CN109867260B - Method for carrying out electron beam or ion beam focusing etching and microscopic imaging on non-conductive substrate - Google Patents
Method for carrying out electron beam or ion beam focusing etching and microscopic imaging on non-conductive substrate Download PDFInfo
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- CN109867260B CN109867260B CN201910208280.8A CN201910208280A CN109867260B CN 109867260 B CN109867260 B CN 109867260B CN 201910208280 A CN201910208280 A CN 201910208280A CN 109867260 B CN109867260 B CN 109867260B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00349—Creating layers of material on a substrate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00523—Etching material
- B81C1/00531—Dry etching
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C99/00—Subject matter not provided for in other groups of this subclass
- B81C99/0035—Testing
- B81C99/004—Testing during manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a method for carrying out electron beam or ion beam focusing etching and microscopic imaging on a non-conductive substrate, belonging to the field of micro-nano processing and comprising the following steps: 1) designing the shape and size of the photoetching mask; 2) carrying out photoetching treatment on the non-conductive substrate; 3) carrying out metal coating treatment on the non-conductive substrate after photoetching treatment to form a metal band; 4) developing the non-conductive substrate after coating to obtain a sample; 5) carrying out grounding treatment on the metal strip; 6) carrying out vacuum-pumping treatment on the sample; 7) focusing a metal band of a sample, selecting an electron beam, and adjusting a sample stage to a sample area to be engraved after imaging is clear; 8) and importing or drawing the appearance of the micro-nano structure to be etched, and after setting parameters, carrying out FIB (focused ion beam) or EBL (electron beam lithography) etching and imaging on the sample. The local conductivity of the surface of the non-conductive substrate material is effectively improved, and stable focusing of electron beams and ion beams is realized, so that micro-nano etching and micro-imaging of the surface of the non-conductive material are realized.
Description
Technical Field
The invention relates to the field of micro-nano processing, in particular to a method for carrying out electron beam or ion beam focusing etching and microimaging on a non-conductive substrate.
Background
Focused ion beam technology (FIB) is a microdissection technique that focuses an ion beam to a very small size using an electrostatic lens. Similarly, Electron-beam lithography (EBL) is a technique in which a resist on a substrate is exposed to focused Electron beams to generate regions having different dissolution properties in the resist, and the regions are developed with a developer having selectivity according to the dissolution properties of the regions to obtain a desired pattern.
The two technologies have important application value in the field of micro-nano processing. The principle of the focused Ion beam microscope is compared with that of the scanning electron microscope, wherein the Ion beam is a Liquid Metal Ion Source (LMIS), and the Metal material is Gallium (galium, Ga), because Gallium has a low melting point, a low vapor pressure, and a good oxidation resistance. The secondary electrons and secondary ions excited by gallium ion scanning impact on the surface of the test piece of the ion beam microscope are the source of the image, and the resolution of the image is determined by the size and distortion correction of the ion beam, the acceleration voltage of the charged ions, the intensity of the secondary ion signal and the like. Similarly, the resolution of the e-beam lithography is mainly determined by the focusing effect of the electron beam.
By being limited by the two technical principles, if the observed sample is a non-conductive material, charged ions or electrons are easily accumulated on the surface of the sample, so that the charged ions or the electrons interact with the focused ion beam to interfere the focusing effect of the electron beam or the ion beam, the imaging becomes fuzzy, and the work of focused ion beam etching, electron beam etching and the like cannot be realized.
The observation of some non-conductive materials can be achieved to a certain extent by the existing silicon-silicon nitride substrate with windows, but the substrate material of the method is limited, and a silicon layer with a certain thickness is required. At the same time, it can only be used for observation. If observation and micro-nano processing on different substrate materials are to be realized, the requirements cannot be met at all. At present, the minimum resolution ratio capable of being processed on an insulating substrate without conductive material support is more than 80 nanometers, which greatly limits the application range of two technologies of focused ion beam etching and electron beam etching and brings great inconvenience to the research and application of related fields.
Disclosure of Invention
The invention aims to provide a method for carrying out electron beam or ion beam focusing etching and microscopic imaging on a non-conductive substrate. The method can effectively improve the local conductivity of the surface of the non-conductive substrate material, effectively reduce the accumulation of charges on the surface of the non-conductive substrate material, and realize the long-term stable focusing of electron beams and ion beams, thereby realizing the micro-nano etching/exposure/deposition, the micro-imaging and the like on the surface of the non-conductive material.
