CN103121659A - Method for processing microstructure on highly oriented pyrolytic graphite by using photolithography technique - Google Patents
Method for processing microstructure on highly oriented pyrolytic graphite by using photolithography technique Download PDFInfo
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Abstract
The invention discloses a method for processing a microstructure on highly oriented pyrolytic graphite by using a photolithography technique. The method comprises the following steps: 1, leveling the surface, namely grinding a highly oriented pyrolytic graphite (HOPG) surface by using a grinding machine, and polishing the surface; 2, cleaning the surface; 3, manufacturing a mask of the HOPG; 4, spinning a photoresist to serve as a mask of a SiO2 film or a metal film; 5, photoetching; 6, patterning the HOPG mask; 7, etching the HOPG; 8, removing the photoresist; and 9, removing the HOPG film. The method has the effective effects that the HOPG is directly processed by means of the common photoetching method for micro-electronics and micro-electromechanical systems (MEMS), and the method is mature in process production line, high in cost performance and suitable for directly processing patterns with the characteristic scale of more than 500nm on the HOPG.
Description
Technical field
The present invention relates to photoetching technique, highly oriented pyrolytic graphite (HOPG) be carried out little processing.
Background technology
Have good electric conductivity for using in micro-nano research field, diamagnetism, the HOPG of soft and excellent surface greasy property, a lot of research institutions are all in the how work of little processing HOPG that conducts a research.Find by investigation, present research is all that the method for directly writing with laser, ion beam, electron beam etc. is graphical with HOPG, and this type of processing method economy and time cost are high.
Summary of the invention
The invention provides a kind of introducing photoetching technique, realize the HOPG method for processing microstructure that cost performance is higher.Allow and have good electric conductivity, the HOPG of diamagnetism and soft can directly apply to the MEMS(MEMS) field, and requiring chip integral body to have satisfactory electrical conductivity, diamagnetism, substituting the silica-based MEMS that does not have above performance for particular application such as sound wave LPFs, this patterned HOPG also can be used as the synthetic metal of stay in place form or semiconductor microactuator structure.Simultaneously, the HOPG in the present invention is also a kind of base material of novelty for photoetching technique.
The present invention is achieved by the following technical solutions, and the method with photoetching process processing micro structure on highly oriented pyrolytic graphite comprises the following steps:
Step 1: surfacing, use grinder to grind the HOPG surface, to its polishing.
Step 2: surface clean
Ultrasonic wave specification during ultrasonic cleaning is: adopt the frequency of 20,000 hertz to 200,000 hertz, every premium on currency is not less than the power of 30w.First HOPG is soaked in pure water, ultrasonic cleaning is not less than 5 minutes, and most of particle contamination and other parts that can remove in the surfacing process are polluted; Then HOPG is soaked in successively in two kinds of liquid of acetone and ethanol, ultrasonic cleaning is not less than 5 minutes, is mainly used in removing organic contamination, washes to be not less than 1 minute with pure water rinsing afterwards; Then hydrogen peroxide, hydrochloric acid and pure water are prepared washing lotion according to volume ratio 1:1:6～1:2:50,50 ℃ to 80 ℃ of heating-up temperature scopes are cleaned HOPG and are not less than 5 minutes, can remove most of metal ion; Be not less than 1 minute with pure water rinsing at last and drying;
Step 3: the mask of making HOPG:
Deposit one deck SiO on the HOPG after surfacing and cleaning
2Film or metallic film are as the mask of HOPG;
Step 4: gluing:
The uniform photoresist of spin coating a layer thickness is as SiO on substrate
2The mask of film or metallic film;
Step 5: photoetching: comprise soft baking, exposure, post exposure bake, development, post bake;
Step 6: the mask of graphical HOPG:
If the mask of HOPG is silica, can use hydrofluoric acid or potassium hydroxide, concentrated ammonia liquor wet etching pattern mask layer, perhaps use fluorine sulfide as the method pattern mask layer of reacting gas etching; If the mask of HOPG is metal, according to can corroding metal but can not dissolve the suitable corrosive liquid pattern mask layer of principle preparation of photoresist and graphite;
Step 7: etching HOPG:
With MEMS industry various dry etching equipments commonly used, comprise that drum type brake, flat, following current plasma, planar tripolar, reactive ion etching (RIE), deep reaction ion etching (DRIE), electron cyclotron accelerate concussion (ECR), distributed ECR, inductively coupled plasma etching (ICP) or magnetic intensified response ion etching (MERIE) and other dry etching equipment, use oxygen or fluorocarbon gases etching HOPG, go out to have the micro-structural of design configuration in the HOPG Surface Machining;
Step 8: remove photoresist
After etching finishes, to soak with acetone, residual photoresist is removed in ultrasonic cleaning; Need complete immediately the operation of this step after completing for the 7th step, occur otherwise may there be photoresist to remove incomplete situation; With this technique remove photoresist simple to operate, with low cost, remove fully, can avoid the physics and chemistry destruction of removing photoresist that mechanical-physical that the HOPG micro-structural is caused destroys and the HOPG micro-structural being caused with oxygen gas plasma stripping with machinery;
Step 9: the mask of removing HOPG
Use the operation the same with the 6th step to remove the mask of residual HOPG, obtain the HOPG that the surface has the micro-structural of design configuration.
