CN101598645B - Method for manufacturing standard sample for scanning electron microscope magnification calibration - Google Patents
Method for manufacturing standard sample for scanning electron microscope magnification calibration Download PDFInfo
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- CN101598645B CN101598645B CN2009103039144A CN200910303914A CN101598645B CN 101598645 B CN101598645 B CN 101598645B CN 2009103039144 A CN2009103039144 A CN 2009103039144A CN 200910303914 A CN200910303914 A CN 200910303914A CN 101598645 B CN101598645 B CN 101598645B
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- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title abstract description 8
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 58
- 239000010703 silicon Substances 0.000 claims abstract description 58
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000000758 substrate Substances 0.000 claims abstract description 44
- 238000012545 processing Methods 0.000 claims abstract description 11
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- 239000002184 metal Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000001459 lithography Methods 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000005566 electron beam evaporation Methods 0.000 claims description 3
- 235000011149 sulphuric acid Nutrition 0.000 claims description 3
- 239000001117 sulphuric acid Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000010894 electron beam technology Methods 0.000 abstract description 16
- 238000001020 plasma etching Methods 0.000 abstract description 6
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000000609 electron-beam lithography Methods 0.000 abstract 2
- 238000003754 machining Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
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Abstract
The invention discloses a method for manufacturing a scanning electron microscope magnification calibration standard sample, and belongs to the technical field of nano pattern processing. The method comprises the following steps: processing the surface of a silicon substrate, and coating an electron beam lithography resist on the silicon substrate; baking the silicon substrate coated with the electron beam lithography resist; carrying out electron beam direct writing exposure on the baked silicon substrate in a single line exposure mode; and developing, fixing, drying and annealing the silicon substrate subjected to electron beam direct writing exposure, and covering a metal film on the surface of the processed silicon substrate to form a scanning electron microscope magnification calibration standard sample. The invention avoids the figure quality reduction caused by the plasma etching process, is beneficial to the manufacture of a high-resolution dense line figure structure and the realization of the electron beam exposure limit resolution.
Description
Technical field
The present invention relates to the nano-pattern processing technique field, relate in particular to a kind of method for making of scanning electron microscope magnification calibration standard sample.
Background technology
The detection of being carried out in the semiconductor manufacturing industry is that (Scanning Electron Microscope SEM) carries out the dependence scanning electron microscope to a great extent.Present most of scanning electron microscope all has the demonstration of enlargement ratio, and is equipped with micron, nano level scale strip, and these data all are recorded in the corresponding image file.Measuring numerical value can directly draw on image, microphoto or digital measuring system.The precision of measuring depends on many factors, a wherein very important enlargement ratio that factor is exactly SEM.The enlargement ratio of SEM can be defined as the ratio of area that sample shows and the area of electron beam scanning.Usually to amplify the variable resistor shelves number of resolution voltage divider be limited to scanning electron microscope, can't reach enough sensitivity to adjust transfer point continuously, exactly; The hysteresis of the aberration of electron-optical system and lens etc. all can have influence on the accuracy of amplifying resolution in addition.For this reason, except the system design of improving SEM, normally make in the world and carry out the standard model of magnification calibration regularly the enlargement ratio of SEM system is calibrated.
The domain that scanning electron microscope magnification calibration standard sample adopts is generally intensive scale mark.The key index of properties of sample has the relative error, error profile in cycle, the cycle of scanning electron microscope magnification calibration standard sample, through the stability of electron beam scanning and time stability or the like.The cycle of intensive scale mark relative error more little, the cycle is more little, error profile is even more, stability is high more, and the quality of sample is high more.At present in the world the method for silicon chip being carried out plasma etching is generally all adopted in the making of the type sample.
