CN103112818B - Method of manufacturing metal electrodes on single micro-nano line by utilizing scanning electron microscope - Google Patents
Method of manufacturing metal electrodes on single micro-nano line by utilizing scanning electron microscope Download PDFInfo
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Abstract
The invention discloses a method of manufacturing metal electrodes on a single micro-nano line by utilizing a scanning electron microscope, and belongs to the field design and manufacture of micro-nano devices. According to the method, the metal electrodes are manufactured at the two ends of the single micro-nano line by virtue of the simple scanning electron microscope and a film coater; the electrodes cover the micro-nano line and are in stable electrode contact with the micro-nano line, so that the signal stability in an electrical property measuring process is guaranteed; and the metal utilized as the electrode has multiple options so as to provide a technical support for designing and building multi-form micro-nano devices. In a manufacturing process, expensive equipment such as an FIB is not used, the effect of the manufacturing the same electrode is achieved, the cost is saved, and the method is simple and is easy to operate.
Description
Technical field
The present invention relates to a kind of method utilizing ESEM to make metal electrode in single micro-nano line, belong to micro-nano device design and manufacture field.
Background technology
Realizing the good contact between single micro-nano line and metal electrode, is study the electrical property of single micro-nano line all the time and utilize the crucial matter of science and technology of bottleneck of single micro-nano line structure micro-nano device.Single micro-nano line is as the basic functional units in minute mechanical and electrical system, and it is the basis giving full play to single micro-nano line power photoelectric properties that surface interface good between material with electrode contacts, and is the prerequisite of design novel micro nanometer device.For nano-ZnO, the contact solving single ZnO micro-nano line and metal electrode at present roughly can be divided into following four kinds of approach.
The first, the metal microelectrode of well in advance sprinkles ZnO micro-nano line at random, relies on the Van der Waals adsorption power between ZnO micro-nano line and electrode to realize electrode contact.2002, " Advanced Materials ", vol.14, " ultraviolet light detector that single nano-wire builds and photoswitch " on 158-160 reports in (Nanowire ultraviolet photodetectors and optical switches) literary composition to utilize and is sprinkled upon contacting of ZnO nano-wire and Au electrode on metal A u electrode, measures the ultraviolet response performance of single ZnO nano-wire.Equally also be on Au electrode, 2006, " Nano Letters ", the diode making single ZnO nano-band/nano wire two ends form Schottky contacts respectively with ready-made Au electrode to form with electrophoresis method is reported in " building ZnO nano-band/nano wire Schottky diode by electrophoresis between Au electrode " (ZnO nanobelt/nanowire Schottky diodes formed by dielectrophoresis alignment across Au electrodes) article on vol.6,263-266.
The second, utilize electron-beam exposure system (EBL) to make metal electrode at single ZnO nano-wire two ends.2007, " Physics Letters A ", vol. 367, report in " surface state is on the impact of single ZnO nano-wire electronic transport performance " (Effect of surface states on electron transport in individual ZnO nanowires) literary composition on 207-210 and on single ZnO nano-wire, make metal electrode with EBL, research surface state is on the impact of single ZnO nano-wire electronic transport performance.
3rd, utilize focused ion beam equipment (FIB) deposit metal electrodes in single ZnO micro-nano line.2006, " Nano Letters ", vol.6, report in " single ZnO nano-wire build wide-band light emitting diode " (Broadband ZnO single-nanowire light-emitting diode) literary composition on 1719-1722 with FIB depositing Ti/Au electrode on single ZnO nano-wire, and make single ZnO nano-wire and P-type silicon form pn to bind up one's hair optical diode.
4th, utilize nanometer manipulation metal probe and single ZnO micro-nano line to form electrode contact.2010, " Applied Physics Letters ", vol.96, form loop by nanometer manipulation metal W probe and ZnO nano-wire two end in contact in the electroluminescent damage of ZnO nano-wire " in the metal-semiconductor-metal " (Electrical breakdown of ZnO nanowires in metal-semiconductor-metal structure) literary composition on 253112, have studied electroluminescent damage phenomenon and the mechanism of ZnO nano-wire.
