CN104616954A - Nickel-titanium amorphous alloy grid supporting film for transmission electron microscope - Google Patents
Nickel-titanium amorphous alloy grid supporting film for transmission electron microscope Download PDFInfo
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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
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Abstract
The invention discloses a nickel-titanium amorphous alloy grid supporting film for a transmission electron microscope and a preparation method of the nickel-titanium amorphous alloy grid supporting film. A conductive film used is a nickel-titanium alloy nanometer film; the nickel-titanium alloy is shape memory alloy which is high in elasticity and mechanical strength, serves as a good conductor for power and heat and can be widely applied to medical apparatuses and instruments. The nickel-titanium alloy is in a large-scale industry at present and is the alloy material easily obtained. The grid supporting film is prepared from the nickel-titanium alloy material, and thus the superelasticity, the high mechanical strength and the outstanding conductivity of the shape memory alloy can be fully utilized to problems of low mechanical strength and serious electric charge of a carbon supporting film can be solved.
Description
Technical field
The invention belongs to new opplication field and the transmission electron microscope field of metal material, especially by NiTi amorphous alloy film for the preparation of grid of transmission electronic microscope supporting film.
Background technology
Nitinol, as a kind of marmem of superior performance, except having shape memory function, also has good super-elasticity, conductivity, resistance to wear, anticorrosive.Block Nitinol has a wide range of applications in the various fields of engineering and medical science, can be used for making angiocarpy bracket etc.Film Nitinol, by the method for magnetron sputtering, is easy to obtain noncrystalline membrane, remains good conductivity and mechanical strength simultaneously, can be used as backing material.
Transmission electron microscope can carry out Micro-Structure Analysis to material, reach subatomic resolution now, at natural science applied numerous areas, particularly the field such as physics, chemistry, material science, biology, medical science, geology plays more and more important effect, and becomes the indispensable means of Micro-Structure Analysis.Sample to be seen needs to use transmission electron microscope carrier net supporting film as support as thin-film material, nano material, biomaterial etc., just can put into transmission electron microscope and carry out Microstructure characterization.
The magnificent film in the transmission electron microscope carrier net supporting film kind side of having, carbon supporting film, the collodion membrane that use at present, thickness is a few nanometer to tens nanometers.The magnificent powder in side is dissolved in organic solvent by the preparation method of the magnificent film in side, with the magnificent powder solution in slide insertion side, proposes slide, after drying, inserted by slide in clean water, namely film is peeled off from slide, floats on the water surface, then metal is carried net laying on film, finally filter paper being layered on metal carries on net, after filter paper is soaked completely by water, filter paper is carried net together with metal and takes out from the water surface, dry, namely obtain China of used in transmission electron microscope side film; The preparation method of collodion membrane is the collodion solution dripping about 2% concentration in clean water face, until collodion solution after the water surface launches, spread metal thereon and carry net, then filter paper is spread, after filter paper soaks, filter paper is carried net together with metal take out from the water surface, dry, namely obtain used in transmission electron microscope collodion membrane; The preparation of carbon supporting film is based on above-mentioned two kinds of supporting films, and for the object increasing conductivity, evaporation one deck amorphous carbon on film, namely obtains used in transmission electron microscope carbon supporting film.These three kinds of supporting films are easy to prepare, and price is low,
lackpoint is that conductivity is very poor.The magnificent film in side and collodion membrane are organic films, are insulator, non-conductive.Although carbon supporting film conductivity increases, substantially or insulator, conductivity is very poor.According to " Journal of Structural Biology " 174, (2011), 420 – 423 report, the conductivity of carbon film reduces with thickness and reduces, and when thickness is at 5 below nm, conductivity is 0, even if thickness is 20 nm, conductance is at 5*10
-5below Siemens, much smaller than the conductance (> 10 of metal
5siemens), the conductance (10 of semiconductor is at the most
-8-10
5siemens) in scope.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.These electric charges form electrostatic field on the one hand, and the Coulomb repulsion power between electric charge can make carbon film be subject to the effect of stress, produces small displacement, sample on it is also in company with drifting about, thus make image blurring, particularly to high resolution picture, be a key factor of restriction resolution; The electrostatic field that on the other hand charge accumulated produces can change the contrast of high resolution picture, superposes the contrast that an electrostatic field causes on sample image, charged serious time show as and form blackspot or black ring at sample surfaces, thus affect picture quality.Meanwhile, three kinds of supporting films are low due to mechanical strength, easily break, once break, will occur rapidly curling, the sample on film be occurred curling thereupon, cannot observe under electron beam irradiation.