The quality of sample is common and its method for making is closely related.The classic method of making scanning electron microscope magnification calibration standard sample is to have on the silicon chip on the basis of resist graphic structure, by plasma etching the resist graphic structure is being transferred to silicon substrate.When machining precision is deep into hundred nanometers and when following, though can go out high-resolution resist figure by the electric lithography fabrication techniques, but the machining precision of plasma etching equipment and running status can produce bigger influence to the quality of figure transfer, edge roughness or the like for example, thus limited the raising of sample precision.
Summary of the invention
In view of above-mentioned, the present invention proposes a kind of method for making of scanning electron microscope magnification calibration standard sample, this method has overcome the machining precision of plasma etching equipment and running status to the influence that the quality of figure transfer can produce, and has improved the machining precision to sample.
The invention provides a kind of method for making of scanning electron microscope magnification calibration standard sample, described method comprises:
Step 1: surface of silicon is handled, and on described silicon substrate, applied the beamwriter lithography resist;
Step 2: the described silicon substrate that will be coated with described beamwriter lithography resist toasts;
Step 3: the described silicon substrate after the baking is carried out e-beam direct-writing exposure under the single line exposure mode;
Step 4: to the described silicon substrate behind the e-beam direct-writing exposure develop, photographic fixing, drying and annealing in process, and the surface of silicon covering metal film after processing forms scanning electron microscope magnification calibration standard sample.
Step at the surface of silicon covering metal film after the processing in the described step 4 is specially: by the surface of silicon evaporation metal film of electron beam evaporation after processing.
The thickness of described metallic film is 3nm.
The step of in the described step 1 surface of silicon being handled specifically comprises:
Step 101: pending silicon substrate is placed concentrated sulphuric acid heating 30 minutes, and cooling is then taken out;
Step 102: place deionized water to clean cooled silicon substrate;
Step 103: the silicon substrate after dry the cleaning, and under 100 ℃, toasted 5 minutes.
Described step 2 is specially: the described silicon substrate that will be coated with the beamwriter lithography resist placed on 180 ℃ the hot plate baking 2 minutes.
The step of in the described step 4 the described silicon substrate behind the e-beam direct-writing exposure being carried out annealing in process is specially: will develop, the silicon substrate after photographic fixing and the dried handled 20-30 minute in 300-450 ℃ tube type resistance furnace.
Beneficial effect of the present invention: the method for making of scanning electron microscope magnification calibration standard sample provided by the invention, directly adopt the e-beam direct-writing exposure fabrication techniques to go out the HSQ resist graphic structure of sample domain, the graphical quality of having avoided plasma etch process to bring descends, and helps the making of the intensive line graph structure of high resolving power; In addition, the present invention has also adopted the single line exposure mode in electron beam exposure, make electron beam only scan, and the live width size that can reach on another dimension depend on the bundle spot size of electron beam, helps the realization of electron beam exposure limiting resolution along dimension with size.
Description of drawings
Fig. 1 is the method for making process flow diagram of the scanning electron microscope magnification calibration standard sample that provides of the embodiment of the invention;
Fig. 2 and Fig. 3 are the stereoscan photographs of the scanning electron microscope magnification calibration standard sample of embodiment of the invention making.
Embodiment
For making the purpose, technical solutions and advantages of the present invention clearer, embodiment of the present invention is described further in detail below in conjunction with accompanying drawing.