Although single micro-nano line can be formed with metal electrode and contact in the first approach, because this Van der Waals adsorption power is in fact very little, contact is easy to loosen.The electron-beam exposure system that the second approach uses needs on the basis of plain scan Electronic Speculum, install electron beam control system additional.And the third approach needs to use expensive FIB equipment, as huge in wanted lot of experiments then to spend, a lot of laboratory does not possess such condition.In 4th kind of approach, the contact point of nanometer manipulation probe and single micro-nano line is not fixed, and easily slides, can affect the Measurement accuracy of electrical property.
Summary of the invention
In order to solve the problem, the object of this invention is to provide a kind of stability that can ensure signal in electrical property measuring process, and when not using the expensive device such as FIB, reach the effect making same electrode, cost-saving, the simple and easy to do ESEM that utilizes makes the method for metal electrode in single micro-nano line.
Technical scheme of the present invention is, a kind of method utilizing ESEM to make metal electrode in single micro-nano line, specifically comprises the following steps:
A. spin coating polymetylmethacrylate electron beam lithography glue on silicon-on-insulator substrate, and the solid film of baking;
B. electron beam lithography: the silicon-on-insulator after above-mentioned steps process is placed in ESEM, adjustment Electronic Speculum multiplication factor, make electron beam irradiation sub-fraction PMMA, irradiated area is equal to Electronic Speculum display picture and represents area;
C. developing fixing: use developer solution and fixing solution to wash away the PMMA degraded by electron beam irradiation;
D. d.c. sputtering: the silicon-on-insulator after step c process is put into d.c. sputtering instrument, carries out the d.c. sputtering of metal, forming thickness is the metallic film of 100nm;
E. remaining glue is peeled off: to be steeped respectively by the silicon-on-insulator after steps d process in acetone, ethanol, isopropyl alcohol each ultrasonic 60 seconds, still unexposed PMMA is removed and cleaned up, finally on silicon-on-insulator substrate, obtains the mark that material is splash-proofing sputtering metal;
F. micro-nano line is dispersed in aqueous isopropanol, and be added drop-wise on the silicon-on-insulator substrate after step e process, in ESEM, read and record the absolute position of metal marker, and record the absolute position at precompose metal electrode place in micro-nano line, calculate precompose metal electrode place to the relative coordinate position (X1, Y1) of metal marker and (X2, Y2);
G. step a process is repeated at the silicon-on-insulator after step f process;
H. the silicon-on-insulator after step g process is placed in ESEM, focus in ESEM and aim at metal marker, and record the absolute position of now metal marker, according to precompose metal electrode place to the relative position of metal marker, calculate the absolute position at now precompose metal electrode place, utilize electron microscopic sample platform to move to immediately below electron beam by the absolute position at precompose metal electrode place;
I. repeat step b electron beam lithography, c developing fixing, d d.c. sputtering and e and peel off remaining glue four steps, finally obtain the required metal electrode covered in one dimension micro-nano line.
Further, in described step a, the percentage concentration of methyl methacrylate is 0.01; With the rotating speed of 4000rpm, spin coating 30s, then in an oven 160 DEG C baking two hours with solid film.
Further, described step b is in ESEM, will speed up voltage and be transferred to 20kV, make Electron Beam Focusing to silicon-on-insulator surface, be transferred to suitable multiplication factor, in this experiment, multiplication factor be transferred to 10000 times, make electron beam irradiation sub-fraction PMMA, irradiated area is equal to Electronic Speculum display picture and represents area, and exposure time is 120 seconds.