In order to achieve the above object, the method for performing electron beam or ion beam focused etching and microscopic imaging on a non-conductive substrate provided by the present invention comprises the following steps:
1) designing the shape and size of the photoetching mask;
2) carrying out photoetching treatment on the non-conductive substrate;
3) carrying out metal coating treatment on the non-conductive substrate after photoetching treatment to form a metal band;
4) carrying out development treatment on the non-conductive substrate after coating;
5) carrying out grounding treatment on the metal strip;
6) carrying out vacuum-pumping treatment on the sample;
7) selecting an electron beam, carrying out focusing treatment on a metal belt area of a sample, and adjusting a sample stage to a sample area to be engraved after imaging is clear;
8) and importing or drawing the appearance of the micro-nano structure to be etched, and after setting parameters, carrying out FIB (focused ion beam) or EBL (electron beam lithography) etching and imaging on the sample.
According to the technical scheme, the strip-shaped metal strip is introduced to the surface of the non-conductive substrate, so that the local conductivity of the surface of the non-conductive substrate material can be effectively improved, the accumulation of charges on the surface of the non-conductive substrate material can be effectively reduced, and the long-term stable focusing of electron beams and ion beams can be realized, thereby realizing the micro-nano etching/exposure/deposition, the micro-imaging and the like on the surface of the non-conductive material. The design of the photoetching mask needs to consider the selection of later photoetching glue types (positive glue/negative glue) and the size parameters of metal strips prepared later, and the overall size of non-conductive substrate materials. The metal band plays a role in guiding electrons, and the requirement on the precision of photoetching is not high. The prepared photoetching morphology can select a metal ring or a polygonal metal ring connected with the main metal channel. The preparation of the mask plate at the early stage is of great significance to the related work at the later stage: it determines the spacing of the metal strips, the width of the metal strips and the topographical features formed by the metal strips. These feature sizes still need to be optimally designed for different non-conductive materials.
The specific scheme is that metal coating treatment is carried out on the non-conductive substrate after photoetching treatment in the step 3) by methods of electron beam evaporation, thermal evaporation, magnetron sputtering, atomic layer deposition or spraying. But not limited to the above methods, the quality of the metal film prepared by different methods may have a certain difference, but has little influence on the focusing and imaging effects at the later stage.
Another specific solution is that the thickness of the metal strip in step 3) is greater than 50 nm. The thickness of the metal strip mainly affects the later development process, usually the metal thickness of more than 50 nm can ensure that the metal strip is not broken during the development, and the excessive thickness of the metal layer affects the development accuracy.
Another specific scheme is that a matching layer with the thickness of about 10 nanometers is plated on the non-conductive substrate before the metal plating treatment is carried out on the non-conductive substrate in the step 3). When the metal waveguide is prepared, the adhesion degree of the metal material and the substrate material needs to be considered, and if the adhesion degree of the adopted material and the substrate is not high, a matching layer can be plated on the substrate firstly to improve the adhesion degree of the metal strip and the substrate.
More specifically, the thickness of the matching layer is 5-10 nanometers. For example, when a gold thin film is plated on a common glass substrate, it is considered that a titanium film of about 5 to 10 nm is first plated.
Another specific proposal is that the material of the metal belt in the step 3) is gold, platinum or titanium. In addition to the degree of adhesion to the substrate, the metal strip must be produced in consideration of the conductivity, stability, and cost of the metal material. Commonly used gold (gold), platinum (platinum), titanium (titanium) and the like can well meet the requirements. Materials that are easily oxidized, such as silver (silver) and aluminum (aluminum), can also be used as materials for producing metal strips if they can ensure later electrical conductivity. The metal material may be replaced by any conductive material, such as graphite, ITO, etc. The respective metal strips may thus differ in their manner of production.
Another specific scheme is that in the step 5), the metal strip is connected with a sample stage for FIB or EBL etching to realize grounding treatment. When designing the photoetching mask, in order to realize effective dredging of the metal strips to local electrons and ions, metal electrodes which are connected with all the metal strips and an external conductive sample stage or other grounding materials need to be designed.
