CN101545872B - Low-dimensional nano material microstructure and device and method for electrical performance testing - Google Patents
Low-dimensional nano material microstructure and device and method for electrical performance testing Download PDFInfo
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- CN101545872B CN101545872B CN2009100842600A CN200910084260A CN101545872B CN 101545872 B CN101545872 B CN 101545872B CN 2009100842600 A CN2009100842600 A CN 2009100842600A CN 200910084260 A CN200910084260 A CN 200910084260A CN 101545872 B CN101545872 B CN 101545872B
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Abstract
The invention relates to a low-dimensional nano material microstructure and a device and a method for electrical performance testing. The device is characterized in that an amorphous layer is positioned above a substrate, a blocking layer is positioned under the substrate, the middle parts of the blocking layer and the substrate are etched to form a window, metal electrodes are on the amorphous layer, and a low-dimensional nano material is between the metal electrodes, is positioned on the amorphous layer opposite to the right upper part of the window, and is made into an amorphous blocking layer; and conducting wires are led out of the metal electrodes. The invention provides a method for transferring and fixing the low-dimensional nano material, which can simultaneously carry out power turn-on measurement for the low-dimensional nano material, and can measure the correlation of the microstructure and the electrical performance of the low-dimensional nano material in situ under atom lattice resolution.
Description
Technical field:
The present invention relates to the proving installation and the method for a kind of low-dimensional nano material microstructure and electric property, original position real-time and dynamic low-dimensional nano material microstructure-electricity transports the measurement mechanism and the method for performance coherence under more particularly a kind of "on" position.
Background technology:
Transmission electron microscope is one of powerful tool the most in nano science and technical field.The specimen holder of transmission electron microscope is used for supporting sample to be detected.Low-dimension nano material is carrying information transmission as the basic structural unit of device, critical functions such as storage.The low-dimension nano material that in semiconductor and information industry, is applied to; Under the effect in outfield; Study its microstructural variation and size effect to Effect on Performance such as low-dimension nano material charge transport abilities in the device cell, the practical applications such as density of this sensitivity to device, efficient, storage unit have very important significance.And at present; Existing technological means can only be carried out static observation to sample in transmission electron microscope; Obtain low-dimensional nano material microstructure information; And the measurement of in ESEM, switching in situ, but can not obtain the information of low-dimensional nano material microstructure aspect, the measurement of low-dimensional nano material microstructure and electric property is difficult to accomplish under the "on" position.
Summary of the invention:
To the problem that prior art exists, the purpose of this invention is to provide a kind of in transmission electron microscope the apparatus and method of in site measurement low-dimensional nano material microstructure and electric property under the "on" position.Make the device that carries low-dimension nano material earlier; Then low-dimension nano material is fabricated on this device; To the energising of this device, microstructure and the electricity of measuring low-dimension nano material transport performance, the variation of real time record low-dimension nano material microstructure and electric property in the sample for use in transmitted electron microscope bar.By the change procedure of transmission electron microscope imaging system original position record low-dimension nano material, transport the correlativity of performance and microstructure change from the electricity of atomic scale announcement low-dimension nano material.
In order to realize top purpose, be to realize through following technical scheme:
The invention provides a kind of low-dimensional nano material microstructure and electrical performance testing device, it is characterized in that:
It above substrate amorphous layer; The below is the restraining barrier, and the center section of restraining barrier and substrate is etched away the formation window, is metal electrode on amorphous layer; It between the metal electrode low-dimension nano material; Low-dimension nano material is positioned on the amorphous layer facing to directly over the window, is the amorphous restraining barrier on the low-dimension nano material, draws lead on the metal electrode.
Prepare said a kind of low-dimensional nano material microstructure and electrical performance testing device, it is characterized in that, may further comprise the steps:
1. making substrate, substrate top growth thin film are as the amorphous layer that can let electron beam penetrate, and the film of substrate below growth one deck is as the restraining barrier; The double-sided overlay substrate: the amorphous layer gluing, photoetching forms electrode pattern, and the plating layer of metal is removed photoresist as metal electrode on electrode pattern; The restraining barrier gluing, photoetching forms pattern of windows, and the corrosive liquid of a usefulness corrosion barrier layer removes photoresist after eroding the restraining barrier in the window;
2. spin coating one deck photoresist on amorphous layer; The single face cover carves the shape pattern of low-dimension nano material on amorphous layer, and this pattern is created between the metal electrode, growth one deck low-dimension nano material on photoresist; Form low-dimension nano material after removing photoresist; Growth amorphous restraining barrier on low-dimension nano material again, gluing on the amorphous restraining barrier erodes the amorphous restraining barrier on the metal electrode with the corrosive liquid that only corrodes the amorphous restraining barrier after the photoetching;
3. put into the corrosive liquid that only corrodes substrate, the center section that corrodes substrate forms final window afterwards, cleans the impurity on surface;
4. metal electrode is drawn with lead, be connected on the sample for use in transmitted electron microscope bar, insert in the transmission electron microscope.
