CN109867260A - The method of electron beam/ion beam focusing etching and micro-imaging is carried out on nonconductive substrate - Google Patents
The method of electron beam/ion beam focusing etching and micro-imaging is carried out on nonconductive substrate Download PDFInfo
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- CN109867260A CN109867260A CN201910208280.8A CN201910208280A CN109867260A CN 109867260 A CN109867260 A CN 109867260A CN 201910208280 A CN201910208280 A CN 201910208280A CN 109867260 A CN109867260 A CN 109867260A
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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
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Abstract
The method that the invention discloses a kind of to carry out electron beam/ion beam focusing etching and micro-imaging on nonconductive substrate, belongs to micro-nano technology field, comprising: 1) design the morphology and size of lay photoetching mask plate；2) photoetching treatment is carried out to nonconductive substrate；3) the enterprising row metal coating film treatment of nonconductive substrate after photoetching treatment forms metal tape；4) carrying out development treatment to the nonconductive substrate after plated film becomes sample；5) grounding is carried out to metal tape；6) vacuumize process is carried out to sample；7) processing is focused to the metal tape of sample, selects electronic beam current, it is to be imaged it is clear after, adjustment sample stage to sample area to be etched；8) pattern of required etching micro-nano structure is imported or drawn, FIB or EBL is carried out to sample after setting parameter and etches and is imaged.The local electric conductivity for effectively promoting non-conductive substrate material surface realizes that electron beam and stablizing for ion beam focus, to realize the micro-nano etching and micro-imaging to non-conducting material surface.
Description
Technical field
The present invention relates to micro-nano technology fields, specifically, be related to one kind carries out electron beam/ion on nonconductive substrate
The method that beam focuses etching and micro-imaging.
Background technique
Focused ion beam technology (focused ion beam, FIB) is by ion beam focusing using electrostatic lenses at very
The microdissection technology of small size.Similarly, electron beam lithography (Electron-beam lithography, EBL) is benefit
The resist on substrate is exposed with the electron beam after focusing, generates the area with different solubility properties in the resist
Domain is developed according to the dissolution characteristics of different zones using selective developer, and required figure is obtained.
Both the above technology has important application value in micro-nano technology field.Focused ion beam microscope and scanning electricity
The microscopical principle of son compares, and wherein ion beam is liquid metal ion source (Liquid Metal Ion Source, LMIS),
Metal material is gallium (Gallium, Ga), because gallium element has low melting point, low-vapor pressure and good resistance to oxidation.Ion
The secondary electron and secondary ion that the strip of beam microscope is inspired by gallium ion scanning shock are the source of image, shadow
The resolution ratio of picture is decided by the strong of the size of ion beam and distortions correction, the acceleration voltage of charged ion and secondary ion signal
Degree etc..Similarly, the resolution ratio of electron beam lithography depends mainly on the focusing effect of electron beam.
It is limited to the principle of both the above technology, if observed sample is non-conducting material, charged ion or electronics
It is easily accumulated in sample surfaces, to interact with focused ion beam, interferes electron beam/ion beam focusing effect, so that
Imaging thickens, and cannot achieve the work such as focused-ion-beam lithography and electron beam lithography.
Now with silicon-silicon nitrate substrate of windowing, the observation to some non-conducting materials can be realized to a certain extent, but should
The substrate material of kind method is limited, it is necessary to have certain thickness silicon layer.Meanwhile it also can be only used to observe.If real
Observation and micro-nano technology on present various substrates material, then can not meet the requirements completely.It is supported at present in no conductive material
Insulating substrate on, the minimum resolution that can process is greater than 80 nanometers, and this greatly limits focused ion beams and electron beam
The application range of two kinds of technologies is etched, also brings very big inconvenience to the research of related fields and application.
Summary of the invention
It is an object of the present invention to provide one kind on nonconductive substrate carry out electron beam/ion beam focusing etching and it is micro- at
The method of picture.This method can effectively promote the local electric conductivity on non-conductive substrate material surface, and nonconductive substrate material is effectively reduced
Expect the accumulation of surface charge, realize the focusing steady in a long-term of electron beam and ion beam, to realize to non-conducting material surface
Micro-nano etching/exposure/deposition and micro-imaging etc..