In another specific embodiment, the surface of the non-conductive substrate is cleaned before the photolithographic process is performed on the non-conductive substrate in step 2). The non-conductive substrate material is required to have certain surface flatness, and the cleaning work related to the photoetching is carried out, and the cleaning mode is determined according to the material and the requirement. Taking a common glass sheet as an example, the ultrasonic treatment is carried out by using acetone and ethanol.
In the invention, the width of the metal strip has certain influence on the later electron beam or ion beam focusing and microscopic imaging, but the influence is basically negligible for general photoetching precision (less than or equal to 2 microns). The more influential the later results are the presence of a broken metal ring made lithographically and the metal strip of the main track.
Drawings
FIG. 1 is a schematic diagram of the bonding of a non-conductive substrate to a metal tape according to an embodiment of the present invention, FIG. 1(a) is a top view, and FIG. 1(b) is a cross-sectional view of FIG. 1 (a);
FIG. 2 is an SEM image of a three-channel structure with a trench width of 85 nm and a pitch of 85 nm etched by FIB technique on a quartz plate coated with a titanium oxide film according to an embodiment of the present invention;
FIG. 3 is an SEM image of an eagle microstructure with a trench width of 70 nm and a space of 76 nm etched by using FIB technology on a quartz plate coated with a titanium oxide film according to an embodiment of the present invention;
FIG. 4 is an SEM image of a ring microstructure with trench width of 70 nm and pitch of 76 nm etched by FIB technique on a quartz plate coated with a titanium oxide film according to an embodiment of the present invention;
FIG. 5 is an SEM image of a multi-channel structure with a trench width of 30 nm etched on a quartz plate using FIB technology according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described with reference to the following embodiments and accompanying drawings.
Examples
The method for performing electron beam or ion beam focusing etching and microscopic imaging on the non-conductive substrate comprises the following steps:
s1 designing the shape and size of the photoetching mask;
s2, carrying out photoetching treatment on the non-conductive substrate;
s3, carrying out metal coating treatment on the non-conductive substrate after the photoetching treatment to form a metal band;
s4, developing the non-conductive substrate after film plating to obtain a sample;
s5 performing grounding processing on the metal strip;
s6, carrying out vacuum-pumping treatment on the sample;
s7, focusing the metal band of the sample, selecting an electron beam, and adjusting the sample stage to the sample area to be engraved after the image is clear;
s8, importing or drawing the appearance of the micro-nano structure to be etched, and after setting parameters, carrying out FIB or EBL etching and imaging on the sample.
Referring to fig. 1(a) and 1(b), respective metal strips 2 are prepared on a non-conductive substrate 1 by means of photolithography or the like, the metal strips 2 including a lithographically prepared polygonal metal endless belt 21 and a conductive metal strip structure 22. And then the reserved electrode 3 is grounded to guide surface focusing charges during focusing imaging. Corresponding to the arrays 4 and 5 with different metal belt widths; corresponding to arrays 5 and 6 of different sizes of metal rings.
In this embodiment, a corresponding lithography mask is first designed as required, and the flow used for lithography is a standard lithography flow: (1) spinning glue; (2) pre-baking; (3) exposing; (4) developing; (5) hardening the film. Then 5-10 nm titanium gold is prepared by magnetron sputtering and other technologies, and a 50 nm gold film is plated by thermal evaporation and other modes. Subsequently, a desmear treatment with acetone was carried out, which lasted approximately 30 minutes. And then, washing by using deionized water and drying. In this embodiment, a layer of 150 nm titanium oxide film is then formed on the structure by electron beam evaporation. When optical coating is carried out, the reserved electrode needs to be effectively protected and prevented from being covered by the optical medium film. And finally, connecting the reserved electrode with a sample table through a conductive adhesive tape, and carrying out grounding treatment.
Referring to fig. 2, the width of the channel etched on the titanium oxide film by the above method using the focused ion beam etching technique is 85 nm, the center-to-center distance of the channel is 85 nm, the depth is 100 nm, and the length is 5 μm.
FIG. 3 is an SEM image of an eagle emblem etched by the above method, in which the width of the etched channel is 70 nm, the center-to-center distance of the channel is 76 nm, and the depth is 100 nm.
FIG. 4 is a circular ring structure etched by the above method, the width of the channel is 70 nm, the center distance of the channel is 76 nm, the depth is 100 nm, and the diameter of the circular ring is 5 μm.
