CN104616954B - A kind of transmission electron microscope NiTi non-crystaline amorphous metal contained network supports film - Google Patents
A kind of transmission electron microscope NiTi non-crystaline amorphous metal contained network supports film Download PDFInfo
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- CN104616954B CN104616954B CN201510020805.7A CN201510020805A CN104616954B CN 104616954 B CN104616954 B CN 104616954B CN 201510020805 A CN201510020805 A CN 201510020805A CN 104616954 B CN104616954 B CN 104616954B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
Abstract
The invention discloses a kind of transmission electron microscope NiTi non-crystaline amorphous metal contained network and support film and preparation method thereof.Conductive film of the present invention is Nitinol nano thin-film.Nitinol is marmem, has good elasticity and mechanical strength, is again good conductor electrically and thermally simultaneously, is widely used at aspects such as medical apparatus and instruments.Nitinol has defined industry in large scale now, is that a kind of being very easy to obtains alloy material.Prepare contained network with nickel-titanium alloy material and support film, the super-elasticity of marmem, high mechanical properties and excellent electric conductivity can be made full use of, solve the low and charged serious problem of mechanical strength that carbon supports film to exist.
Description
Technical field
The invention belongs to new opplication field and the transmission electron microscope field of metal material, especially NiTi amorphous alloy film being used for prepares grid of transmission electronic microscope and supports film.
Background technology
Nitinol is as the marmem of a kind of superior performance, except having shape memory function, also has good super-elasticity, electric conductivity, wearability, anticorrosive.Block Nitinol has had a wide range of applications in the various fields of engineering and medical science, can be used to make angiocarpy bracket etc..The thin film Nitinol method by magnetron sputtering, it is easy to obtain noncrystalline membrane, remain good electric conductivity and mechanical strength simultaneously, can be used to as backing material.
Transmission electron microscope can carry out Micro-Structure Analysis to material, reach subatomic resolution now, at natural science applied numerous areas, the particularly field such as physics, chemistry, material science, biology, medical science, geology plays the most important effect, and becomes the indispensable means of Micro-Structure Analysis.With transmission electron microscope carrier net, sample to be seen such as thin-film material, nano material, biomaterial etc. are it is generally required to support that film, as support, just can be put in transmission electron microscope and carry out Microstructure characterization.
The transmission electron microscope carrier net used at present supports that China of the film kind side of having film, carbon support film, collodion membrane, and thickness is that a few nanometer is to tens nanometers.The preparation method of China of side film is to be dissolved in organic solvent by China of side powder, with China of microscope slide insertion side powder solution, proposes microscope slide, after drying, being inserted by microscope slide in clean water, thin film is i.e. peeled off from microscope slide, floats on the water surface, then metal contained network is layered on film, finally filter paper is layered on metal contained network, after filter paper is soaked completely by water, filter paper is taken out from the water surface together with metal contained network, dry, i.e. obtain China of used in transmission electron microscope side film；The preparation method of collodion membrane is to drip the collodion solution of about 2% concentration in clean water face, until collodion solution after the water surface launches, spread metal contained network thereon, then filter paper is spread, after filter paper soaks, filter paper is taken out from the water surface together with metal contained network, dries, i.e. obtain used in transmission electron microscope collodion membrane；Carbon supports that the preparation of film is to support based on film by above two, for the purpose of increase electric conductivity, is deposited with one layer of amorphous carbon on film, i.e. obtains used in transmission electron microscope carbon and support film.These three supports that film preparation is convenient, and price is low,LackPoint is that electric conductivity is very poor.Side's China's film and collodion membrane are organic membrane, are insulator, non-conductive.Although carbon supports that film electric conductivity increases, but substantially insulator, electric conductivity is very poor.According to " Journal of Structural
Biology " 174, (2011), 420 423 reports, the electrical conductivity of carbon film reduces with thickness and reduces, and when thickness is at 5 below nm, electrical conductivity is 0, even if thickness is 20 nm, conductance is at 5*10-5Below Siemens, much smaller than the conductance (> 10 of metal5
Siemens), the conductance (10 of quasiconductor at most it is in-8 - 105
Siemens) in the range of.So, in transmission electron microscope, electron beam irradiation is on film, and electric charge cannot conduct diffusion in time, will produce charge accumulated at microcell.On the one hand these electric charges form electrostatic field, and the Coulomb repulsion power between electric charge can make the effect that carbon film is stressed, produce small displacement, sample thereon is also in company with drifting about, so that image blurring, particularly to high resolution picture, it is a key factor of restriction resolution；On the other hand the electrostatic field that charge accumulated produces can change the contrast of high resolution picture, the contrast that one electrostatic field of superposition causes on sample image, charged serious time show as forming black speck or black ring at sample surfaces, thus affect picture quality.Meanwhile, support that film is low due to mechanical strength, be susceptible to rupture, once rupture, will crimp rapidly under electron beam irradiation so that the sample on film crimps therewith for three kinds, it is impossible to observe.
