CN101850945B - Method for removing solvent from micro/nano structure - Google Patents
Method for removing solvent from micro/nano structure Download PDFInfo
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- CN101850945B CN101850945B CN2010101884904A CN201010188490A CN101850945B CN 101850945 B CN101850945 B CN 101850945B CN 2010101884904 A CN2010101884904 A CN 2010101884904A CN 201010188490 A CN201010188490 A CN 201010188490A CN 101850945 B CN101850945 B CN 101850945B
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Abstract
The invention discloses a method for removing a solvent from a micro/nano structure, which comprises the following steps of: (1) manufacturing the micro/nano structure on a substrate, spinning a photoresist on the substrate by utilizing a spin coating process, and obtaining a photoresist structure with the required height on the substrate material by adopting a photoetching process, or transferring the photoresist structure to the substrate by an etching process to obtain the substrate material micro/nano structure with the required height; (2) taking a rinsed sample out of the solvent, making the surface of the sample with the micro/nano structure face upwards, and placing the substrate on the sample to ensure that the micro/nano structure on the substrate material covers the micro/nano structure on the sample, or conversely, making the surface of the substrate with the micro/nano structure face upwards, and placing the sample on the substrate to ensure that the micro/nano structure on the substrate material covers the micro/nano structure on the sample; and (3) after the solvent is volatilized fully, removing the substrate, completing an auxiliary solvent removing process, and obtaining the micro/nano structure required. The method effectively solves the problem that the micro/nano structure is influenced by removing surface tension of the solvent in the solvent removing process.
Description
Technical field
The present invention relates to the solvent removal process in the micro-nano processing, particularly relate to the solvent removal process of large ratio of height to width micro-nano structure.
Background technology
Micro-nano processing mainly can be divided into dry method and wet method two big class technologies.After wet processing is finished micro-nano structure processing, the removal of solvents in the micro-nano structure so that obtain the micro-nano structure of needs, and need be carried out next step technology.So, in wet processing, inevitably have the removal of solvents problem.The most frequently used developing process and rinsing process all comprising the technical process of removing solvent in the micro-nano structure in the micro-nano processing.
Along with the development of micro-nano process technology, it is found that the premium properties of a lot of micro-nano devices comes from the large ratio of height to width of structure, the research of large ratio of height to width micro-nano structure comes into one's own day by day.Have the inertia device of large ratio of height to width micro nano structure, extraordinary semiconductor devices, optics and high energy diagnostic device and have a wide range of applications in a lot of fields, good device performance has broad application prospects it.The large ratio of height to width micro-nano structure has given device good performance, but has also brought many micro-nano processing problems simultaneously, and solvent removal process is exactly one of them.
The removal of solvents problem of large ratio of height to width micro-nano structure comes from the surface tension of solvent.In development and the rinsing process, after sample is finished development and rinsing, need be when from solvent, taking out with the removal of solvents on the sample, the surface tension that the solvent between the micro-nano structure brings will be applied on the micro-nano structure.The surface tension of the liquid that micro-nano structure the is suffered (J.Micromech.Microeng. that is directly proportional with 3 powers of the depth-width ratio of micro-nano structure, 15,2005, p978-983, K D Vora, et al.), along with the depth-width ratio of micro-nano structure increases gradually, its suffered surface tension also increases gradually, when its suffered tension force surpasses the mechanical strength of material itself, and the phenomenon that micro-nano structure deformation will take place, rupture even comes off.So, in the solvent removal process of large ratio of height to width micro-nano structure, micro-nano structure is as easy as rolling off a log to collapse, and the surface tension of uncared-for solvent has brought serious problem for the large ratio of height to width micro-nano structure in the micro-nano structure solvent removal process usually, presses for solution.