Further, in described step c developer solution be use methylisobutylketone MIBK and isopropyl alcohol IPA with 1: 3 ratio be deployed into; Described fixing solution is isopropyl alcohol IPA, and developing time is 75 seconds, and fixing time is 20 seconds.
Further, described micro-nano rice noodles are ZnO, TiO
2or CNT; The metal of described d.c. sputtering can form the metal of Schottky contacts with micro-nano line or can form the metal of Ohmic contact with micro-nano line.
The method utilizing ESEM to make metal electrode in single micro-nano line provided by the invention, can realize single micro-nano line fixing on substrate, can provide well stable electrode contact, can make micro-nano device for the electrical property characterizing single micro-nano line.
The present invention compared with prior art, has the following advantages and outstanding effect: electrode covers above micro-nano line, can form firm electrode contact, ensure that the stability of signal in electrical property measuring process with micro-nano line.Metal as electrode can have multiple choices, for ZnO, both can be can form the Pt metal, Au etc. of Schottky contacts with ZnO micro-nano line, also can be can form metal A g, the Ta etc. of Ohmic contact, for the micro-nano device of design construction various ways provides technical support with ZnO micro-nano line.Making the process of electrode and only used ESEM the most general and the common equipment of the plated film instrument two kind supporting with ESEM, when not using the expensive device such as FIB, reaching the effect making same electrode, cost-saving, simple and easy to do.
Accompanying drawing explanation
ESEM (SEM) figure that Fig. 1 (a) is metal marker, (b) is for utilizing the method schematic diagram of metal marker keeper electrode position.
Fig. 2 (a) ~ (d) is process flow diagram.
Fig. 3 is the SEM figure of the two ends metal electrode of single micro-nano line and making.
In figure:
1. silicon-on-insulator, 2. methyl methacrylate PMMA, 3. micro-nano line, 4. metal electrode, 5. metal marker.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme of the present invention is described further.
Embodiment 1:
1. spin coating polymethyl methacrylate (PMMA) the electron beam lithography glue also solid film of baking, silicon-on-insulator 1 drips the PMMA positron beam etching glue 2 that percentage concentration is 0.01, with the rotating speed of 4000rpm, spin coating 30s, then in an oven with temperature 160 DEG C baking two hours, solvent in PMMA is volatilized, described silicon-on-insulator 1 is formed one deck PMMA glued membrane 2;
2. electron beam lithography.Described silicon-on-insulator 1 is placed in ESEM, will speed up voltage and be transferred to 20kV, make Electron Beam Focusing to silicon-on-insulator surface, Electronic Speculum multiplication factor is transferred to suitable multiple, as multiplication factor being transferred to 10000 times in this experiment, make the PMMA in electron beam irradiation Electronic Speculum display picture, exposure time is 120 seconds;
3. development and fixing.Use methylisobutylketone (MIBK) and isopropyl alcohol (IPA) with 1: 3 ratio be deployed into developer solution, fixing solution is made with IPA, at the temperature of constant temperature 25 DEG C, described silicon-on-insulator is soaked 75 seconds in developer solution, put into fixing solution about 20s again, dried up by residual IPA fixing solution after taking-up, namely the glued membrane at the position that is etched is washed away again;
4. d.c. sputtering metallic film.Described silicon-on-insulator is put into plated film instrument, and the Pt metallic film required for d.c. sputtering is to 100nm;
5. peel off residue glued membrane.Described silicon-on-insulator to be steeped respectively in acetone, ethanol, isopropyl alcohol each ultrasonic 60 seconds, still unexposed PMMA is removed and cleans up, finally on described silicon-on-insulator substrate, obtains the mark 5 that material is Pt metal, as shown in Fig. 1 (a);
6. micro-nano line (3) is dispersed in isopropyl alcohol, and be added drop-wise on described silicon-on-insulator substrate, described silicon-on-insulator is placed in ESEM, read and record the absolute coordinate position that Pt marks 5, and record the absolute coordinate position at precompose metal electrode 4 place in micro-nano line 3, calculate precompose metal electrode 4 place to the relative coordinate position (X1, Y1) of Pt metal mark (5) and (X2, Y2), as shown in Fig. 1 (b);