Summary of the invention
For solving the charge accumulated of above-mentioned support film and the problem that mechanical strength is low, it is an object of the invention to provide a kind of NiTi non-crystaline amorphous metal contained network and support film and preparation method thereof.The present invention utilizes the super-elasticity of marmem, high mechanical properties and satisfactory electrical conductivity, improves transmission electron microscope carrier net and supports electric conductivity and the mechanical strength of film, and a kind of transmission electron microscope carrier net non-crystaline amorphous metal of preparation supports film.
It is an object of the invention to be achieved through the following technical solutions:
A kind of transmission electron microscope NiTi non-crystaline amorphous metal contained network supports film, and described NiTi non-crystaline amorphous metal contained network supports bottom-up contained network and the amorphous alloy film layer of being followed successively by of film, containing nickel element and titanium elements in described amorphous alloy film layer.
Further, content 40-60 at.% of described nickel element, the content of described titanium elements is 60-40 at.%.
Further, the thickness of described amorphous alloy film layer is 5-18 nm.
It is another object of the present invention to be achieved through the following technical solutions:
A kind of transmission electron microscope NiTi non-crystaline amorphous metal contained network supports the preparation method of film, and described preparation method comprises the following steps:
(1) organic membrane is prepared, as transition film；
(2) described organic membrane is floated in water, successively contained network, filter paper are layed on described organic membrane, obtain being covered with the contained network of organic membrane；
(3) use magnetron sputtering method or thermal evaporation, obtain in step (2) described in be covered with organic membrane carry the amorphous alloy film that deposited thereon a layer thickness is 5-18 nm, the contained network after being sputtered；
(4) the described post-depositional contained network that step (3) obtains is soaked in acetone soln, dissolve organic membrane substrate, then rinse in clean distilled water, contained network is pulled out, dry, standby, i.e. prepare described transmission electron microscope NiTi non-crystaline amorphous metal contained network and support film.
Further, the described organic membrane side of being China's film or collodion membrane.
Further, described contained network is copper mesh, nickel screen, molybdenum net or the one of Jin Wangzhong.
Further, described in described step (3), the condition of magnetron sputtering method is: sputtering power is 43 W, and film deposition rate is 0.2-0.5 nm/s, and sedimentation time is 30-90 s, and in coating process, substrate does not heats.
Further, described in step (3), the condition of thermal evaporation is: chooses the nitinol alloy wire of diameter 0.3 0.7 mm, is evacuated to 2*10-4Pa, film deposition rate is 0.2-0.5 nm/s, and sedimentation time is 30-90 s.
Conductive film of the present invention is Nitinol nano thin-film.Nitinol is marmem, has good elasticity and mechanical strength, is again good conductor electrically and thermally simultaneously, is widely used at aspects such as medical apparatus and instruments.Nitinol has defined industry in large scale now, is that a kind of being very easy to obtains alloy material.Prepare contained network with nickel-titanium alloy material and support film, the super-elasticity of marmem, high mechanical properties and excellent electric conductivity can be made full use of, solve the low and charged serious problem of mechanical strength that carbon supports film to exist.