Referring to Fig. 1, the embodiment of the invention provides a kind of method for making of scanning electron microscope magnification calibration standard sample, specifically comprises the steps:
Step 1: surface of silicon is handled, and on silicon substrate, applied the beamwriter lithography resist;
One or more pieces pending silicon substrates are placed the concentrated sulphuric acid, heated several minutes, for example 30 minutes, cooling is then taken out, in deionized water, clean, dry up silicon substrate after the cleaning, make the silicon substrate drying with the nitrogen air gun, and with hot plate this silicon substrate is at high temperature toasted, for example 100 ℃ of bakings 5 minutes down; On silicon substrate, apply beamwriter lithography resist HSQ; In actual applications, can use sol evenning machine at surface of silicon coating resist glue-line HSQ (model is Fox12), the rotating speed of sol evenning machine can be 3000r/m, and the coating time can be 60 seconds;
Step 2: the silicon substrate that will be coated with the beamwriter lithography resist toasts;
The silicon substrate that is coated with the beamwriter lithography resist is placed on the hot plate toasts, the temperature of hot plate can be set to 180 ℃, and stoving time can be set to 2 minutes; Last gained, it is 100nm-180nm that the beamwriter lithography resist that obtains is surveyed the thickness that is, this thickness is 150nm in the present embodiment; The silicon substrate that is coated with the beamwriter lithography resist is toasted, can remove the solvent in the resist, and provide certain mechanical strength to resist;
Step 3: the silicon substrate after the baking is carried out e-beam direct-writing exposure under the single line exposure mode;
Directly write in the exposure mode at single line, because figure only has size on a dimension, on another dimension, be of a size of zero, thereby electron beam only scans along the dimension with size, and the live width size that can reach depends on the bundle spot size of electron beam on another dimension.In actual applications, exposure sources can be JEO-JBX6300FS system or other electron beam exposure equipment, and the parameter of the exposure sources that present embodiment adopted is that accelerating potential is 100kv, and line is 200pA, and the exposure step pitch is 1nm, and exposure dose is 7nc/cm;
Step 4: to the silicon substrate behind the e-beam direct-writing exposure develop, photographic fixing and dried;
In the present embodiment, specifically use the CD26 developer solution, development temperature is 40 ℃, and development time is 1 minute; Use deionized water as stop bath, photographic fixing 30 seconds; After finishing, photographic fixing silicon substrate is dried up with the nitrogen air gun;
Step 5: will develop, the silicon substrate after photographic fixing and the dried carries out annealing in process;
To develop, the silicon substrate after photographic fixing and the dried carries out annealing in process, can reduce HSQ and behind electron beam exposure, form defective in amorphous monox, and further strengthen the physical strength and the stability in scanning electron microscope scanning of its graphic structure, for example can in 300-450 ℃ tube type resistance furnace, handle 20-30 minute; Preferably, in 400 ℃ YFK80*600/13Q-YC tube type resistance furnace, handled 30 minutes;
Step 6: by electron beam evaporation, the metallic film of the surface of silicon evaporation 3nm thickness after annealed processing;
The metallic film of the surface of silicon evaporation 3nm thickness after annealed processing can improve the electric conductivity of sample surfaces, and improves the quality of scanning electron microscope imaging.
Through after the above-mentioned steps, can finally obtain the scanning electron microscope magnification calibration standard sample shown in Fig. 2 and 3.
In the present embodiment, the substrate of employing is a silicon substrate; In actual applications, can select other conductors or Semiconductor substrate according to the requirement of using.Utilize the exposure characteristics of other resists, and utilizing e-beam direct-writing exposure to make scanning electron microscope, to amplify the technical scheme of resolution standard sample be consistent with technical scheme provided by the invention, should be included within protection scope of the present invention on technical thought.
According to above embodiment as can be seen, use the method for making of scanning electron microscope magnification calibration standard sample provided by the invention, solved the problem that the machining precision of plasma etching equipment and running status exert an influence to the quality of figure transfer, improved machining precision to sample, avoid the graphical quality on the sample that plasma etch process brings to descend, helped making the intensive line graph structure of high resolving power; In addition, use manufacture method of the present invention to make electron beam only scan, and the live width size that can reach on another dimension depend on the bundle spot size of electron beam, helps realizing the electron beam exposure limiting resolution along dimension with size.