7. on described silicon-on-insulator 1, spin coating PMMA glue 2 also consolidates film, repeats step 1, as shown in Fig. 2 (a);
8. in ESEM, focus on the Pt metal mark 5 aimed on described silicon-on-insulator, and record the absolute coordinate position of now Pt metal mark 5, according to the relative coordinate position (X1 of precompose metal electrode 4 place to Pt metal mark 5, and (X2 Y1), Y2), calculate the absolute position at now precompose metal electrode 4 place, utilize electron microscopic sample platform to move to immediately below electron beam by the absolute coordinate position at precompose metal electrode 4 place;
9. electron beam lithography, repeats step 2;
10. development and fixing, repetition step 3, final gained is as shown in Fig. 2 (b);
11. d.c. sputtering metallic films, repeat step 4, as shown in Fig. 2 (c);
12. peel off residue glued membrane, and repeat step 5, as shown in Figure 2 (d) shows, finally obtain the required metal electrode 4 covered in micro-nano line 3, SEM photo in kind as shown in Figure 3.
Embodiment 2
1. spin coating polymethyl methacrylate (PMMA) the electron beam lithography glue also solid film of baking, drip the PMMA positron beam etching glue that percentage concentration is 0.01 in a silicon-on-insulator, with the rotating speed of 4000rpm, spin coating 30s, then in an oven with temperature 160 DEG C baking two hours, solvent in PMMA is volatilized, described silicon-on-insulator is formed one deck PMMA glued membrane;
2. electron beam lithography.Described silicon-on-insulator is placed in ESEM, will speed up voltage and be transferred to 20kV, make Electron Beam Focusing to silicon-on-insulator surface, Electronic Speculum multiplication factor is transferred to suitable multiple, as multiplication factor being transferred to 10000 times in this experiment, make the PMMA in electron beam irradiation Electronic Speculum display picture, exposure time is 120 seconds;
3. development and fixing.Use methylisobutylketone (MIBK) and isopropyl alcohol (IPA) with 1: 3 ratio be deployed into developer solution, fixing solution is made with IPA, at the temperature of constant temperature 25 DEG C, described silicon-on-insulator is soaked 75 seconds in developer solution, put into fixing solution about 20s again, dried up by residual IPA fixing solution after taking-up, namely the glued membrane at the position that is etched is washed away again;
4. d.c. sputtering metallic film.Described silicon-on-insulator is put into plated film instrument, and the metal A u film required for d.c. sputtering is to the thickness of its 100nm;
5. peel off residue glued membrane.Described silicon-on-insulator to be steeped respectively in acetone, ethanol, isopropyl alcohol each ultrasonic 60 seconds, still unexposed PMMA is removed and cleans up, finally on described silicon-on-insulator substrate, obtains the mark that material is Au;
6. by TiO
2micro-nano line is dispersed in isopropyl alcohol, and is added drop-wise on described silicon-on-insulator substrate, and described silicon-on-insulator is placed in ESEM, reads and records the absolute coordinate position of Au mark, and recording single TiO
2the absolute coordinate position at precompose metal electrode place in micro-nano line, calculates relative coordinate position (X1, Y1) and (X2, Y2) that precompose metal electrode place marks Au;
7. on described silicon-on-insulator, spin coating PMMA glue also consolidates film, repeats step 1;
8. in ESEM, focus on the Au mark aimed on described silicon-on-insulator, and record the absolute coordinate position of now Au mark, according to the relative coordinate position (X1 that precompose metal electrode place marks Au, and (X2 Y1), Y2), calculate the absolute position at now precompose metal electrode place, utilize electron microscopic sample platform to move to immediately below electron beam by the absolute coordinate position at precompose metal electrode place;
9. electron beam lithography, repeats step 2;
10. development and fixing, repetition step 3;
11. d.c. sputtering metallic films, repeat step 4;
12. peel off residue glued membranes, repeat step 5, finally obtain required covering one dimension TiO
2metal electrode in micro-nano line.