Summary of the invention
For the problem that the charge accumulated and mechanical strength that solve above-mentioned supporting film are low, the object of this invention is to provide a kind of NiTi non-crystaline amorphous metal and carry net supporting film and preparation method thereof.The present invention utilizes the super-elasticity of marmem, high mechanical properties and satisfactory electrical conductivity, improves conductivity and the mechanical strength of transmission electron microscope carrier net supporting film, prepares a kind of transmission electron microscope carrier net non-crystaline amorphous metal supporting film.
The object of the invention is to be achieved through the following technical solutions:
A kind of transmission electron microscope NiTi non-crystaline amorphous metal carries net supporting film, and described NiTi non-crystaline amorphous metal carries bottom-up being followed successively by of net supporting film and carries net and amorphous alloy thin rete, containing nickel element and titanium elements in described amorphous alloy thin rete.
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 thin rete is 5-18 nm.
Another object of the present invention is achieved through the following technical solutions:
Transmission electron microscope NiTi non-crystaline amorphous metal carries a preparation method for net supporting film, and described preparation method comprises the following steps:
(1) organic film is prepared, as transition film;
(2) described organic film is floated in water, successively a year net, filter paper are layed on described organic film, obtain year net being covered with organic film;
(3) adopt magnetron sputtering method or thermal evaporation, what be covered with organic film described in obtaining in step (2) carries the amorphous alloy film that deposited thereon a layer thickness is 5-18 nm, obtains year net after sputtering;
(4) the described post-depositional year net that step (3) obtains is soaked in acetone soln, dissolve organic film substrate, then rinsing in the distilled water of cleaning, net will be carried and pull out, dry, for subsequent use, namely obtained described transmission electron microscope NiTi non-crystaline amorphous metal carries net supporting film.
Further, the magnificent film in the described organic film side of being or collodion membrane.
Further, described year net is the one of copper mesh, nickel screen, molybdenum net or 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 heat.
Further, described in step (3), the condition of thermal evaporation is: the nitinol alloy wire choosing 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 simultaneously the good conductor of electricity and heat, is widely used in medicine equipment etc.Present Nitinol has defined industry in large scale, is that a kind of being very easy to obtains alloy material.Carry a net supporting film with nickel-titanium alloy material preparation, the super-elasticity of marmem, high mechanical properties and excellent conductivity can be made full use of, solve the low and charged serious problem of mechanical strength that carbon supporting film exists.
The atomic structure of carbon supporting film is non crystalline structure, has isotropism, can not have an impact to the contrast of sample to be seen.So in order to ensure that the atomic structure that Nitinol carries net supporting film has isotropism, the present invention adopts the method for magnetron sputtering carrying deposited thereon one deck amorphous nickel-titanium alloy film.In order to guarantee to obtain amorphous alloy film, therefore adopting Nitinol target, according to elemental metals target, then can only obtain polycrystal film, there is crystal grain because of it and not there is isotropic, thus interference can be produced to the contrast of sample to be seen.