The above only is preferred embodiment of the present invention, and is in order to restriction the present invention, within the spirit and principles in the present invention not all, any modification of being done, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. the method for making of a scanning electron microscope magnification calibration standard sample is characterized in that, described method comprises:
Step 1: surface of silicon is handled, and on described silicon substrate, applied the beamwriter lithography resist;
Step 2: the described silicon substrate that will be coated with described beamwriter lithography resist toasts;
Step 3: the described silicon substrate after the baking is carried out e-beam direct-writing exposure under the single line exposure mode;
Step 4: to the described silicon substrate behind the e-beam direct-writing exposure develop, photographic fixing, drying and annealing in process, and the surface of silicon covering metal film after processing forms scanning electron microscope magnification calibration standard sample.
2. the method for making of scanning electron microscope magnification calibration standard sample according to claim 1, it is characterized in that the step at the surface of silicon covering metal film after the processing in the described step 4 is specially: by the surface of silicon evaporation metal film of electron beam evaporation after processing.
3. the method for making of scanning electron microscope magnification calibration standard sample according to claim 2 is characterized in that, the thickness of described metallic film is 3nm.
4. the method for making of scanning electron microscope magnification calibration standard sample according to claim 1 is characterized in that, the step of in the described step 1 surface of silicon being handled specifically comprises:
Step 101: pending silicon substrate is placed concentrated sulphuric acid heating 30 minutes, and cooling is then taken out;
Step 102: place deionized water to clean cooled silicon substrate;
Step 103: the silicon substrate after dry the cleaning, and under 100 ℃, toasted 5 minutes.
5. according to the method for making of claim 1 or 4 described scanning electron microscope magnification calibration standard samples, it is characterized in that described step 2 is specially: the described silicon substrate that will be coated with the beamwriter lithography resist placed on 180 ℃ the hot plate baking 2 minutes.
6. according to the method for making of claim 1 or 4 described scanning electron microscope magnification calibration standard samples, it is characterized in that the step of in the described step 4 the described silicon substrate behind the e-beam direct-writing exposure being carried out annealing in process is specially: will develop, the silicon substrate after photographic fixing and the dried handled 20-30 minute in 300-450 ℃ tube type resistance furnace.
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| CN2009103039144A CN101598645B (en) | 2009-07-01 | 2009-07-01 | Method for manufacturing standard sample for scanning electron microscope magnification calibration |
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| CN2009103039144A CN101598645B (en) | 2009-07-01 | 2009-07-01 | Method for manufacturing standard sample for scanning electron microscope magnification calibration |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2445660C2 (en) * | 2010-03-11 | 2012-03-20 | Андрей Сергеевич Рябченко | Using thermal compound as adhesive and heat-conducting composition when analysing biological samples on scanning electron microscope using freezing attachments |
| CN103868766A (en) * | 2012-12-18 | 2014-06-18 | 中国科学院物理研究所 | Preparation method of length standard sample for length measurement of scanning electron microscopy |
| CN107941346A (en) * | 2017-11-16 | 2018-04-20 | 中国电子科技集团公司第十三研究所 | Spatial resolution calibrating installation and preparation method |
| CN109981966B (en) * | 2017-12-27 | 2023-09-12 | 上海德运光电技术有限公司 | Super-resolution imaging camera and imaging method thereof |
| CN110054150A (en) * | 2019-04-29 | 2019-07-26 | 西安交通大学 | A kind of calibration nanometer geometric sense standard jig and preparation method thereof |
| CN114220724A (en) * | 2021-12-01 | 2022-03-22 | 中国电子科技集团公司第十三研究所 | Scanning electron microscope calibration method, device, terminal and storage medium |
| CN114414747B (en) * | 2022-03-14 | 2022-08-12 | 中芯越州集成电路制造(绍兴)有限公司 | Verification method for laser annealing uniformity |
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Address after: No. 3, North Tu Cheng West Road, Chaoyang District, Beijing Patentee after: Institute of Microelectronics of the Chinese Academy of Sciences Address before: 100029 Microelectronics Institute, Chinese Academy of Sciences, 3 north earth road, Chaoyang District, Beijing Patentee before: Institute of Microelectronics of the Chinese Academy of Sciences |