Up to the present, mainly contain two kinds of methods and can improve the influence that the surface tension of solvent in the removal of solvents process is brought to micro-nano structure.A kind of method is to reduce or remove the surface tension that acts on the micro-nano structure.Method (J.Vac.Sci.Technol., B18 (6), 2000, p3308-3312, Hideo Namatsu) by freeze drying, supercritical drying at first is frozen into solid with solvent, then it is directly changed into gaseous state and vapors away.Owing to do not have liquid state to occur mutually in the technical process, the yet influence of just having avoided surface tension to bring.But because the solvent of suitable this technology seldom, technical process also can exert an influence to micro-nano structure simultaneously, add also more complicated of technology itself, need specific equipment,, seldom can use in development and the rinsing process so the application of this method has a lot of restrictions.Another kind method is the surface tension of resisting solvent by the mechanical strength that strengthens micro-nano structure, prevents micro-nano structure generation deformation or collapses.Use the extraordinary material (Adv.Mater. of mechanical performance, 15 (14), 2003, p1180-1184, Mark.P.Stoykovich, et al.) or in micro-nano structure, add reinforcing rib structure (J.Micromech.Microeng., 15,2005, p978-983, K D Vora, et al.) can improve the mechanical strength of micro-nano structure effectively, improve the influence that the surface tension of solvent is brought in the solvent removal process.But also in research is explored, the material that can select for use seldom at present for the material that the existing good mechanical performance of this class has not only good photosensitive property, while but also adapts to the micro-nano processing technology; And the method that adds reinforcing rib structure in micro-nano structure all can reduce the performance of device usually, can not use in a lot of functional structures, so also seldom use.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of method of removing solvent in the micro-nano structure is provided,, the problem of collapsing yielding with the structure that occurs in the solvent removal process that solves micro-nano structure obtains required micro-nano structure.
Performing step of the present invention is as follows: a kind of method of removing solvent in the micro-nano structure, and step is as follows:
(1) on substrate, make micro-nano structure,
The photoresist that at first utilizes spin coating proceeding to coat on substrate adopts photoetching process to obtain the photoresist structure of desired height then on substrate; Also can utilize etching technics that photoresist structure is transferred on the substrate again, obtain the substrate material micro-nano structure of desired height;
(2) sample that will finish rinsing takes out from the rinsing solvent, and facing up of micro-nano structure arranged on the sample, then substrate is placed on the sample, makes on-chip structure cover the micro-nano structure on the sample; Or on the contrary substrate is had facing up of micro-nano structure, and then sample is placed on substrate, make micro-nano structure on the substrate material cover the micro-nano structure on the sample;
(3) after solvent evaporates is finished, substrate is removed, finished the auxiliary solvent process of removing, obtain required micro-nano structure.
Principle of the present invention: as shown in Figure 1, on the large ratio of height to width micro-nano structure of sample, add a substrate, for the upper surface of large ratio of height to width micro-nano structure provides a mechanical support, limit its motion, strengthen its opposing solvent capillary ability, thereby improve the influence that the surface tension of solvent in the solvent removal process is brought to micro-nano structure.On the large ratio of height to width micro-nano structure, add substrate and may cause some structure, make the solvent that is enclosed in wherein to volatilize, can not finish the removal of solvents process by complete closed.So, make micro-nano structure on the substrate, and when placing, making these structures stride across the figure of those sealings, so just solvent wherein can be taken away, realize removal of solvents.Certainly,, just do not need to make micro-nano structure on the substrate, only need a face to have provided support just if the large ratio of height to width micro-nano structure can not form closed figure.
In the step (1), the selection of manufacture craft should decide according to the character of photoresist.If photoresist and substrate have good adhesion, removing at follow-up secondary solvent can be not destroyed in the technology, just can select photoresist structure as on-chip final structure; Can be destroyed in the technology if photoresist structure is removed at follow-up secondary solvent, just should select to utilize etching technics that photoresist structure is transferred on the substrate again, the micro-nano structure of substrate material is a final structure.
Substrate material, photoresist kind should decide according to the character of the rinsing solvent in the solvent removal process.Because substrate or photoresist are for solvent is guided away from the micro-nano structure of sample, so it must soak into solvent, contact angle is less than 90 °, so that utilize capillarity that solvent is derived.Certainly, also can utilize surface treatment that substrate or photoresist are carried out surface modification, make the contact angle of itself and solvent littler, more help the derivation of solvent.Usually substrate material is quartz, silicon and metal.Photoresist can be ultraviolet or electron beam resist, considers the practicality of technology, selects commercial ultraviolet photoresist usually for use.Solvent is an employed solvent in the previous step wet processing, and kind is a lot, and wherein using more is water and alcohols.