Carbon supports that the atomic structure of film is non crystalline structure, has isotropism, the contrast of sample to be seen will not be produced impact.So, in order to ensure that Nitinol contained network supports that the atomic structure of film has isotropism, the present invention uses the method for magnetron sputtering carrying one layer of amorphous nickel-titanium alloy film of deposited thereon.In order to guarantee to obtain amorphous alloy film, therefore use Nitinol target, according to elemental metals target, then can only obtain polycrystal film, because it exists crystal grain and does not have isotropic, thus the contrast of sample to be seen can be produced interference.
Owing to being amorphous alloy film, so in transmission electron microscope, the diffraction ring of non-crystaline amorphous metal remains as typical amorphous ring, can be used to judge the state of object lens astigmatism.
In transmission electron microscope, when electron beam irradiation is on amorphous alloy film, electronics can be diffused into the non-irradiated region of surrounding rapidly from irradiation zone conduction, so that whole amorphous alloy film such that it is able to significantly weaken the charge accumulated phenomenon that electron beam irradiation region produces.
The present invention having the beneficial effect that compared to existing technology
1, NiTi non-crystaline amorphous metal contained network of the present invention supports film, utilize electric conductivity and the super-elasticity of marmem, can significantly weaken transmission electron microscope carrier net and support the charged phenomenon of film, the mechanical strength supporting film can be improved, it is not easy breakage, remain the non crystalline structure supporting film simultaneously, do not change the use habit using China of tradition side film, collodion membrane and carbon to support film to be formed；
2, during NiTi non-crystaline amorphous metal contained network of the present invention supports the preparation method of film, deposition process is selected and is used magnetron sputtering method and thermal evaporation.Use control sputtering method can realize large-scale mass production, stable performance, it is simple to state modulator；Using thermal evaporation also can realize batch production, stable performance, state modulator needs rule of thumb, and advantage is that equipment is cheap, and volume is little, can support that film uses same evaporation equipment with carbon, it is not necessary to add new equipment, it is possible to be greatly saved equipment cost, more economical.
Accompanying drawing explanation
Fig. 1 is that carbon supports that film and NiTi non-crystaline amorphous metal contained network support the Performance comparision schematic diagram of film.
Detailed description of the invention
Embodiment
1
A kind of transmission electron microscope NiTi non-crystaline amorphous metal contained network supports film, and described NiTi non-crystaline amorphous metal contained network supports bottom-up contained network and the amorphous alloy film layer of being followed successively by of film, containing nickel element and titanium elements in described amorphous alloy film layer.
Further, content 40-60 at.% of described nickel element, the content of described titanium elements is 60-40 at.%.
Further, the thickness of described amorphous alloy film layer is 5-18 nm.
Described transmission electron microscope NiTi non-crystaline amorphous metal contained network supports the preparation method of film, comprises the following steps:
(1) organic membrane is prepared, as transition film；
(2) described organic membrane is floated in water, successively contained network, filter paper are laid on described organic membrane, obtain being covered with the contained network of organic membrane；
(3) use magnetron sputtering method or hot steaming method, obtain in step (2) described in be covered with organic membrane carry the amorphous alloy film that deposited thereon a layer thickness is 5-18 nm, the contained network after being sputtered；
(4) the described post-depositional contained network that step (3) obtains is soaked in acetone soln, dissolve organic membrane substrate, then rinse in clean distilled water, contained network is pulled out, dry, standby, i.e. prepare described transmission electron microscope NiTi non-crystaline amorphous metal contained network and support film.
Further, the described organic membrane side of being China's film or collodion membrane.
Further, described contained network is copper mesh, nickel screen, molybdenum net or the one of Jin Wangzhong.
Further, described in described step (3), the condition of magnetron sputtering method is: sputtering power is 43 W, and film deposition rate is 0.2-0.5 nm/s, and sedimentation time is 30-90 s, and in coating process, substrate does not heats.
