene film is grown using chemical vapour deposition technique on metal foil (copper foil or nickel foil) substrate,
4%PMMA solution is spun to the metal foil-based bottom surface with graphene；
(2) thermal station temperature is set as 70 DEG C, and graphene/metal foil of spin coating PMMA is placed in thermal station and heats 3~5min, is made
Solvent volatilization is clean in PMMA solution；
(3) there is the one side of PMMA to be put into ferric chloride solution in a manner of upward by spin coating graphene/metal foil, stand extremely
Substrate is separated with graphene/PMMA layers；
(4) graphene/PMMA layers is fished in pure deionized water with clean filter paper, 1~2 drop isopropyl is added dropwise
Alcohol makes graphene/PMMA sufficiently unfold, move, to remove the iron chloride of its adsorption；
(5) by Sapphire Substrate (being not limited only to Sapphire Substrate herein, other any need materials to be protected)
Successively respectively it is cleaned by ultrasonic 5min with ultrapure water, isopropanol, acetone, cleaning finishes use and is dried with nitrogen, wherein the power of ultrasound is
90W；
(6) graphite is fished for the TEM sample to be sampled (length and width are respectively that 5 × 5mm is advisable) after the cleaning of required size
Alkene/PMMA, 70 DEG C of heating make film tightly be attached to sample surfaces；
(7) it takes a beaker that proper amount of acetone is added to be heated to boiling, clamps PMMA- graphene/sapphire with tweezers, transfer has
The one of graphene is placed face down at acetone ullage 1-2cm, stands 10-15min, is condensed back to acetone in sapphire surface
Stream is taken out and with removing PMMA with being dried with nitrogen later；
Specifically, the parameter for growing graphene directly on the material resistant to high temperature of required sample preparation is as follows：
In the graphene chemical vapor deposition, the method for chemical vapor deposition concretely aumospheric pressure cvd
(APCVD), low-pressure chemical vapor deposition (LPCVD) or plasma enhanced chemical vapor deposition (PECVD).
(1) specifically, in the aumospheric pressure cvd, carbon source is methane or ethylene；
Depositing temperature is 1000 DEG C -1100 DEG C, specially 1050 DEG C；
Deposition pressure is normal pressure；
Carrier gas is the gaseous mixture being made of argon gas and hydrogen, and wherein the flow-rate ratio of argon gas and hydrogen is 1-10：1, specially
5：1；The flow of argon gas is specially 100-1000sccm, specially 500sccm；The flow of hydrogen is 50-500sccm, specially
100sccm；
The flow of carbon source is 10-50sccm, concretely 20sccm；
Sedimentation time is 0.5h-5h, specially 3h；
(2) in the low-pressure chemical vapor deposition, carbon source is alcohol vapour；
Depositing temperature is 1000 DEG C -1100 DEG C, concretely 1080 DEG C；
Deposition pressure is 200-5000Pa, specially 250Pa；
Carrier gas is the gaseous mixture being made of argon gas and hydrogen, and wherein the flow-rate ratio of argon gas and hydrogen is 1-10:1, specifically may be used
It is 5：1；The flow of argon gas concretely 100-1000sccm, specially 500sccm；The flow of hydrogen is 50-500sccm, tool
Body is 100sccm；
The flow of carbon source is 500sccm；The partial pressure of carbon source is 250Pa；
Sedimentation time is 0.5h-5h, specially 1h；
(3) in the plasma enhanced chemical vapor deposition, carbon source is methane or ethylene；
Depositing temperature is 500 DEG C -800 DEG C, specially 600 DEG C；
Deposition pressure is 100-2000Pa, specially 500Pa；
The flow of carbon source concretely 5-50sccm, specially 18sccm；
Plasma generator power is 60-200W, specially 120W；
Sedimentation time is 0.5h-2h, specially 1h.
The method also includes：Before the chemical vapor deposition step, to the high temperature resistant of required protection material to be sampled
Material is pre-processed；
Specifically, the pretreatment includes that the need material to be sampled to be protected is successively used ultrapure water, isopropanol, third
Ketone is respectively cleaned by ultrasonic 5min, and cleaning finishes use and is dried with nitrogen；
In the ultrasonic step, ultrasonic power is 90W.