Effective effect of the present invention is: use for reference microelectronics and MEMS photoetching method commonly used and directly HOPG is processed, the production line of the method is ripe, and cost performance is higher, is adapted at directly processing on HOPG characteristic dimension greater than the figure of 500 nanometers.
Description of drawings:
Fig. 1 implements in 1 with photoetching process processing micro structure method schematic diagram on highly oriented pyrolytic graphite;
Fig. 2 implements in 2 with photoetching process processing micro structure method schematic diagram on highly oriented pyrolytic graphite;
Fig. 3 implements in 3 with photoetching process processing micro structure method schematic diagram on highly oriented pyrolytic graphite;
Fig. 4 implements in 4 with photoetching process processing micro structure method schematic diagram on highly oriented pyrolytic graphite;
Concrete embodiment:
Embodiment 1:
Comprise the steps: with photoetching process processing micro structure method on highly oriented pyrolytic graphite in the present embodiment
Step 1: surfacing
Use the chemical mechanical grinder attenuate and grinding HOPG surface of CETR board CP-4, adjust the depth of parallelism of thickness and the assurance upper and lower surface of HOPG, then to its polishing.
Step 2: surface clean
Ultrasonic wave specification during ultrasonic cleaning is: adopt the frequency of 20,000 hertz, and the power of every premium on currency 30w, Hereinafter the same.First HOPG is soaked in ultra-pure water ultrasonic cleaning 10 minutes; Then HOPG successively is soaked in two kinds of liquid of acetone and ethanol, used successively ultrasonic cleaning 5 minutes, wash rear ultra-pure water 1 minute of using; Then hydrogen peroxide, hydrochloric acid and ultra-pure water are prepared washing lotion according to volume ratio 1:2:9, be heated to 80 ℃ and cleaned HOPG approximately 5 minutes; Rinse with ultra-pure water at last and be not less than 1 minute and drying.
The ultra-pure water of this patent indication is to adopt multistage filtering, the counter-infiltration of high-performance ion-exchange unit, the processing of ultrapureization of ultra filtration filter, with uviol lamp, the water of the based on very high purity that almost there is no impurity and ion except the multiple processing method rear class such as organic carbon device after processing, its resistivity can surpass 15M Ω cm in use at last
Step 3: the mask of making HOPG
In surfacing with the about Cu film of 200 nanometers of the method deposit a layer thickness that adopts magnetron sputtering on the HOPG after cleaning;
Step 4: gluing
On the Cu of HOPG film, with rotating speed spin coating one deck of 3000rpm approximately the BP212-37 eurymeric photoresist of 2 micron thickness as the mask of HOPG;
Step 5: photoetching
First be heated to 110 degrees centigrade on hot plate, soft baking 60 seconds; Then do the exposure mask version with the glass plate of chromium plating, with the ultraviolet ray of wavelength 365 nanometers, at exposure intensity 7.5mw/cm
2Condition under, 15 seconds time for exposure; Then be heated to 110 degrees centigrade on hot plate, carried out post exposure bake 60 seconds; Then be that 0.5% KOH solution developed 30 seconds with regard to the service property (quality) mark; Be heated at last 110 degrees centigrade on hot plate, post bake 360 seconds.