Owing to being amorphous alloy film, so in transmission electron microscope, the diffraction ring of non-crystaline amorphous metal is still typical amorphous ring, can be used for judging 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-irradiation zone of surrounding rapidly from irradiation zone conduction, so that whole amorphous alloy film, thus greatly can weaken the charge accumulated phenomenon of electron beam irradiation region generation.
the present invention's beneficial effect is compared to existing technology:
1, NiTi non-crystaline amorphous metal of the present invention carries net supporting film, utilize conductivity and the super-elasticity of marmem, greatly can weaken the charged phenomenon of transmission electron microscope carrier net supporting film, the mechanical strength of supporting film can be improved, be not easy breakage, remain the non crystalline structure of supporting film simultaneously, do not change the use habit using the magnificent film in tradition side, collodion membrane and carbon supporting film to be formed;
2, NiTi non-crystaline amorphous metal of the present invention carries in the preparation method of net supporting film, and deposition process is selected and adopted magnetron sputtering method and thermal evaporation.Adopt control sputtering method can realize large-scale mass production, stable performance, be convenient to state modulator; Adopt thermal evaporation also can realize batch production, stable performance, state modulator needs rule of thumb, advantage is that equipment is cheap, and volume is little, can use same evaporation equipment with carbon supporting film, do not need to add new equipment, greatly can save equipment cost, more economical.
Accompanying drawing explanation
Fig. 1 is the Performance comparision schematic diagram that carbon supporting film and NiTi non-crystaline amorphous metal carry net supporting film.
Embodiment
embodiment 1
A kind of transmission electron microscope NiTi non-crystaline amorphous metal carries net supporting film, and described NiTi non-crystaline amorphous metal carries bottom-up being followed successively by of net supporting film and carries net and amorphous alloy thin rete, containing nickel element and titanium elements in described amorphous alloy thin rete.
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 thin rete is 5-18 nm.
Described transmission electron microscope NiTi non-crystaline amorphous metal carries the preparation method of net supporting film, comprises the following steps:
(1) organic film is prepared, as transition film;
(2) described organic film is floated in water, successively a year net, filter paper are laid on described organic film, obtain year net being covered with organic film;
(3) adopt magnetron sputtering method or hot steaming method, what be covered with organic film described in obtaining in step (2) carries the amorphous alloy film that deposited thereon a layer thickness is 5-18 nm, obtains year net after sputtering;
(4) the described post-depositional year net that step (3) obtains is soaked in acetone soln, dissolve organic film substrate, then rinsing in the distilled water of cleaning, net will be carried and pull out, dry, for subsequent use, namely obtained described transmission electron microscope NiTi non-crystaline amorphous metal carries net supporting film.
Further, the magnificent film in the described organic film side of being or collodion membrane.
Further, described year net is the one of copper mesh, nickel screen, molybdenum net or 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 heat.
Further, described in step (3), the condition of thermal evaporation is: the nitinol alloy wire choosing 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 embodiment 1 basis, wherein the magnificent film in the organic film side of selecting, and the preparation method that described NiTi non-crystaline amorphous metal gold carries net supporting film comprises the following steps:
(1) compound concentration is the magnificent powder solution in side of 0.5%, by magnificent for the slide insertion side of cleaning powder solution, leave standstill 10 s, from solution, propose slide, in culture dish holding, dry, by the surrounding of film on blade scribing slide, tilt to insert in clean distilled water by slide, namely the magnificent film in side comes off from slide, swims in distilled water surface.
(2) year net acetone ultrasonic cleaning 5 min of supporting film will be there is no, 2 times are cleaned again with clean distilled water, pull out, dry, one by one on the magnificent film in the side of being laid in, cutting and the onesize filter paper of membrane area, be layered on and carry on net, after filter paper is flooded profit completely, carry net and the side magnificent film of filter paper together with absorption is pulled out from distilled water, dry in the cultivation face of being placed on, what namely obtain the magnificent film in the side of being covered with carries net.
(3) the Nitinol target customizing 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) net that carries of magnificent for 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 slide, put into magnetic control sputtering device, be evacuated to 2*10
-4pa, adopt direct current sputtering, power 43 W, film deposition rate is 0.2 nm/s, and sedimentation time is 30-90 s, is preferably 50 s, namely obtains the nickel-titanium alloy film of thickness about 5-18 nm.In deposition process, substrate does not heat.
(5) net that carries after sputtering is soaked 1 min, the magnificent film substrate in the side of dissolving, rinsing in the distilled water of cleaning in acetone soln, rinsing 3 times, will carry net and pull out, dry, for subsequent use, and namely obtained described NiTi non-crystaline amorphous metal carries net supporting film.