Further, described in step (3), the condition of thermal evaporation is: chooses the nitinol alloy wire of diameter 0.3 0.7 mm, is evacuated to 2*10-4Pa, film deposition rate is 0.2-0.5 nm/s, and sedimentation time is 30-90 s.
Embodiment
2
The present embodiment is the preferred version on the basis of embodiment 1, wherein China of organic membrane selection side film, and described NiTi non-crystaline amorphous metal gold contained network supports that the preparation method of film comprises the following steps:
(1) compound concentration is China of the side powder solution of 0.5%, by clean China of microscope slide insertion side powder solution, stand 10 s, from solution, propose microscope slide, in culture dish holding, dry, by the surrounding of thin film on blade scribing microscope slide, tilting to insert in clean distilled water by microscope slide, China of side film i.e. comes off from microscope slide, swims in distilled water surface.
(2) contained network acetone ultrasonic cleaning 5 min of film will not be supported, clean 2 times with clean distilled water again, pull out, dry, one by one on China of the side of being laid in film, cutting and an equal amount of filter paper of membrane area, it is layered on contained network, after filter paper is flooded profit completely, filter paper is pulled out together with contained network and the Fang Hua film of absorption from distilled water, the cultivation face of being placed on is dried, i.e. obtains the contained network of China of the side of being covered with film.
(3) the Nitinol target of customization suitable dimension is sputtering target material, and wherein the content of nickel element is 40-60 at.%, and the content of titanium elements is 60-40 at.%, and NiTi optimum ratio is 50: 50 at.%.
(4) contained network of China of the side of being covered with film is placed on the sample carrier of magnetic control sputtering device together with filter paper, fastens filter paper edge with microscope slide, put into magnetic control sputtering device, be evacuated to 2*10-4Pa, uses d.c. sputtering, and power 43 W, film deposition rate is 0.2 nm/s, and sedimentation time is 30-90 s, preferably 50 s, i.e. obtains the nickel-titanium alloy film of thickness about 5-18 nm.In deposition process, substrate does not heats.
(5) contained network after sputtering is soaked in acetone soln 1 min, China of the side of dissolving film substrate, rinse in clean distilled water, rinse 3 times, contained network is pulled out, dries, standby, i.e. prepare described NiTi non-crystaline amorphous metal contained network and support film.
Fig. 1 is that carbon supports that film and NiTi non-crystaline amorphous metal contained network support the Performance comparision of film.Fig. 1 (a) is that carbon supports film X rays topographs and at 450 pA/cm2Chronic exposure 4 min's as a result, it is possible to see gem-pure black irradiation ring under electron beam intensity.The ring of black is owing to the electronics in electron beam accumulates on carbon film, forms electrostatic field, causes contrast and strengthens and produce.Fig. 1 (b) is that NiTi non-crystaline amorphous metal contained network supports film X rays topographs and at 500 pA/cm2Under electron beam intensity, chronic exposure 8 min's as a result, it is possible to see simple black irradiation ring, shows that the degree of charge accumulated supports film much smaller than carbon, further relates to NiTi non-crystaline amorphous metal contained network and support that the electric conductivity of film is substantially better than carbon and supports the electric conductivity of film.Fig. 1 (c) and Fig. 1 (d) is that carbon supports that film and NiTi non-crystaline amorphous metal contained network support the electron diffraction pattern of film respectively, and both are typical amorphous dispersion ring, show that NiTi non-crystaline amorphous metal contained network supports that film is amorphous material, have isotropism.
