CN1794086A - Method of covering and patterning nanometer structure on sensitive material surface - Google Patents
Method of covering and patterning nanometer structure on sensitive material surface Download PDFInfo
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- CN1794086A CN1794086A CN 200610023238 CN200610023238A CN1794086A CN 1794086 A CN1794086 A CN 1794086A CN 200610023238 CN200610023238 CN 200610023238 CN 200610023238 A CN200610023238 A CN 200610023238A CN 1794086 A CN1794086 A CN 1794086A
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Abstract
A method for coating pattenized carbonyl nanostructure on photosensitive material surface includes preparing carbon nanotube film, preparing photosensitive material pattern, carrying out intensified gas phase deposit of reaction ion assisted with plasma, etching carbon nanotube by etching gas with physical bombardment and chemical reaction process to decompose carbon nanotube to be carbonyl nanoparticles for forming composite plasma.
Description
Technical field
The present invention relates to the method in a kind of Micrometer-Nanometer Processing Technology field, specifically, relate to a kind of method at photosensitive material surface coverage and patterning nanometer structure.
Technical background
(carbon based nanostructures CNSs) has extensive and unique application to the carbon-based nano structure in micro-nano systems technology, vacuum electronic technology, sensor technology, can be used as electrode material usually and use.The carbon-based nano structure can cover the surface of certain substrate, thereby uses as the specialty films material; Simultaneously, it also can be peeled off from matrix, thereby uses as extraordinary powder body material.Wherein, the method for using as powder still is among the exploitation, and the most ripe technology widely is and the using method of matrix bond as membraneous material, for example on the scene causing in the device, it as the field emission cold-cathode material, also is about to carbon-based nano structure and matrix bond, as membrane electrode.Exist following key technical problem as the carbon-based nano structure of specialty films material is current: the one, this structure structurally is different with matrix, therefore the adhesion problem that has two kinds of structural interface places, the too small meeting of adhesion causes the carbon-based nano structure to break away from substrate under electrostatic forcing, thereby causes device instability and even short circuit to lose efficacy; The 2nd, the growth of this structure is selective to matrix, some matrix, and for example the photosensitive material of widespread use in microelectric technique and micro-nano systems technology is not also developed suitable job operation in its superficial growth carbon-based nano structure; The 3rd, the graphic method of this structure is perfect not enough.The material that this present situation has greatly limited this kind structure extends to more wide application.
Find through literature search prior art, pattern technology field at the carbon-based nano structured material, people such as Young-Rae Cho are in Journal of Vacuum Science and Technology B (vacuum science technology journal B) May/July calendar year 2001, the the 19th (3) volume, the article on the 1012-1015 page or leaf " Patterning technology of carbon nanotubes for field emission display (carbon tube nanometer tube figuring of field-emission display device) ".Article uses the carbon nano-tube slurry that has mixed photosensitive material to carry out the ultraviolet light photoetching development, carbon nano-tube slurry film is carried out graphically, but the minimum positive shape live width that the document is reported is about 30 microns, but pattern edge is very irregular, and minimum negative shape live width is approximately the hundreds of micron, and coarse like this lines can not satisfy request for utilization for micro element.Simultaneously, growth technique as a kind of carbon-based nano structure, find that through literature search also the method for generation of the photosensitive material (photoresist) of widespread use in microelectric technique and micro-nano systems technology surface and patterning nanometer structure does not see open report to prior art.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, a kind of method at photosensitive material surface coverage and patterning nanometer structure is proposed, make photosensitive material (photoresist) surface coverage one deck carbon-based nano structure that it can widespread use in microelectric technique and micro-nano systems technology, and realize the graphical of this structure simultaneously.
The present invention is achieved by the following technical solutions, the present invention at first prepares carbon nano-tube film, prepare the photosensitive material figure then, carry out the reactive ion auxiliary plasma at last and strengthen vapour deposition, promptly use reactive ion auxiliary plasma etching (RIE) technology etching carbon nano-tube film, utilize the composite plasma body that forms to form new carbon-based nano structure simultaneously at the photosensitive material laminar surface.Employed etching gas must be able to rely on physical bombardment, chemical reaction or both combined action etching carbon nano-tube, just carbon nano-tube can be decomposed into the carbon-based nano particle, thereby forms the composite plasma body.