Fig. 1 is the Performance comparision that carbon supporting film and NiTi non-crystaline amorphous metal carry net supporting film.Fig. 1 (a) is carbon supporting film X rays topographs and at 450 pA/cm
2the result of chronic exposure 4 min under electron beam intensity, can see gem-pure black irradiation ring.The ring of black is because 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 carries net supporting film X rays topographs and at 500 pA/cm
2the result of chronic exposure 8 min under electron beam intensity, can see simple black irradiation ring, shows that the degree of charge accumulated is much smaller than carbon supporting film, and then illustrates that conductivity that NiTi non-crystaline amorphous metal carries net supporting film is obviously better than the conductivity of carbon supporting film.Fig. 1 (c) and Fig. 1 (d) is the electron diffraction pattern that carbon supporting film and NiTi non-crystaline amorphous metal carry net supporting film respectively, both are typical amorphous dispersion ring, showing that NiTi non-crystaline amorphous metal carries net supporting film is amorphous material, has isotropism.
embodiment 3
The present embodiment is the preferred version on embodiment 1 basis, and wherein organic film selects collodion membrane, and the preparation method that described NiTi non-crystaline amorphous metal gold carries net supporting film comprises the following steps:
(1) solvent is made with pentyl acetate, the collodion solution of preparation 2%;
(2) drip collodion solution on clean distilled water surface with glass dropper, the collodion membrane of the water surface, rapidly in water surface extension film forming, with the lens wiping paper of cleaning, is plunderred, with the clean water surface by collodion solution;
(3) drip collodion solution again on distilled water surface, collodion solution is rapidly in water surface extension film forming;
(4) being immersed in 5 min in clean acetone by carrying net, to clean the organic substance carrying net surface, then using clean distilled water rinsing 3 times, obtain cleaned year net;
(5) the cleaned net that carries is layered on collodion membrane one by one, lines up array;
(6) filter paper of cutting one piece of suitable size, is layered on and carries on the net, after filter paper complete wetting, is taken out by filter paper, dry together with year net and collodion membrane from the water surface, namely prepares year net being covered with collodion membrane;
(7) the Nitinol target customizing 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) net that carries 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 slide, put into magnetic control sputtering device, be evacuated to 2*10
-4pa, adopt direct current sputtering, power 43 W, film deposition rate is 0.2 nm/s, and sedimentation time is 30-90 s, is preferably 50 s, namely obtains the nickel-titanium alloy film of thickness about 5-18 nm.In deposition process, substrate does not heat.
(9) net that carries after sputtering is soaked 1 min in acetone soln, dissolve collodion membrane substrate, rinsing in the distilled water of cleaning, rinsing 3 times, will carry net and pull out, and dry, for subsequent use, the NiTi non-crystaline amorphous metal described in namely obtaining carries net supporting film.
embodiment 4
The present embodiment is the preferred version on embodiment 1 basis, wherein the magnificent film in the organic film side of selecting, and the preparation method that described NiTi non-crystaline amorphous metal gold carries net supporting film comprises the following steps:
(1) compound concentration is the magnificent powder solution in side of 0.5%, by magnificent for the slide insertion side of cleaning powder solution, leave standstill 10 seconds, from solution, propose slide, in culture dish holding, dry, by the surrounding of film on blade scribing slide, tilt to insert in clean distilled water by slide, namely the magnificent film in side comes off from slide, swims in distilled water surface.
(2) year net acetone ultrasonic cleaning 5 min of supporting film will be there is no, 2 times are cleaned again with clean distilled water, pull out, dry, one by one on the magnificent film in the side of being laid in, cutting and the onesize filter paper of membrane area, be layered on and carry on net, after filter paper is flooded profit completely, carry net and the side magnificent film of filter paper together with absorption is pulled out from distilled water, dry in the cultivation face of being placed on, what namely obtain the magnificent film in the side of being covered with carries net.