Embodiment
3
The present embodiment is the preferred version on the basis of embodiment 1, and wherein organic membrane selects collodion membrane, and described NiTi non-crystaline amorphous metal gold contained network supports that the preparation method of film comprises the following steps:
(1) solvent, the collodion solution of preparation 2% are made with pentyl acetate；
(2) dripping collodion solution on clean distilled water surface with glass dropper, the collodion membrane of the water surface in water surface extension film forming, with clean lens paper, is plunderred, to clean the water surface rapidly by collodion solution；
(3) dripping collodion solution again on distilled water surface, collodion solution is rapidly in water surface extension film forming；
(4) contained network is immersed in 5 min in the acetone of cleaning, to clean the Organic substance on contained network surface, then rinses 3 times with clean distilled water, obtain cleaned contained network；
(5) cleaned contained network is layered on collodion membrane one by one, lines up array；
(6) filter paper of one piece of suitable size of cutting, is layered in contained network, after filter paper complete wetting, is taken out from the water surface together with contained network and collodion membrane by filter paper, dries, i.e. prepare the contained network being covered with collodion membrane；
(7) the Nitinol target of customization suitable dimension is sputtering target material, and wherein the content of nickel element is 40-60 at.%, and the content of titanium elements is 60-40 at.%, and NiTi optimum ratio is 50: 50 at.%.
(8) contained network being covered with collodion membrane is placed on the sample carrier of magnetic control sputtering device together with filter paper, fastens filter paper edge with microscope slide, put into magnetic control sputtering device, be evacuated to 2*10-4Pa, uses d.c. sputtering, and power 43 W, film deposition rate is 0.2 nm/s, and sedimentation time is 30-90 s, preferably 50 s, i.e. obtains the nickel-titanium alloy film of thickness about 5-18 nm.In deposition process, substrate does not heats.
(9) contained network after sputtering is soaked 1 min in acetone soln, dissolve collodion membrane substrate, rinse in clean distilled water, rinse 3 times, contained network is pulled out, dry, standby, i.e. prepare described NiTi non-crystaline amorphous metal contained network support film.
Embodiment
4
The present embodiment is the preferred version on the basis of embodiment 1, wherein China of organic membrane selection side film, and described NiTi non-crystaline amorphous metal gold contained network supports that the preparation method of film comprises the following steps:
(1) compound concentration is China of the side powder solution of 0.5%, by clean China of microscope slide insertion side powder solution, stand 10 seconds, from solution, propose microscope slide, in culture dish holding, dry, by the surrounding of thin film on blade scribing microscope slide, tilting to insert in clean distilled water by microscope slide, China of side film i.e. comes off from microscope slide, swims in distilled water surface.
(2) contained network acetone ultrasonic cleaning 5 min of film will not be supported, clean 2 times with clean distilled water again, pull out, dry, one by one on China of the side of being laid in film, cutting and an equal amount of filter paper of membrane area, it is layered on contained network, after filter paper is flooded profit completely, filter paper is pulled out together with contained network and the Fang Hua film of absorption from distilled water, the cultivation face of being placed on is dried, i.e. obtains the contained network of China of the side of being covered with film.
(3) contained network of China of the side of being covered with film is placed on the sample carrier of thermal evaporation instrument together with filter paper, filter paper edge is fastened with microscope slide, put into thermal evaporation plated film instrument, choose the nitinol alloy wire of diameter 0.3-0.7 mm, it is preferably 0.5 mm, in described nitinol alloy wire, the content of nickel element is 40-60 at.%, and the content of titanium elements is 60-40 at.%, and NiTi optimum ratio is 50: 50 at.%.Take nitinol alloy wire described in 1-2 cm and hang in tungsten filament evaporating basket, be evacuated to 2*10-4Pa, film deposition rate is 0.2 nm/s, and sedimentation time is 30-90 s, preferably 50 s, i.e. obtain deposited after contained network.
(4) post-depositional contained network is soaked in acetone soln 1 min, China of the side of dissolving film substrate, rinse in clean distilled water, rinse 3 times, contained network is pulled out, dry, standby, i.e. prepare described NiTi non-crystaline amorphous metal contained network support film.