Employed etching gas is in oxygen, fluoride gas and the chloride gas one or more, or the combination of one or more and inert gas in oxygen, fluoride gas and the chloride gas.
When one or several the combination or the combination of one or several and inert gas of fluoride gas during as etching gas of adopting fluoride gas, the yardstick of the carbon-based nano structure that obtains is less, in several nanometers to tens nanometers.
When the combination of adopting oxygen or oxygen and inert gas during as etching gas, the yardstick of the carbon-based nano structure that obtains is bigger, arrives the hundreds of nanometer in tens nanometers.
Described preparation carbon nano-tube film is to form carbon nano-tube film in substrate material surface, forms the method for carbon nano-tube film, is meant the growth in situ method based on chemical vapor deposition, or based on coating, the printing process of carbon nano-tube slurry.
Described preparation photosensitive material figure is to use the described whirl coating of standard microelectronic processing technology, drying glue, exposure, developing process to make photosensitive material layer form figure.
The present invention proposes the photosensitive material surface coverage of widespread use in microelectric technique and micro-nano systems technology and the method for patterning nanometer structure, reactive ion in the use reactive ion auxiliary plasma lithographic technique is to the bombardment and the sputter effect of carbon nano-tube film, in etching cavity, form the composite plasma body that comprises the carbon-based nano particle, this composite plasma knows from experience because plasma enhanced vapor deposition mechanism, and then can form new carbon-based nano structure on the patterned photosensitive material of high precision surface, the experiment proved that, carbon-based nano structure and matrix that this method forms can have good adhesion, good vertical orientated property and density, the consistance of length, simultaneously, its density, length can Be Controlled.The present invention has also realized the graphical of this kind carbon-based nano structure simultaneously, again because photoresist can be graphical accurately in the following magnitude of micron by the whirl coating of microelectronics standard-processing techinque, drying glue, exposure, developing technique, therefore, can form the high-precision figure of this carbon-based nano structure.Owing to use microelectronic processing technology, the present invention is suitable for processing realization array design and produces in batches, and therefore wide application prospect is arranged simultaneously.
Description of drawings
Fig. 1 is the synoptic diagram of the preparation of carbon nano-tube film of the present invention
Fig. 2 is the synoptic diagram of the preparation of photosensitive material figure of the present invention
Fig. 3 is the synoptic diagram that reactive ion auxiliary plasma of the present invention strengthens vapour deposition
Fig. 4 is the field emission microscope photo of the specific embodiment of the invention in the carbon-based nano structure of positive photoresist surface working.
Fig. 5 is the field emission microscope photo of the specific embodiment of the invention in the carbon-based nano structure of SU-8 negative photoresist surface working.
Fig. 6 is the field emission microscope photo of the specific embodiment of the invention in the carbon-based nano structure of positive photoresist surface working.
Fig. 7 is the field emission microscope photo of the specific embodiment of the invention in the carbon-based nano structure of SU-8 negative photoresist surface working.
Embodiment
Provide embodiment below in conjunction with accompanying drawing and technical solution of the present invention:
(1) as shown in Figure 1, the preparation of carbon nano-tube film.Employed substrate is a sandwich construction, wherein, 1 is glass, 2 is 200 nanometer thickness crome metals with the magnetically controlled sputter method deposition, with the carbon nano-tube slurry with 350 order method for printing screen optionally at metallic film 2 surface filmings, baking 20 minutes and cool off in 300 degrees centigrade of heat-treatment furnaces then with stove, obtain the carbon nano-tube material film 3 of 2 microns average thicknesss, the carbon nano-tube slurry is that multi-walled carbon nano-tubes and mass ratio are that 1: 100 the ethyl cellulose and the organic solution of terpinol composition mix.