To achieve the goals above, provided by the invention that electron beam/ion beam focusing etching is carried out on nonconductive substrate
And micro-imaging method the following steps are included:
1) morphology and size of lay photoetching mask plate is designed；
2) photoetching treatment is carried out to nonconductive substrate；
3) the enterprising row metal coating film treatment of nonconductive substrate after photoetching treatment forms metal tape；
4) development treatment is carried out to the nonconductive substrate after plated film；
5) grounding is carried out to metal tape；
6) vacuumize process is carried out to sample；
7) select electronic beam current, processing be focused to the metal region of sample, it is to be imaged it is clear after, adjustment sample stage
To sample area to be etched；
8) import or draw needed for etching micro-nano structure pattern, be arranged parameter after to sample carry out FIB or EBL etching and
Imaging.
In above-mentioned technical proposal, by carrying out the introducing of bullion band in non-conductive substrate surface, can effectively it be promoted non-
The accumulation of non-conductive substrate material surface charge is effectively reduced in the local electric conductivity on conductive substrate material surface, realizes electron beam
With the focusing steady in a long-term of ion beam, thus realize to the micro-nano etching/exposure/deposition on non-conducting material surface and it is micro- at
As etc..Wherein the design of lay photoetching mask plate needs to consider the selection and later period preparation of later period photoresist type (positive photoresist/negtive photoresist)
Metal strip dimensional parameters and non-conductive substrate material overall dimensions.Metal tape plays the role of guiding electronics, to light
The required precision at quarter is not high.The photoetching pattern of preparation can choose the metal ring being connected with main metal passage or polygon gold
Belong to ring.Early period, the preparation of mask had vital meaning in relation to work to the later period: it determines the spacing of metal strip, gold
Belong to shape characteristic composed by the width and metal strip of item.According to different non-conducting materials, these characteristic sizes still need into
Row optimization design.
Specific scheme is in step 3) by electron beam evaporation, thermal evaporation, magnetron sputtering, atomic layer deposition or spraying plating
The enterprising row metal coating film treatment of nonconductive substrate of the method after photoetching treatment.But it is not limited to the above several method, distinct methods
The quality for the metallic film prepared can there is some difference, but influences very little to the focusing in later period and imaging effect.
Another specific scheme be step 3) in metal tape with a thickness of be greater than 50 nanometers.The thickness of metal tape mainly can
The developing process in later period is influenced, usual 50 nanometers or more of metal thickness can guarantee that metal tape is not broken in development, and mistake
Thick metal layer will affect the accuracy of development.
Another specific scheme is first to lead non-before to the enterprising row metal coating film treatment of nonconductive substrate in step 3)
The matching layer of one layer of 10 ran is plated on electric substrate.When preparing metal waveguide, need to consider metal material and substrate material
Degree of adhesion can first plate one layer of matching layer on substrate if the degree of adhesion of used material and substrate is not high, with improve
The degree of adhesion of metal tape and substrate.
More specific scheme is matching layer with a thickness of 5~10 nanometers.For example, being coated with gold thin film on common glass substrate
When, it may be considered that it is coated with the titanium film of one layer of 5-10 ran first.
Another specific scheme is that the material of metal tape in step 3) is gold, platinum or titanium.In addition to wanting when preparing metal tape
Consider outer with the degree of adhesion of substrate height, it is also necessary to comprehensively consider the electric conductivity of metal, the cost of stability and metal material
Deng.Common gold (gold), platinum (platinum), titanium (titanium) etc. can be met the requirements well.Silver-colored (silver) and
Aluminium (aluminum) etc. is easy to the material aoxidized, if it is possible to which the electric conductivity for guaranteeing the later period then can also serve as preparing metal tape
Material.Metal material can be substituted using any conductive material, such as graphite, ITO etc..Corresponding metal tape production
Therefore mode may have different.
Another specific scheme be step 5) in by by metal band and carry out FIB or EBL etching sample stage into
Row connection is grounded processing.When designing lay photoetching mask plate, in order to realize having for metal strip local area electronics and ion
Effect is dredged, and the metal electrode that all metal strips are connected with extraneous conducting sample platform or other earthing materials need to be designed.