The present invention has following advantage:
1. the present invention has carried out special structure design to the device that carries low-dimension nano material in the transmission electron microscope, is implemented in the transmission electron microscope in situ low-dimension nano material to be powered up, from the zone axis observation full resolution pricture of the best; Realize X; Verting of Y both direction maximum angle provides a kind of low-dimension nano material original position electrical performance test method, has dependable performance; Easy for installation, characteristic of simple structure.
2. the present invention is applied to the electric property research of low-dimension nano material, applied range, and research object is abundant.For the low-dimension nano material made from photoetching process, can carry out the home position observation monitoring of electric property to it through this kind method.
3. the invention provides a kind of transfer, the fixing method of low-dimension nano material, can be simultaneously to the low-dimension nano material measurement of switching on, can under atom lattice resolution, measure the microstructure of low-dimension nano material and the correlativity of electric property in situ.
Description of drawings
Fig. 1 TEM micro grid device front view
The upward view of Fig. 2 Fig. 1
The vertical view of Fig. 3 Fig. 1
Fig. 4,5,6 nano material live widths are respectively the voltage-current curve of 0.07,0.15,0.2 μ m
Fig. 7,8,9 nano material live widths are respectively the microstructure change of 0.07,0.15,0.2 μ m
1, restraining barrier; 2, substrate; 3, amorphous layer; 4, metal electrode; 5, photoetching alignment mark; 6, window; 7, low-dimension nano material; 8, amorphous restraining barrier; 9, lead
Embodiment:
The present invention carries out original position energising test through to the device energising to low-dimension nano material, implements through following steps:
Concrete, the device that carries low-dimension nano material is followed successively by from top to bottom: use SiO
2As restraining barrier 1, silicon chip is as substrate 2, and SiN is as amorphous layer 3, and what on amorphous layer 3, use is that gold is as metal electrode 4 and photoetching alignment mark 5, SiO
2What restraining barrier and silicon chip were etched formation is window 6, uses the GeSbTe phase-change material as low-dimension nano material 7 between the gold electrode, and the GeSbTe phase-change material is directly over window 6, and what use on the GeSbTe phase-change material is that SiN is as amorphous restraining barrier 8.
Use the method for testing that said apparatus carries out low-dimensional nano material microstructure and electric property under the "on" position, it is characterized in that may further comprise the steps:
1. make the substrate 2 of 100-500 μ m, the top grow a layer thickness at the film of 0.03-0.3 μ m as the amorphous layer 3 that can let electron beam penetrate, the film of below growth one deck 0.05-0.5 μ m is as etching barrier layer 1.The double-sided overlay substrate: amorphous layer 3 gluings, photoetching forms electrode pattern, and the plating layer of metal is removed photoresist as metal electrode 4 on electrode pattern; Restraining barrier 1 gluing, photoetching forms pattern of windows, erodes the restraining barrier in the window, a corrosive liquid corrosion barrier layer, remove photoresist afterwards in the restraining barrier that corrodes in the window.
2. spin coating one deck photoresist on amorphous layer 3; On amorphous layer, carve the shape pattern of low-dimension nano material according to photoetching alignment mark 5 single face covers; This pattern is created between the metal electrode 4, and growth one deck low-dimension nano material forms low-dimension nano material 7 after removing photoresist on photoresist; Again on low-dimension nano material growth one layer thickness on the amorphous restraining barrier 8 of 0.03-0.3 μ m; Gluing on amorphous restraining barrier 8, photoetching post-etching fall the amorphous restraining barrier 8 on the metal electrode, and corrosive liquid only corrodes amorphous restraining barrier 8.
3. put into the corrosive liquid that only corrodes substrate 2, form window 6 after etching, take out the impurity that sample is cleaned the surface.
4. metal electrode 4 usefulness leads 9 are drawn, be connected on the sample for use in transmitted electron microscope bar, insert in the transmission electron microscope.