(3) net that carries of magnificent for 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 slide, put into thermal evaporation plated film instrument, choose the nitinol alloy wire of diameter 0.3-0.7 mm, be 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.%.Getting nitinol alloy wire described in 1-2 cm hangs in tungsten filament evaporating basket, is evacuated to 2*10
-4pa, film deposition rate is 0.2 nm/s, and sedimentation time is 30-90 s, is preferably 50 s, namely obtains through post-depositional year net.
(4) post-depositional year net is soaked 1 min in acetone soln, the magnificent film substrate in the side of dissolving, rinsing in the distilled water of cleaning, rinsing 3 times, net will be carried and pull out, and dry, for subsequent use, namely obtained described NiTi non-crystaline amorphous metal carries net supporting film.
Claims (9)
1. transmission electron microscope NiTi non-crystaline amorphous metal carries a net supporting film, it is characterized in that, described NiTi non-crystaline amorphous metal carries bottom-up being followed successively by of net supporting film and carries net and amorphous alloy thin rete, containing nickel element and titanium elements in described amorphous alloy thin rete.
2. transmission electron microscope NiTi non-crystaline amorphous metal according to claim 1 carries net supporting film, it is characterized in that, content 40-60 at.% of described nickel element, and the content of described titanium elements is 60-40 at.%.
3. transmission electron microscope NiTi non-crystaline amorphous metal according to claim 2 carries net supporting film, it is characterized in that, described NiTi optimum ratio is 50: 50 at.%.
4. transmission electron microscope NiTi non-crystaline amorphous metal according to claim 1 carries net supporting film, it is characterized in that, the thickness of described amorphous alloy thin rete is 5-18 nm.
5. the transmission electron microscope NiTi non-crystaline amorphous metal as described in any one of claim 1-4 carries a preparation method for net supporting film, and it is characterized in that, described preparation method comprises the following steps:
(1) organic film is prepared, as transition film;
(2) described organic film is floated in water, successively a year net, filter paper are layed on described organic film, obtain year net being covered with organic film;
(3) adopt magnetron sputtering method or thermal evaporation, what be covered with organic film described in obtaining in step (2) carries the amorphous alloy film that deposited thereon a layer thickness is 5-18 nm, obtains year net after sputtering;
(4) the described post-depositional year net that step (3) obtains is soaked in acetone soln, dissolve organic film substrate, then rinsing in the distilled water of cleaning, net will be carried and pull out, dry, for subsequent use, namely obtained described transmission electron microscope NiTi non-crystaline amorphous metal carries net supporting film.
6. transmission electron microscope NiTi non-crystaline amorphous metal according to claim 5 carries the preparation method of net supporting film, it is characterized in that, the magnificent film in the described organic film side of being or collodion membrane.
7. transmission electron microscope NiTi non-crystaline amorphous metal according to claim 5 carries the preparation method of net supporting film, it is characterized in that, described year net is the one of copper mesh, nickel screen, molybdenum net or Jin Wangzhong.
8. transmission electron microscope NiTi non-crystaline amorphous metal according to claim 5 carries the preparation method of net supporting film, it is characterized in that, described in step (3), the condition of magnetron sputtering method is: select Nitinol target to be 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 heat.
9. transmission electron microscope NiTi non-crystaline amorphous metal according to claim 5 carries the preparation method of net supporting film, it is characterized in that, described in step (3), the condition of thermal evaporation is: the nitinol alloy wire choosing 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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| CN111816538A (en) * | 2020-07-17 | 2020-10-23 | 兰州大学 | Transmission electron microscope micro-grid based on heavy ion irradiation and preparation method |
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| CN108660426A (en) * | 2018-04-12 | 2018-10-16 | 中国科学院生物物理研究所 | A kind of NiTi non-crystaline amorphous metal microarray supports the preparation method of film |
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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 |
| CN111816538A (en) * | 2020-07-17 | 2020-10-23 | 兰州大学 | Transmission electron microscope micro-grid based on heavy ion irradiation and preparation method |
| CN111816538B (en) * | 2020-07-17 | 2022-03-25 | 兰州大学 | Transmission electron microscope micro-grid based on heavy ion irradiation and preparation method |
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