Another specific scheme be step 2) in nonconductive substrate carry out photoetching treatment before to nonconductive substrate
Surface cleaned.Non-conductive substrate material requires certain surface smoothness, related clear carrying out photoetching progress
Work is washed, depending on cleaning way is because of material and needs.By taking common glass sheet as an example, it need to be carried out at ultrasound with acetone and ethyl alcohol
Reason.
In the present invention, the width of metal tape has certain influence to the electron beam/ion beam focusing and micro-imaging in later period,
But for general lithographic accuracy (≤2 microns), this influence can be ignored substantially.Anaphase is influenced bigger be
The case where whether standby becket of optical graving and major trunk roads metal tape are with the presence of fracture.
Detailed description of the invention
Fig. 1 is the nonconductive substrate of the embodiment of the present invention and the schematic diagram of metal tape bonding, and Fig. 1 (a) is top view, Fig. 1
(b) cross-sectional view for being Fig. 1 (a)；
Fig. 2 is the embodiment of the present invention on the quartz plate for being coated with thin film of titanium oxide, is using the ditch road width that FIB technique etches
85 nanometers, the SEM figure for the triple channel structure that spacing is 85 nanometers；
Fig. 3 is the embodiment of the present invention on the quartz plate for being coated with thin film of titanium oxide, is using the ditch road width that FIB technique etches
70 nanometers, the SEM figure for the hawk micro-structure that spacing is 76 nanometers；
Fig. 4 is the embodiment of the present invention on the quartz plate for being coated with thin film of titanium oxide, is using the ditch road width that FIB technique etches
70 nanometers, the SEM figure for the annulus micro-structure that spacing is 76 nanometers；
Fig. 5 is more channel structures that the embodiment of the present invention is 30 nanometers using the groove width that FIB technique etches on quartz plate
SEM figure.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, with reference to embodiments and its attached drawing is to this hair
It is bright to be described further.
Embodiment
The method that the present embodiment carries out electron beam/ion beam focusing etching and micro-imaging on nonconductive substrate include with
Lower step:
The morphology and size of S1 design lay photoetching mask plate；
S2 carries out photoetching treatment to nonconductive substrate；
The enterprising row metal coating film treatment of nonconductive substrate of the S3 after photoetching treatment forms metal tape；
S4, which carries out development treatment to the nonconductive substrate after plated film, becomes sample；
S5 carries out grounding to metal tape；
S6 carries out vacuumize process to sample；
S7 is focused processing to the metal tape of sample, selects electronic beam current, it is to be imaged it is clear after, adjustment sample stage to
Carve sample area；
S8 import or draw needed for etching micro-nano structure pattern, be arranged parameter after to sample carry out FIB or EBL etching and
Imaging.
Referring to Fig. 1 (a) and Fig. 1 (b), corresponding metal tape 2 is prepared by means such as photoetching on nonconductive substrate 1, gold
Belonging to band 2 includes the standby polygon metal ring band 21 and conductive metal band structure 22 of optical graving.It is carried out later by reserved electrode 3
Ground connection, surface focus charge when to focal imaging guide.Corresponding metal tape array 4 and array 5 of different size；It is corresponding
Metal ring size different array 5 and array 6.
In the present embodiment, first, in accordance with requiring to design corresponding lay photoetching mask plate, process used in photoetching is standard lithographic
Process: (1) glue is revolved；(2) front baking；(3) it exposes；(4) develop；(5) post bake.Later using the technologies such as magnetron sputtering preparation 5~10
The titanium of nanometer, 50 nanometers of golden film is coated with using modes such as thermal evaporations.Then, processing of removing photoresist is carried out using acetone, the process
Probably continue 30 minutes.It is cleaned, is dried using deionized water later.In this embodiment, electron beam is then also used
The mode of evaporation prepares one layer of 150 nanophase titania films in structure.Needs when optical coating are carried out to carry out reserved electrode
Effective protection prevents from being covered by optical medium film.Finally, reserved electrode is connected with sample stage by conductive tape, connect
Ground processing.
Referring to fig. 2, the ditch road width of focused-ion-beam lithography technology etching is utilized on thin film of titanium oxide using above method
It is 85 nanometers, the triple channel structure that channel center spacing is 85 nanometers, depth is 100 nanometers, and length is 5 microns.