(2) as shown in Figure 2, the preparation of photosensitive material figure.At metal level 2 and 10 microns positive photoresists 4 of carbon nano-tube film 3 surperficial spin coatings, and successively in 60 degrees centigrade and 90 degrees centigrade of baking ovens fired sample 30 minutes, 90 minutes to solidify photoresist 4; Use chromium plate as mask plate then, with mercury lamp uv-exposure machine exposure 200 seconds, graphical photoresist in developer solution; The photoresist figure that finally obtains is the crossed electrode figure of 3.5 microns of minimum feature.
(3) as shown in Figure 3, the reactive ion auxiliary plasma strengthens vapour deposition.With fluoroform and sulfur hexafluoride (SF
6) with the mixed gas of argon gas be etching gas, flow is respectively 10sccm, 10sccm and 30sccm (standard cubic centimeters per minute), operating air pressure are 80mTorr (milli takes off), power is 40 watts, etching time is 120 seconds.Form carbon-based nano structure 5 on the positive photoresist surface.
3.5 microns of the carbon-based nano structure graph minimum feature that finally obtains are negative shape groove structure, and carbon-based nano body structure surface pattern as shown in Figure 4.As seen from Figure 4, the carbon-based nano structure that generates on the positive photoetching rubber surface, it is the array of the sharp-pointed lance shape nanostructured of a kind of head, the yardstick of each lance shape nanostructured is all in nanometer scale, its most advanced and sophisticated radius-of-curvature is several nanometers, this structure has good vertical orientated property, and uniform Density Distribution is arranged.
(1) as shown in Figure 1, the preparation of carbon nano-tube film.Employed substrate is a sandwich construction, wherein, 1 is glass, 2 is 1 micron thickness Titanium with the magnetically controlled sputter method deposition, with the carbon nano-tube slurry with 250 order method for printing screen optionally at metallic film 2 surface filmings, baking 20 minutes and cool off in 300 degrees centigrade of heat-treatment furnaces then with stove, obtain the carbon nano-tube material film 3 of 3 microns average thicknesss, the carbon nano-tube slurry is that multi-walled carbon nano-tubes and mass ratio are that 1.5: 100 the ethyl cellulose and the organic solution of terpinol composition mix.
(2) as shown in Figure 2, the preparation of photosensitive material figure.At metal level 2 and 10 microns SU-8 types of carbon nano-tube film 3 surperficial spin coatings negative photoresist 4, and successively in 60 degrees centigrade and 90 degrees centigrade of baking ovens fired sample 30 minutes, 120 minutes to solidify photoresist 4; Use chromium plate as mask plate then, after 150 seconds, fired sample is 40 minutes in 90 degree baking ovens with the exposure of mercury lamp uv-exposure machine; Graphical photoresist in developer solution then; The photoresist figure that finally obtains is the miniature arm beam electrode pattern of 5 microns of negative shape minimum feature.
(3) as shown in Figure 3, the reactive ion auxiliary plasma strengthens vapour deposition.With oxygen is etching gas, and flow is 100sccm (standard cubic centimeters per minute), and operating air pressure is 150mTorr (milli takes off), and power is 60 watts, and etching time is 1600 seconds.Form carbon-based nano structure 5 on SU-8 negative photoresist surface.
5 microns of the carbon-based nano structure graph minimum feature that finally obtains are negative shape groove structure, and carbon-based nano body structure surface pattern as shown in Figure 5.As seen from Figure 5, the carbon-based nano structure that generates on SU-8 type negative photoresist surface, it is the array of the sharp-pointed one dimension columnar microstructure of a kind of head, the tip portion of each columnar microstructure is in nanometer scale, and distribution characteristics with ring-type, its length has good vertical orientated property simultaneously in the hundreds of nanometer scale.
(1) as shown in Figure 1, the preparation of carbon nano-tube film.Employed substrate is a sandwich construction, wherein, 1 is glass, 2 is 200 nanometer thickness crome metals with the magnetically controlled sputter method deposition, with the carbon nano-tube slurry with 350 order method for printing screen optionally at metallic film 2 surface filmings, baking 20 minutes and cool off in 300 degrees centigrade of heat-treatment furnaces then with stove, obtain the carbon nano-tube material film 3 of 2 microns average thicknesss, the carbon nano-tube slurry is that multi-walled carbon nano-tubes and mass ratio are that 1: 100 the ethyl cellulose and the organic solution of terpinol composition mix.