The micro-nano structure that on-chip structure should go up is per sample selected, and guarantee that it can provide mechanical support to the micro-nano structure of sample, can guide the solvent between micro-nano structure again simultaneously.In order to be used in the auxiliary substrate of removing solvent wider applicability is arranged, select periodic structure (as grating) on the substrate usually for use, the cycle is generally from 500 nanometers to 20 micron; For solvent being derived, structure should be a male structure on the substrate, and height is from 100 nanometers to 10 micron, and area is wanted and can fully micro-nano structure on the sample be covered.
The manufacture craft parameter of micro-nano structure on the substrate: spin speed and time, photoresist thickness, etching parameters and etch period etc. are selected according to the process specification of photoresist and etching machine.
Common spin speed is 1000 rev/mins to 4000 rev/mins in the technology, and the spin coating time is 20 seconds to 40 seconds, and the thickness of photoresist is 0.3 micron to 10 microns.
The parameter of common ion beam etching: vacuum 1 * 10-2-2 * 10-2Pa, ion beam current are 40-200mA, etch period 5-50 minute.
In the step (2), when covering on the sample structure with structure on the substrate, should be by adjusting the position of substrate or sample, make that micro-nano structure covers micro-nano structure on the sample fully on the substrate, should make micro-nano structure on the substrate stride across the enclosed construction on the sample simultaneously, guarantee that the solvent on the sample can be derived.
The present invention's advantage compared with prior art is: the present invention has adopted by add the auxiliary method of removing solvent of the substrate that comprises micro-nano structure in the removal of solvents process to provide mechanical support for the micro-nano structure on the sample first, strengthen the capillary ability of its opposing solvent, solved the influence that the surface tension of solvent is brought to micro-nano structure in the solvent removal process effectively; Because the present invention can provide effective mechanical support for a face of micro-nano structure, it can also be applicable to the technical process of removal of solvents in the movable micro-nano structure simultaneously.The inventive method technology is simple, and different micro-nano structures is had applicability preferably, is improving and expanding solvent removal process.
Description of drawings
Fig. 1 is the structural representation among the present invention, and wherein 1 is substrate, and 2 is the large ratio of height to width structure, and 3 is micro-structural on the substrate, and 4 is sample.
The specific embodiment
Below in conjunction with example the auxiliary detailed process of removing solvent method is described in further details:
The auxiliary removal solvent of example 1. quartz construction
(1) on substrate, makes micro-structural
Get the thick quartz substrate of a slice 1mm, be of a size of 5cm * 5cm.Quartz substrate is put into photoresist spinner, drip to go up 1500,3000 rev/mins of photoresist AZ down rotation be coated with 30 seconds, 100 ℃ of bakings are 90 seconds on the hot platform, obtain thickness and be 1.5 microns photoresist layer.Uv-exposure, development, exposure dose are 40mJ/cm
2, the acquisition cycle is 2 microns a optical grating construction.Substrate is put into the ion etching machine carry out etching, etching parameters is: vacuum 1 * 10
-2Pa, CHF
3/ Ar is 1: 1, and ion beam current is 100mA, etch period 20 minutes.Utilize acetone that photoresist is removed, obtaining on substrate highly is the optical grating construction of 300 nanometers;
(2) solvent in the auxiliary removal large ratio of height to width structure
Get a slice finished exposure, include wide be 200 nanometers, highly be one inch silicon chip of 2 microns PMMA (polymethyl methacrylate) large ratio of height to width optical grating construction, this sheet sample is put into methyl iso-butyl ketone (MIBK): isopropyl alcohol is that the solution of 1: 3 (volume ratio) developed 30 seconds, put into isopropyl alcohol and water rinsing then successively, in water, obtain live width and be 200 nanometers, highly be 2 microns PMMA large ratio of height to width optical grating construction.
The silicon chip of finishing rinsing is taken out from water, facing up of large ratio of height to width nanostructured arranged, the substrate that will contain the periodicity micrometer structure then is placed on the silicon chip, makes on-chip optical grating construction cover the nanostructured on the silicon chip.Adjust substrate position, make on the substrate that optical grating construction is perpendicular on the optical grating construction and sample;
(3) treat that water is evaporated completely after, quartz substrate is removed, finish the auxiliary solvent process of removing, obtain live width and be 200 nanometers, highly be 2 microns PMMA large ratio of height to width nanostructured.