Fig. 3 is that the SEM of the hawk emblem etched using above method is schemed, and etching ditch road width is 70 nanometers, between channel center in figure
Away from being 76 nanometers, depth is 100 nanometers.
Fig. 4 is the circular ring structure etched using above method, and ditch road width is 70 nanometers, and channel center spacing is 76 nanometers,
Depth is 100 nanometers, and circle diameter is 5 microns.
Fig. 5 is using above method on pure quartz plate, is 30 nanometers by the ditch road width that focused ion beam technology etches,
More channel structures that depth is 100 nanometers.
Claims (8)
1. a kind of method for carrying out electron beam/ion beam focusing etching and micro-imaging on nonconductive substrate, which is characterized in that
The following steps are included:
1) morphology and size of lay photoetching mask plate is designed；
2) photoetching treatment is carried out to nonconductive substrate；
3) the enterprising row metal coating film treatment of nonconductive substrate after photoetching treatment forms metal tape；
4) carrying out development treatment to the nonconductive substrate after plated film becomes sample；
5) grounding is carried out to metal tape；
6) vacuumize process is carried out to sample；
7) processing is focused to the metal tape of sample, selects electronic beam current, it is to be imaged it is clear after, adjustment sample stage to sample to be etched
Product region；
8) import or draw needed for etching micro-nano structure pattern, be arranged parameter after to sample carry out FIB or EBL etching and at
Picture.
2. electron beam/ion beam focusing etching and the micro-imaging according to claim 1 of being carried out on nonconductive substrate
Method, it is characterised in that:
In step 3) through electron beam evaporation, thermal evaporation, magnetron sputtering, atomic layer deposition or the method for spraying plating after photoetching treatment
The enterprising row metal coating film treatment of nonconductive substrate.
3. electron beam/ion beam focusing etching and the micro-imaging according to claim 1 of being carried out on nonconductive substrate
Method, it is characterised in that:
Metal tape described in step 3) with a thickness of be greater than 50 nanometers.
4. electron beam/ion beam focusing etching and the micro-imaging according to claim 1 of being carried out on nonconductive substrate
Method, it is characterised in that:
First plate one layer of matching in step 3) on the nonconductive substrate before to the enterprising row metal coating film treatment of nonconductive substrate
Layer.
5. electron beam/ion beam focusing etching and the micro-imaging according to claim 4 of being carried out on nonconductive substrate
Method, it is characterised in that:
The matching layer with a thickness of 5~10 nanometers.
6. electron beam/ion beam focusing etching and the micro-imaging according to claim 1 of being carried out on nonconductive substrate
Method, it is characterised in that:
The material of metal tape described in step 3) is gold, platinum or titanium.
7. electron beam/ion beam focusing etching and the micro-imaging according to claim 1 of being carried out on nonconductive substrate
Method, it is characterised in that:
Processing is grounded by the way that the sample stage of metal band and progress FIB or EBL etching to be attached in step 5).
8. electron beam/ion beam focusing etching and the micro-imaging according to claim 1 of being carried out on nonconductive substrate
Method, it is characterised in that:
The surface of nonconductive substrate is cleaned before carrying out photoetching treatment to nonconductive substrate in step 2).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2018109830311 | 2018-08-27 | ||
| 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 |
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| CN109867260A true CN109867260A (en) | 2019-06-11 |
| CN109867260B 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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| 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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| 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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2019
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101551476A (en) * | 2009-05-07 | 2009-10-07 | 吉林大学 | Laser three-dimensional preparing method of non-spherical micro-lens |
| JP2013119512A (en) * | 2011-12-08 | 2013-06-17 | Mitsubishi Electric Corp | Method for producing glass substrate and method for producing solar cell |
| CN104246974A (en) * | 2012-02-13 | 2014-12-24 | 印可得株式会社 | Method for forming patterns using laser etching |
| 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 |
| CN104995335A (en) * | 2013-02-13 | 2015-10-21 | 埃托特克德国有限公司 | Method for depositing a first metallic layer onto non-conductive polymers |
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| Publication number | Publication date |
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| CN109160488A (en) | 2019-01-08 |
| CN109867260B (en) | 2021-02-02 |
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