Of the invention is mainly characterized by transferring graphene to or directly grow into the material table for needing to prepare TEM sample
Face, the material observed needed for being avoided using graphene in sample preparation procedure caused by damage and pollution, and contained
The TEM sample of graphene protective layer can be directly placed into transmission electron microscope observing if this protective layer does not influence Germicidal efficacy, if
Want to remove this layer of protective layer, then (550 DEG C) calcining a period of times (2h) are removed at high temperature.The present invention is for structure
The production of complete whole, zero damage TEM sample is of great significance.
Detailed description of the invention
Figure one is the TEM sample spherical aberration Electronic Speculum HADDF picture made using this method, by comparison it can be seen that there is graphite
The sample performance structure of alkene protective layer is complete；Surface texture without graphene protective layer is destroyed, and can not judge structure.
Specific embodiment
The present invention is further elaborated combined with specific embodiments below, but the present invention is not limited to following embodiments.Institute
State method is conventional method unless otherwise instructed.Affiliated raw material can obtain unless otherwise instructed from public commercial source.
Embodiment 1
A kind of preparation method of the surface texture using graphene protection TEM sample preparation, steps are as follows：
(1) graphene is grown using chemical vapour deposition technique on metal foil (copper foil or nickel foil) substrate, by 0.5mL
4%PMMA solution is spun to the metal foil-based bottom surface with graphene；
(2) thermal station temperature is set as 70 DEG C, and graphene/metal foil of spin coating PMMA is placed in thermal station and heats 3~5min, is made
Solvent volatilization is clean in PMMA solution；
(3) there is the one side of PMMA to be put into ferric chloride solution in a manner of upward by spin coating graphene/metal foil, stand extremely
Substrate is separated with graphene/PMMA layers；
(4) graphene/PMMA layers is fished in pure deionized water with clean filter paper, 1~2 drop isopropyl is added dropwise
Alcohol makes graphene/PMMA sufficiently unfold, move, to remove the iron chloride of its adsorption；
(5) by Sapphire Substrate (being not limited only to Sapphire Substrate herein, other any need materials to be protected)
Successively respectively it is cleaned by ultrasonic 5min with ultrapure water, isopropanol, acetone, cleaning finishes use and is dried with nitrogen, wherein the power of ultrasound is
90W；
(6) graphite is fished for the TEM sample to be sampled (length and width are respectively that 5 × 5mm is advisable) after the cleaning of required size
Alkene/PMMA, 70 DEG C of heating make film tightly be attached to sample surfaces；
(7) it takes a beaker that proper amount of acetone is added to be heated to boiling, clamps PMMA- graphene/sapphire with tweezers, transfer has
The one of graphene is placed face down at acetone ullage 1-2cm, stands 10-15min, is condensed back to acetone in sapphire surface
Stream is taken out and with removing PMMA with being dried with nitrogen later；
(8) silicon wafer of required size acetone is cleaned by ultrasonic 5min, cleaning finishes use and is dried with nitrogen；
(9) G1 glue is configured by corresponding proportion, after mixing evenly with toothpick, is applied on silicon wafer after cleaning at once, and
Glue is even flat, even thin as far as possible with toothpick, then there is the side of graphene to gluing with sapphire, is pressed with tweezers, make two
Person is in close contact, and is sandwiched to be placed in thermal station on spring base and heats 3h, and heating temperature is 70 DEG C；
(10) heating finishes and after Temperature fall, it is contacted with the fixed iron block of the cutting for filling paraffin, is solidificated in it
On iron block, and it is cut to 2 × 3mm size (on the basis of sapphire) with saw at a slow speed；
(11) take one piece of sample cut, make section sample, with tripod sample grinding tool platform by thickness be ground to 100 microns with
Under, molybdenum ring is then glued, is removed after heating 20min, is put and steep 30min in acetone, ion milling can be carried out by, which taking out, obtains
Final transmission sample；
(12) if desired graphene protective layer is removed, then sample can be put into crucible upwards, then crucible is put into pipe
In formula furnace (or other any instruments that can complete high-temperature process), 550 DEG C are warming up to, high-temperature process 2h delays crucible
Slowly it takes out, under the microscope glue (paraffin), is sticked to sample firmly on molybdenum ring, obtain the sample of removal graphene protective layer；
If this step can be ignored without removing graphene protective layer.