The auxiliary removal solvent of example 2.SU8 photoresist structure
(1) on substrate, makes micro-structural
Get the silicon chip of 2 inches of a slices, put into photoresist spinner, drip to go up photoresist SU82010,3000 rev/mins down rotation be coated with 30 seconds, 95 ℃ of bakings are 5 minutes on the hot platform, obtain thickness and be 10 microns photoresist layer.Uv-exposure, development, exposure dose are 140mJ/cm
2, the acquisition cycle is 20 microns a optical grating construction;
(2) solvent in the auxiliary removal large ratio of height to width structure
Get a slice finished exposure, include wide be 20 microns, highly be 2 inches silicon chips of 300 microns SU8 large ratio of height to width structure, putting into developer solution developed 30 minutes, put into the isopropyl alcohol rinsing again, in solution, obtain live width and be 20 microns, highly be 300 microns SU8 large ratio of height to width structure.
The silicon chip of finishing rinsing is taken out from solution, facing up of large ratio of height to width structure arranged, the substrate that will contain the periodicity micrometer structure then is placed on the sample, makes on-chip optical grating construction cover the large ratio of height to width structure on the sample;
(3) treat that solvent evaporates is intact after, silicon chip is removed, finish the auxiliary solvent process of removing, obtain live width and be 20 microns, highly be 300 microns SU8 large ratio of height to width structure.
The auxiliary removal solvent of example 3. silicon chips
(1) on substrate, makes micro-structural
Get the silicon chip of 2 inches of a slices, clean the back oven dry;
(2) solvent in the moving micro-structural of auxiliary deactivation
Get a slice utilized wet etching finish that substrate is removed, include the sample that the cycle is mobilizable golden light grid structure of 2 microns, long 1 centimetre, put into the water rinsing, the acquisition cycle is mobilizable golden light grid structure of 2 microns, long 1 centimetre in the aqueous solution.
The sample of finishing rinsing is taken out from solution, be placed on the silicon chip, make a face of the movable microstructure on the sample contact fully with silicon chip;
(3) treat that water is evaporated completely after, silicon chip is removed, finish the auxiliary solvent process of removing, the acquisition cycle is mobilizable golden light grid structure of 2 microns, long 1 centimetre.
The non-elaborated part of the present invention belongs to general knowledge known in this field.
The above only is a preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (2)
1. method of removing solvent in the micro-nano structure is characterized in that step is as follows:
(1) making micro-nano structure on the substrate: utilize spin coating proceeding spin coating photoresist on substrate, adopt photoetching process on substrate material, to obtain the photoresist structure of desired height then, utilize etching technics that photoresist structure is transferred on the substrate again, obtain the substrate material micro-nano structure of desired height;
(2) sample that will finish rinsing takes out from solvent, and facing up of micro-nano structure arranged on the sample, then substrate is placed on the sample, makes micro-nano structure on the substrate material cover the micro-nano structure on the sample; Or on the contrary substrate is had facing up of micro-nano structure, and then sample is placed on substrate, make micro-nano structure on the substrate material cover the micro-nano structure on the sample;
(3) treat that solvent evaporates is intact after, substrate is removed, finish the auxiliary solvent process of removing, obtain required micro-nano structure; Described substrate or photoresist are wanted and can be soaked into solvent, and contact angle is less than 90 °.
2. a kind of method of removing solvent in the micro-nano structure according to claim 1, it is characterized in that: the micro-nano structure on the described substrate material is for having periodic optical grating construction, cycle is from 500 nanometers to 20 micron, and be male structure, height is from 100 nanometers to 10 micron, and area is wanted and can fully micro-nano structure on the sample be covered.
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| CN102910575B (en) * | 2012-11-09 | 2015-04-08 | 中国电子科技集团公司第三十八研究所 | Manufacture method of polymer nano channel |
| CN104386646B (en) * | 2014-10-15 | 2016-06-22 | 中国科学技术大学 | A kind of method controlling micro-nano structure lodging |
| CN111115563A (en) * | 2019-12-23 | 2020-05-08 | 湖南大学 | Method for stripping functional material by full-dry method |
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| M.P.Stoykovich et al.Deformation of Nanoscopic Polymer Structures in Response to Well-Defined Capillary Forces.《Advanced Materials》.2003,第15卷(第14期),第1180-1184页. * |
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