(2) as shown in Figure 2, the preparation of photosensitive material figure.At metal level 2 and 10 microns positive photoresists 4 of carbon nano-tube film 3 surperficial spin coatings, and successively in 60 degrees centigrade and 90 degrees centigrade of baking ovens fired sample 30 minutes, 90 minutes to solidify photoresist 4; Use chromium plate as mask plate then, with mercury lamp uv-exposure machine exposure 200 seconds, graphical photoresist in developer solution; The photoresist figure that finally obtains is the crossed electrode figure of 3.5 microns of minimum feature.
(3) as shown in Figure 3, the reactive ion auxiliary plasma strengthens vapour deposition.With oxygen and argon gas is etching gas, and flow is respectively 50 and 5sccm (standard cubic centimeter part clock), and operating air pressure is 80mTorr (milli takes off), and power is 40 watts, and etching time is 90 seconds.Form carbon-based nano structure 5 on the positive photoresist surface.
35 microns of the carbon-based nano structure graph minimum feature that finally obtains are negative shape groove structure, and carbon-based nano body structure surface pattern as shown in Figure 6.As seen from Figure 6, the carbon-based nano structure that generates on the positive photoetching rubber surface, it is a kind of crater array structure, a plurality of single one dimension carbon-based nano structures gatherings form micron-sized loop configuration, and single one dimension carbon-based nano structure is the lance shape, and its most advanced and sophisticated yardstick is all in nanometer scale, its most advanced and sophisticated radius-of-curvature is several nanometers, this structure has good vertical orientated property, and certain electric conductivity is arranged, and uniform Density Distribution is arranged.
(1) as shown in Figure 1, the preparation of carbon nano-tube film.Employed substrate is a sandwich construction, wherein, 1 is glass, 2 are 30 nanometers that successively deposit with magnetically controlled sputter method, the crome metal and the gold thin film of 270 nanometer thickness, with the carbon nano-tube slurry with 150 order method for printing screen optionally at metallic film 2 surface filmings, baking 20 minutes and cool off in 300 degrees centigrade of heat-treatment furnaces then with stove, obtain the carbon nano-tube material film 3 of 4 microns average thicknesss, the carbon nano-tube slurry is that multi-walled carbon nano-tubes and mass ratio are that 3: 100 the ethyl cellulose and the organic solution of terpinol composition mix.
(2) as shown in Figure 2, the preparation of photosensitive material figure.At metal level 2 and 70 microns SU-8 types of carbon nano-tube film 3 surperficial spin coatings negative photoresist 4, and successively in 60 degrees centigrade and 90 degrees centigrade of baking ovens fired sample 30 minutes, 120 minutes to solidify photoresist 4; Use chromium plate as mask plate then, after 330 seconds, fired sample is 40 minutes in 90 degree baking ovens with the exposure of mercury lamp uv-exposure machine; Graphical photoresist in developer solution then; The photoresist figure that finally obtains is the crossed electrode figure of 25 microns of minimum feature.
(3) as shown in Figure 3, the reactive ion auxiliary plasma strengthens vapour deposition.Combination gas with oxygen and argon gas is an etching gas, and flow is respectively 50 and 10sccm (standard cubic centimeters per minute), and operating air pressure is 80mTorr (milli takes off), and power is 40 watts, and etching time is 3000 seconds.Form carbon-based nano structure 5 on SU-8 negative photoresist surface.
25 microns of the carbon-based nano structure graph minimum feature that finally obtains are negative shape groove structure, and carbon-based nano body structure surface pattern as shown in Figure 7.As seen from Figure 7, the carbon-based nano structure that generates on SU-8 type negative photoresist surface, be that a kind of head is comparatively thick and the array of the one dimension columnar microstructure of cluster effect takes place, the tip portion of each columnar microstructure is in the hundreds of nanometer scale, its length has good vertical orientated property simultaneously greater than ten microns.