As a result, it has been found that the TEM sample prepared using the method, is able to observe that lossless in the region for having graphene to protect
Sapphire surface, and can be clearly seen that sapphire stop layer is Al atomic layer (Fig. 1 f)；In the area of no graphene protection
Domain, sample have different degrees of damage (Fig. 1 a-e).
Embodiment 2
Step is a difference in that in (5) step that TEM sample to be made is not limited only to Sapphire Substrate with embodiment 1, other
Any material for needing sample preparation such as material such as AlN, GaN, InGaN, AlGaN, SrTiO3, is not limited only to single material, and two kinds
Or the function element that compound, stacking material and any materials of multiple material are constituted is whether great or small, is not limited only to without special place
Situations such as material of the surfacing of reason further includes the substrate material of various surface graphics, above equal is also applicable in.
Embodiment 3
For step with embodiment 1, being a difference in that can be using the method for CVD directly by graphite for TEM sample resistant to high temperature
Alkene is grown in its surface, specifically by step 1-7 replace with following two step (1) Sapphire Substrate successively used ultrapure water,
Isopropanol, acetone are respectively cleaned by ultrasonic 5min, and cleaning finishes use and is dried with nitrogen, wherein the power of ultrasound is 90W；
(2) graphene film is grown：The clean sapphire glass substrate that step (1) is obtained is put into APCVD cavity, will
Ar and H2 gas flowmeter is respectively set as 500sccm and 300sccm, after gas washing, furnace body is warming up to 1060 DEG C, is being risen
Keep Ar and H2 flow velocity constant during temperature.After furnace temperature rises to 1060 DEG C, after stablizing 15min, it is by CH4 flow meter settings
30sccm, growth time 5h, growth finish, Temperature fall, obtain the sapphire of graphene covering.
Finally it is similarly obtained the TEM sample with lossless surface protected by graphene.
Embodiment 4
For the material of TEM sample to be made described in embodiment 2, if its high temperature resistant, step 1-7 can be replaced with to utilization
The method of CVD is directly by graphene growth on its surface.Specifically replace with 1,2 two step in embodiment 3.
Embodiment 5
The step of according to embodiment 1, APCVD only is replaced with LPCVD, depositional environment is environment under low pressure；Depositing temperature is
1080℃；Carrier gas is the gaseous mixture being made of argon gas and hydrogen, and wherein the flow-rate ratio of argon gas and hydrogen is 5：1, specifically, argon gas
Flow be 500sccm, the flow of hydrogen is 100sccm；Carbon source is alcohol vapour, flow set 500sccm, divides and is
250Pa；Sedimentation time is 1h.Finally it is similarly obtained lossless TEM sample.
Embodiment 6
It the step of according to embodiment 1, is only replaced in APCVD with PECVD, depositional environment is environment under low pressure, and pressure is
100Pa；Depositing temperature is 600 DEG C；Carbon source is methane, flow 18sccm, and plasma generator power is 120W, when deposition
Between be 1h.Finally it is similarly obtained lossless TEM sample.
The above example of making is general embodiment of the invention, can actually take embodiment there are also very much, including stone
Black alkene protects other any materials to do TEM sample and other microobjects, and all claims according to the present invention are done
Equivalent change or modification, all should belong to covering scope of the invention.
Claims (7)
1. a kind of using graphene as the method for protective layer preparation TEM sample, which is characterized in that transfer graphene to or sharp
The material surface of preparation TEM sample needed for directly being grown into chemical vapor deposition, is observed needed for being avoided using graphene
Material in sample preparation procedure caused by surface damage and pollution, and by manual sample grinding, ion beam be thinned or utilize Fib
(focused ion-electronics double-beam system) obtains the TEM sample containing graphene protective layer, if this protective layer does not influence experiment and sees
Examine, transmission electron microscope observing can be directly placed into, if wanting to remove this layer of protective layer, at high temperature (550 DEG C) calcining one section when
Between (2h) be removed.