Claims (5)
1. utilize ESEM in single micro-nano line, make a method for metal electrode, it is characterized in that:
A. at upper spin coating polymetylmethacrylate electron beam lithography glue (2) of silicon-on-insulator substrate (1), and the solid film of baking;
B. electron beam lithography: the silicon-on-insulator after above-mentioned steps process is placed in ESEM, adjustment Electronic Speculum multiplication factor, make electron beam irradiation sub-fraction PMMA, irradiated area is equal to Electronic Speculum display picture and represents area;
C. developing fixing: use developer solution and fixing solution to wash away the PMMA degraded by electron beam irradiation;
D. d.c. sputtering: the silicon-on-insulator after step c process is put into d.c. sputtering instrument, carries out the d.c. sputtering of metal, forming thickness is the metallic film of 100nm;
E. remaining glue is peeled off: to be steeped respectively by the silicon-on-insulator after steps d process in acetone, ethanol, isopropyl alcohol each ultrasonic 60 seconds, still unexposed PMMA is removed and cleaned up, finally on silicon-on-insulator substrate, obtains the mark that material is splash-proofing sputtering metal;
F. micro-nano line is dispersed in aqueous isopropanol, and be added drop-wise on the silicon-on-insulator substrate after step e process, in ESEM, read and record the absolute position of metal marker, and record the absolute position at the upper precompose metal electrode place of micro-nano line (3), calculate precompose metal electrode place to the relative coordinate position (X1, Y1) of metal marker and (X2, Y2);
G. step a process is repeated at the silicon-on-insulator after step f process;
H. the silicon-on-insulator after step g process is placed in ESEM, focus in ESEM and aim at metal marker, and record the absolute position of now metal marker, according to precompose metal electrode place to the relative position of metal marker, calculate the absolute position at now precompose metal electrode place, utilize electron microscopic sample platform to move to immediately below electron beam by the absolute position at precompose metal electrode place;
I. repeat step b electron beam lithography, c developing fixing, d d.c. sputtering and e and peel off remaining glue four steps, finally obtain the required metal electrode covered in one dimension micro-nano line.
2. method according to claim 1, is characterized in that: in described step a, the percentage concentration of methyl methacrylate is 0.01; With the rotating speed of 4000rpm, spin coating 30s, then in an oven 160 DEG C baking two hours with solid film.
3. method according to claim 1, it is characterized in that: described step b is in ESEM, will speed up voltage and be transferred to 20kV, make Electron Beam Focusing to silicon-on-insulator surface, be transferred to suitable multiplication factor, in this experiment, multiplication factor be transferred to 10000 times, make electron beam irradiation sub-fraction PMMA, irradiated area is equal to Electronic Speculum display picture and represents area, and exposure time is 120 seconds.
4. method according to claim 1, is characterized in that: in described step c developer solution be use methylisobutylketone MIBK and isopropyl alcohol IPA with 1: 3 ratio be deployed into; Described fixing solution is isopropyl alcohol IPA, and developing time is 75 seconds, and fixing time is 20 seconds.
5. method according to claim 1, is characterized in that: described micro-nano rice noodles are ZnO, TiO
2or CNT; The metal of described d.c. sputtering is to form the metal of Schottky contacts with micro-nano line or can form the metal of Ohmic contact with micro-nano line.
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| JP2011119291A (en) * | 2009-10-06 | 2011-06-16 | National Institute For Materials Science | BLUE/ULTRAVIOLET LIGHT DETECTION DEVICE USING SINGLE-CRYSTAL ZnSe NANOBELT, AND METHOD OF MANUFACTURING THE SAME |
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