FIG. 5 shows a multi-channel structure with a channel width of 30 nm and a channel depth of 100 nm etched by focused ion beam technique on a pure quartz plate by the above method.
Claims (8)
1. A method for performing electron beam or ion beam focused etching and microscopic imaging on a non-conductive substrate is characterized by comprising the following steps:
1) designing the shape and size of the photoetching mask;
2) carrying out photoetching treatment on the non-conductive substrate;
3) carrying out metal coating treatment on the non-conductive substrate after photoetching treatment to form a metal band;
4) developing the non-conductive substrate after coating to obtain a sample;
5) carrying out grounding treatment on the metal strip;
6) carrying out vacuum-pumping treatment on the sample;
7) focusing a metal band of a sample, selecting an electron beam or an ion beam, and adjusting a sample stage to a sample area to be engraved after imaging is clear;
8) and importing or drawing the appearance of the micro-nano structure to be etched, and after setting parameters, carrying out FIB (focused ion beam) or EBL (electron beam lithography) etching and imaging on the sample.
2. The method of claim 1, wherein the step of performing electron beam or ion beam focused etching and microscopic imaging on the non-conductive substrate comprises:
and 3) performing metal coating treatment on the photoetching-treated non-conductive substrate by using electron beam evaporation, thermal evaporation, magnetron sputtering, atomic layer deposition or spraying.
3. The method of claim 1, wherein the step of performing electron beam or ion beam focused etching and microscopic imaging on the non-conductive substrate comprises:
the thickness of the metal belt in the step 3) is more than 50 nanometers.
4. The method of claim 1, wherein the step of performing electron beam or ion beam focused etching and microscopic imaging on the non-conductive substrate comprises:
and 3) plating a matching layer on the non-conductive substrate before performing metal plating treatment on the non-conductive substrate.
5. The method of claim 4, wherein the step of performing electron beam or ion beam focused etching and microscopic imaging on the non-conductive substrate comprises:
the thickness of the matching layer is 5-10 nanometers.
6. The method of claim 1, wherein the step of performing electron beam or ion beam focused etching and microscopic imaging on the non-conductive substrate comprises:
the metal belt in the step 3) is made of gold, platinum or titanium.
7. The method of claim 1, wherein the step of performing electron beam or ion beam focused etching and microscopic imaging on the non-conductive substrate comprises:
and in the step 5), the metal strip is connected with a sample stage for FIB or EBL etching to realize grounding treatment.
8. The method of claim 1, wherein the step of performing electron beam or ion beam focused etching and microscopic imaging on the non-conductive substrate comprises:
cleaning the surface of the non-conductive substrate before the photolithographic processing of the non-conductive substrate in step 2).
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810983031.1A CN109160488A (en) | 2018-08-27 | 2018-08-27 | The method of electron beam/ion beam focusing etching and micro-imaging is carried out on nonconductive substrate |
| CN2018109830311 | 2018-08-27 |
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| CN109867260B true CN109867260B (en) | 2021-02-02 |
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| CN201910208280.8A Active CN109867260B (en) | 2018-08-27 | 2019-03-19 | Method for carrying out electron beam or ion beam focusing etching and microscopic imaging on non-conductive substrate |
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| CN105246850A (en) * | 2012-11-29 | 2016-01-13 | 康宁股份有限公司 | Methods of fabricating glass articles by laser damage and etching |
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2018
- 2018-08-27 CN CN201810983031.1A patent/CN109160488A/en active Pending
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| JPH01140765A (en) * | 1987-11-27 | 1989-06-01 | Semiconductor Energy Lab Co Ltd | Manufacture of image sensor |
| JP2008019123A (en) * | 2006-07-12 | 2008-01-31 | Nagaoka Univ Of Technology | Finely processed glass and processing method of the same |
| US8747599B2 (en) * | 2008-05-29 | 2014-06-10 | Chidella Krishna Sastry | Process for making self-patterning substrates and the product thereof |
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| JP2013119512A (en) * | 2011-12-08 | 2013-06-17 | Mitsubishi Electric Corp | Method for producing glass substrate and method for producing solar cell |
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| CN109867260A (en) | 2019-06-11 |
| CN109160488A (en) | 2019-01-08 |
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