Claims (6)
1, a kind of method at photosensitive material surface coverage and patterning nanometer structure, it is characterized in that, at first prepare carbon nano-tube film, prepare the photosensitive material figure then, carry out the reactive ion auxiliary plasma at last and strengthen vapour deposition, promptly use reactive ion auxiliary plasma lithographic technique etching carbon nano-tube film, utilize the composite plasma body that forms to form new carbon-based nano structure simultaneously at the photosensitive material laminar surface, employed etching gas, physical bombardment must can be relied on, chemical reaction or both combined action etching carbon nano-tube, promptly carbon nano-tube can be decomposed into the carbon-based nano particle, thereby form the composite plasma body.
2, the method at photosensitive material surface coverage and patterning nanometer structure according to claim 1, it is characterized in that, described preparation carbon nano-tube film, be to form carbon nano-tube film in substrate material surface, form the method for carbon nano-tube film, be meant growth in situ method based on chemical vapor deposition, or based on coating, the printing process of carbon nano-tube slurry.
3, the method at photosensitive material surface coverage and patterning nanometer structure according to claim 1, it is characterized in that, described preparation photosensitive material figure is to use the described whirl coating of standard microelectronic processing technology, drying glue, exposure, developing process to make photosensitive material layer form figure.
4, the method at photosensitive material surface coverage and patterning nanometer structure according to claim 1, it is characterized in that, employed etching gas, be in oxygen, fluoride gas and the chloride gas one or more, or the combination of one or more and inert gas in oxygen, fluoride gas and the chloride gas.
5, according to claim 1 or 4 described methods at photosensitive material surface coverage and patterning nanometer structure, it is characterized in that, when the etching gas that uses as fluoride gas one or several combination or during the combination of one or several and inert gas of fluoride gas, the yardstick of the carbon-based nano structure that obtains in several nanometers to tens nanometers.
6, according to claim 1 or 4 described methods at photosensitive material surface coverage and patterning nanometer structure, it is characterized in that, when the etching gas that uses as the combination of oxygen or oxygen and inert gas during as etching gas, the yardstick of the carbon-based nano structure that obtains in tens nanometers to the hundreds of nanometer.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100594177C (en) * | 2008-06-03 | 2010-03-17 | 北京大学 | Method for preparing carbon nano-tubes by gas induce and products produced thereby |
| CN102530854A (en) * | 2012-01-17 | 2012-07-04 | 上海交通大学 | Method for preparing semiconductor single-walled carbon nanotube by adopting a room-temperature plasma etching method |
| CN104609362A (en) * | 2014-12-26 | 2015-05-13 | 上海维凯光电新材料有限公司 | Preparation method of polymer nanometer ring |
| CN111693906A (en) * | 2020-06-24 | 2020-09-22 | 电子科技大学 | Method for processing Lorentz force magnetic field sensor of silicon-based cavity optical mechanical system |
-
2006
- 2006-01-12 CN CNB2006100232381A patent/CN100543583C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100594177C (en) * | 2008-06-03 | 2010-03-17 | 北京大学 | Method for preparing carbon nano-tubes by gas induce and products produced thereby |
| CN102530854A (en) * | 2012-01-17 | 2012-07-04 | 上海交通大学 | Method for preparing semiconductor single-walled carbon nanotube by adopting a room-temperature plasma etching method |
| CN104609362A (en) * | 2014-12-26 | 2015-05-13 | 上海维凯光电新材料有限公司 | Preparation method of polymer nanometer ring |
| CN111693906A (en) * | 2020-06-24 | 2020-09-22 | 电子科技大学 | Method for processing Lorentz force magnetic field sensor of silicon-based cavity optical mechanical system |
| CN111693906B (en) * | 2020-06-24 | 2022-02-01 | 电子科技大学 | Method for processing Lorentz force magnetic field sensor of silicon-based cavity optical mechanical system |
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