The method of making and testing is specially: through the method growth SiO of PECVD (plasma chemical vapor deposition)
2, its thickness is 0.5 μ m; Silicon wafer thickness is 200 μ m, and diameter is 2 inches, the heavy doping of P type, and resistivity is 5 Ω .cm, through twin polishing, the crystal orientation does<100>Through the method growth SiN of PECVD, its thickness is 0.1 μ m.Make two 2.5 inches mask blanks that are used for double-sided overlay, elder generation's gluing above silicon chip, photoetching forms the electrode pattern of top; Plate one deck gold electrode above that, remove photoresist, again gluing below silicon chip; Photoetching is formed for the window of etching, falls the SiO in the window with rare HF solution corrosion
2, remove photoresist.Spin coating one deck photoresist PMMA (polymethylmethacrylate) above bogey; The single face cover carves low dimension lines, and the width of lines is from 0.02 μ m-2 μ m, and the two ends of lines are connected on the gold electrode; The thick GeSbTe phase-change material of sputter one deck 0.05 μ m up; Substrate is put into the acetone ultrasonic cleaning, obtain the GeSbTe lines of different live widths, again the low temperature PECVD SiN layer of a layer thickness of growing up at 0.2 μ m.Make the mask blank of 2.5 inches of a slices again, gluing on the SiN layer, photoetching is formed for the window of etching, is etched away the SiN on the metal electrode with ICP (inductively coupled plasma), removes photoresist.
Ready-made silicon chip is cut into the little grid of square of 2.15*2.15mm, put into the EDP corrosive liquid, the temperature of solution is controlled at 80-100 ℃, through more than 3 hours etching, takes out sample and in acetone, cleans more than three times.Under light microscopic, gold electrode is drawn with Herba Anoectochili roxburghii, again Herba Anoectochili roxburghii is welded on the sample for use in transmitted electron microscope bar that has the energising function with press welder.
Device is carried out original position energising, and the micromechanism of GeSbTe phase-change material changes, and through high-resolution original position imaging system record whole variation process, measures the correlativity that microstructure and the electricity of low-dimension nano material under "on" position transports performance.
Experimental result: on-load voltage in transmission electron microscope; The scope that voltage loads is in the interval of 0-25V; Having measured length is the GeSbTe lines of three kinds of different live widths of 0.7 μ m, and line thickness is from being respectively 0.07,0.15,0.2 μ m, following Fig. 4 of voltage-current curve, 5, shown in 6:
Corresponding microstructure change is like Fig. 7,8, shown in 9, and in the process that voltage raises, the microstructure in the GST phase transformation lines takes place by following the variation, and this is a process that has amorphous to arrive crystallization.
Claims (1)
1. the preparation method of low-dimensional nano material microstructure and electrical performance testing device, this apparatus structure is following:
It above substrate amorphous layer; The below is the restraining barrier, and the center section of restraining barrier and substrate is etched away the formation window, is metal electrode on amorphous layer; It between the metal electrode low-dimension nano material; Low-dimension nano material is positioned on the amorphous layer facing to directly over the window, is the amorphous restraining barrier on the low-dimension nano material, draws lead on the metal electrode;
It is characterized in that, may further comprise the steps:
1) make substrate, growth thin film in substrate top is as the amorphous layer that can let electron beam penetrate, and the film of substrate below growth one deck is as the restraining barrier; The double-sided overlay substrate: the amorphous layer gluing, photoetching forms electrode pattern, and the plating layer of metal is removed photoresist as metal electrode on electrode pattern; The restraining barrier gluing, photoetching forms pattern of windows, and the corrosive liquid of a usefulness corrosion barrier layer removes photoresist after eroding the restraining barrier in the window;
2) spin coating one deck photoresist on amorphous layer; The single face cover carves the shape pattern of low-dimension nano material on amorphous layer, and this pattern is created between the metal electrode, growth one deck low-dimension nano material on photoresist; Form low-dimension nano material after removing photoresist; Growth amorphous restraining barrier on low-dimension nano material again, gluing on the amorphous restraining barrier erodes the amorphous restraining barrier on the metal electrode with the corrosive liquid that only corrodes the amorphous restraining barrier after the photoetching;
3) put into the corrosive liquid that only corrodes substrate, the center section that corrodes substrate forms final window afterwards, cleans the impurity on surface;
4) metal electrode is drawn with lead, be connected on the sample for use in transmitted electron microscope bar, insert in the transmission electron microscope.
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