Claims (9)
1. a transmission electron microscope NiTi non-crystaline amorphous metal contained network supports film, it is characterised in that described NiTi non-crystaline amorphous metal contained network supports bottom-up contained network and the amorphous alloy film layer of being followed successively by of film, containing nickel element and titanium elements in described amorphous alloy film layer；
Described transmission electron microscope NiTi non-crystaline amorphous metal contained network supports that the preparation method of film comprises the following steps:
(1) organic membrane is prepared, as transition film；
(2) described organic membrane is floated in water, successively contained network, filter paper are layed on described organic membrane, obtain being covered with the contained network of organic membrane；
(3) use magnetron sputtering method or thermal evaporation, obtain in step (2) described in be covered with organic membrane carry the amorphous alloy film that deposited thereon a layer thickness is 5-18 nm, the contained network after being sputtered；
(4) the described post-depositional contained network that step (3) obtains is soaked in acetone soln, dissolve organic membrane substrate, then rinse in clean distilled water, contained network is pulled out, dry, standby, i.e. prepare described transmission electron microscope NiTi non-crystaline amorphous metal contained network and support film.
Transmission electron microscope NiTi non-crystaline amorphous metal contained network the most according to claim 1 supports film, it is characterised in that the content of described nickel element is 40-
60 at.%, the content of described titanium elements is 60-40 at.%.
Transmission electron microscope NiTi non-crystaline amorphous metal contained network the most according to claim 2 supports film, it is characterised in that the proportioning of described nickel element and titanium elements is 50
: 50 at.%。
Transmission electron microscope NiTi non-crystaline amorphous metal contained network the most according to claim 1 supports film, it is characterised in that the thickness of described amorphous alloy film layer is 5
- 18 nm。
5. the preparation method of NiTi non-crystaline amorphous metal contained network support film of the transmission electron microscope as described in any one of claim 1-4, it is characterised in that described preparation method comprises the following steps:
(1) organic membrane is prepared, as transition film；
(2) described organic membrane is floated in water, successively contained network, filter paper are layed on described organic membrane, obtain being covered with the contained network of organic membrane；
(3) use magnetron sputtering method or thermal evaporation, obtain in step (2) described in be covered with organic membrane carry the amorphous alloy film that deposited thereon a layer thickness is 5-18 nm, the contained network after being sputtered；
(4) the described post-depositional contained network that step (3) obtains is soaked in acetone soln, dissolve organic membrane substrate, then rinse in clean distilled water, contained network is pulled out, dry, standby, i.e. prepare described transmission electron microscope NiTi non-crystaline amorphous metal contained network and support film.
Transmission electron microscope NiTi non-crystaline amorphous metal contained network the most according to claim 5 supports the preparation method of film, it is characterised in that the described organic membrane side of being China's film or collodion membrane.
Transmission electron microscope NiTi non-crystaline amorphous metal contained network the most according to claim 5 supports the preparation method of film, it is characterised in that described contained network is copper mesh, nickel screen, molybdenum net or the one of Jin Wangzhong.
Transmission electron microscope NiTi non-crystaline amorphous metal contained network the most according to claim 5 supports the preparation method of film, it is characterized in that, described in step (3), the condition of magnetron sputtering method is: selecting Nitinol target is sputtering target material, sputtering power is 43 W, film deposition rate is 0.2-0.5 nm/s, sedimentation time is 30-90 s, and in coating process, substrate does not heats.
Transmission electron microscope NiTi non-crystaline amorphous metal contained network the most according to claim 5 supports the preparation method of film, it is characterized in that, described in step (3), the condition of thermal evaporation is: chooses the nitinol alloy wire of diameter 0.3-0.7 mm, is evacuated to 2 × 10-4Pa, film deposition rate is 0.2-0.5 nm/s, and sedimentation time is 30-90 s.
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| CN110632105B (en) * | 2019-09-17 | 2021-10-29 | 东南大学 | Liquid sample cavity for transmission electron microscope characterization and preparation method thereof |
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| CN111218657B (en) * | 2020-01-03 | 2021-07-30 | 北京工业大学 | Amorphous tungsten-based high-entropy alloy thin film material and preparation method thereof |
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