2. as described in claim 1 using graphene as the method for protective layer preparation TEM sample, which is characterized in that described
Graphene transfer method, the specific steps are：
(1) continuous graphite alkene film is grown using chemical vapour deposition technique on metal foil (copper foil or nickel foil) substrate, by 4%
PMMA solution is spun to the metal foil-based bottom surface with graphene；
(2) thermal station temperature is set as 70 DEG C, and graphene/metal foil of spin coating PMMA is placed in thermal station and heats 3~5min, makes PMMA
Solvent volatilization is clean in solution；
(3) there is the one side of PMMA to be put into ferric chloride solution in a manner of upward by spin coating graphene/metal foil, stand to substrate
It is separated with graphene/PMMA layers；
(4) graphene/PMMA layers is fished in pure deionized water with clean filter paper, 1~2 drop isopropanol is added dropwise,
Graphene/PMMA is set sufficiently to unfold, move, to remove the iron chloride of its adsorption；
(5) successively by Sapphire Substrate (being not limited only to Sapphire Substrate herein, other any need materials to be protected)
Respectively it is cleaned by ultrasonic 5min with ultrapure water, isopropanol, acetone, cleaning finishes use and is dried with nitrogen, wherein the power of ultrasound is 90W；
(6) with the TEM sample to be sampled (length and width are respectively that 5 × 5mm is advisable) after the cleaning of required size fish for graphene/
PMMA, 70 DEG C of heating make film tightly be attached to sample surfaces；
(7) it takes a beaker that proper amount of acetone is added to be heated to boiling, clamps PMMA- graphene/sapphire with tweezers, transfer has graphite
The one of alkene is placed face down at acetone ullage 1-2cm, stand 10-15min, make acetone sapphire surface be condensed back with
PMMA is removed, is taken out later and with being dried with nitrogen.
3. as described in claim 1 using graphene as the method for protective layer preparation TEM sample, which is characterized in that directly
The parameter that graphene is grown on the material resistant to high temperature of required sample preparation is as follows：In the graphene chemical vapor deposition, chemistry
The method of vapor deposition concretely aumospheric pressure cvd (APCVD), low-pressure chemical vapor deposition (LPCVD) or plasma
Body enhances chemical vapor deposition (PECVD).
(1) specifically, in the aumospheric pressure cvd, carbon source is methane or ethylene；
Depositing temperature is 1000 DEG C -1100 DEG C, specially 1050 DEG C；
Deposition pressure is normal pressure；
Carrier gas is the gaseous mixture being made of argon gas and hydrogen, and wherein the flow-rate ratio of argon gas and hydrogen is 1-10：1, specially 5：1；
The flow of argon gas is specially 100-1000sccm, specially 500sccm；The flow of hydrogen is 50-500sccm, specially
100sccm；
The flow of carbon source is 10-50sccm, concretely 20sccm；
Sedimentation time is 0.5h-5h, specially 3h；
(2) in the low-pressure chemical vapor deposition, carbon source is alcohol vapour；
Depositing temperature is 1000 DEG C -1100 DEG C, concretely 1080 DEG C；
Deposition pressure is 200-5000Pa, specially 250Pa；
Carrier gas is the gaseous mixture being made of argon gas and hydrogen, and wherein the flow-rate ratio of argon gas and hydrogen is 1-10:1, concretely 5：
1；The flow of argon gas concretely 100-1000sccm, specially 500sccm；The flow of hydrogen is 50-500sccm, specially
100sccm；
The flow of carbon source is 500sccm；The partial pressure of carbon source is 250Pa；
Sedimentation time is 0.5h-5h, specially 1h；
(3) in the plasma enhanced chemical vapor deposition, carbon source is methane or ethylene；
Depositing temperature is 500 DEG C -800 DEG C, specially 600 DEG C；
Deposition pressure is 100-2000Pa, specially 500Pa；
The flow of carbon source concretely 5-50sccm, specially 18sccm；
Plasma generator power is 60-200W, specially 120W；
Sedimentation time is 0.5h-2h, specially 1h.
4. as described in claim 1 using graphene as the method for protective layer preparation TEM sample, which is characterized in that described
Manual sample grinding the specific steps are：
(1) sapphire that there is graphene on surface is obtained using graphene transfer method as claimed in claim 2；
(2) silicon wafer of required size acetone is cleaned by ultrasonic 5min, cleaning finishes use and is dried with nitrogen；
(3) G1 glue is configured by corresponding proportion, after mixing evenly with toothpick, is applied on silicon wafer after cleaning at once, and by glue
Water is even flat, even thin as far as possible with toothpick, then has the side of graphene to gluing with sapphire, is pressed with tweezers, keeps the two tight
Contiguity touching, and be sandwiched to be placed in thermal station on spring base and heat 3h, heating temperature is 70 DEG C；
(4) heating finishes and after Temperature fall, it is contacted with the fixed iron block of the cutting for filling paraffin, it is made to be solidificated in iron block
On, and it is cut to 2 × 3mm size (on the basis of sapphire) with saw at a slow speed；
(5) one piece of sample cut is taken, section sample is made, thickness is ground to 100 microns hereinafter, benefit with tripod sample grinding tool platform
Molybdenum ring (molybdenum annular aperture there are the plurality of specifications such as 0.6mm, 0.8mm, 1.0mm, 1.5mm) is adhered in ground sample in cross section with AB glue,
Make molybdenum ring inner hole just in the interface of sapphire and silicon wafer, then specimen holder is put into thermal station and heats 20min, by sheet glass
It is removed together with sample, puts and steep 30min in acetone, sample, which is taken out, can carry out ion milling.
5. it is as described in claim 1 using graphene as the method for protective layer preparation TEM sample, it is characterized in that, uses ion
Instrument is thinned, thickness of sample obtained in claim 4 is reduced into 50nm or so according to parameter once：
(1) high pressure：4.5kv, angle：6 °, left rifle line：25uA, right rifle line：26uA, time：40min；
(2) high pressure：4kv, angle：6 °, left rifle line：20uA, right rifle line：21uA, time：90min；
(3) high pressure：3.5kv, angle：6 °, left rifle line 15uA, right rifle line：16uA, time：65min；
(4) high pressure：1.5kv, angle：3 °, left rifle line：5uA, right rifle line：6uA, time：5min.
6. as described in claim 1 using graphene as the method for protective layer preparation TEM sample, which is characterized in that can benefit
With Fib according to the acquisition of following general steps with a thickness of the TEM sample of 50nm or so：
(1) needle point initializes；
(2) needle point is repaired；
(3) sample is moved to the operating position FIB；
(4) needle point is encountered on the sample cut；
(5) sample cut is welded on needle point；
(6) cutting sample right edge connection；
(7) lift sample；
(8) sample will be cut and is moved to V-groove；
(9) sample on needle point is moved to V-groove；
(10) sample cut is soldered on V-groove；
(11) needle point is cut off；
(12) continued to reduce to thickness of sample into 50nm or so with the ion beam of Fib, or use thickness of sample according to claim 5
Ion Beam Thinner reduces to 50nm or so.
7. as described in claim 1 using graphene as the method for protective layer preparation TEM sample, which is characterized in that required system
The material of standby TEM sample, not only the block materials such as including Al2O3, AlN, SiO2, GaN, further include thin-film material, stratiform material
The material of any need TEM characterization such as material and nano particle.
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| CN111855716A (en) * | 2019-04-25 | 2020-10-30 | 中国科学院物理研究所 | Preparation method of TEM sample |
| CN111996793A (en) * | 2020-09-09 | 2020-11-27 | 宁波中冶电子科技有限公司 | Preparation method and application of graphene antibacterial cloth |
| CN111326310B (en) * | 2020-02-24 | 2020-12-29 | 上海景瑞阳实业有限公司 | High-temperature-resistant samarium-cobalt permanent magnet and preparation method thereof |
| CN112687605A (en) * | 2020-12-28 | 2021-04-20 | 华东师范大学 | Method for reducing chip electron radiation damage and chip with less electron radiation damage |
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| CN110579495A (en) * | 2019-10-23 | 2019-12-17 | 长江存储科技有限责任公司 | TEM sample and preparation method thereof |
| CN110579495B (en) * | 2019-10-23 | 2022-06-28 | 长江存储科技有限责任公司 | TEM sample and preparation method thereof |
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