Step 6: the mask of graphical HOPG
Red fuming nitric acid (RFNA) and ultra-pure water that commodity in use is analyzed pure level configure the approximately dilute nitric acid solution of 5mol/L, in approximately corrosion approximately after 20 seconds under 20 ℃ of normal temperature, whether the red copper that detects by an unaided eye disappears, with can present silver gray even the method on the surface of the HOPG of black confirm whether the Cu film is etched fully, this kind method generally can make live width slightly increase, but technique is simple, with low cost.
Step 7: etching
With oxygen etching HOPG, can process micro-structural on HOPG the ICP etching machine;
Step 8: remove photoresist
Soak ultrasonic removal residual photoresist with acetone.This method process costs is simple, with low cost, can avoid removing photoresist with machinery the mechanical-physical of HOPG micro-structural is destroyed and with the chemical depletion of oxygen gas plasma stripping to the HOPG micro-structural;
Step 9: the mask of removing HOPG
Commodity in use is analyzed the approximately dilute nitric acid solution of 5mol/L of the red fuming nitric acid (RFNA) of pure level and ultra-pure water configuration, and the redness that approximately is dipped to the surface at normal temperature under 20 ℃ disappears fully.
Comprise the steps: with photoetching process processing micro structure method on highly oriented pyrolytic graphite in the present embodiment
Use the chemical mechanical grinder attenuate of CETR board CP-4 and grind the HOPG surface, tested the thickness of HOPG every 5 minutes, and note guaranteeing the depth of parallelism of its upper and lower surface, then to its polishing.
Ultrasonic wave specification during ultrasonic cleaning is: adopt the frequency of 20,000 hertz, and the power of every premium on currency 30w, Hereinafter the same.First HOPG is soaked in ultra-pure water (in this patent to the description of ultra-pure water for details, see the appendix 1) ultrasonic cleaning 10 minutes; Then HOPG successively is soaked in two kinds of liquid of acetone and ethanol, used successively ultrasonic cleaning 5 minutes, wash rear ultra-pure water 1 minute of using; Then hydrogen peroxide, hydrochloric acid and ultra-pure water are prepared washing lotion according to volume ratio 1:2:9, be heated to 80 ℃ and cleaned HOPG approximately 5 minutes; Rinse with ultra-pure water at last and be not less than 1 minute and drying.
In surfacing with the about SiO of 300 nanometers of the method deposit a layer thickness that adopts LPCVD on the HOPG after cleaning
2Film, 330 ° of temperature are because HOPG also can react with oxygen, so consider to use lower reaction temperature, flatness and the smoothness on heavy damage HOPG surface when avoiding deposit;
SiO at HOPG
2On film, with rotating speed spin coating one deck of 200rpm approximately the SU-8 negative photoresist of 200 micron thickness as the mask of HOPG;
First be heated to 90 degrees centigrade on hot plate, soft baking 30 minutes; Then do the exposure mask version with the glass plate of chromium plating, with the ultraviolet ray of wavelength 365 nanometers, exposure intensity 7.5mw/cm
2, 5 minutes time for exposure; Then be heated to 95 degrees centigrade on hot plate, carried out post exposure bake 30 minutes; Then just use the PGMEA(electronic grade propylene glycol methyl ether acetate) developed 20 minutes; Be heated at last 95 degrees centigrade on hot plate, post bake 30 minutes.
Use the carbon tetrafluoride gas etching in the ICP etching machine, the silica membrane above HOPG can be processed micrographics, during with the earth silicon mask of the graphical HOPG of this method, live width keeps better, without obviously enlarging;
Used the ICP etching machine on the basis in upper step, directly be filled with oxygen etching HOPG, can process micro-structural on HOPG;
First soak with acetone, then ultrasonic softening photoresist uses special-purpose SU-8 glue-dispenser to remove residual photoresist.This method process costs is simple, with low cost, can avoid removing photoresist with machinery the mechanical-physical of HOPG micro-structural is destroyed and with the chemical depletion of oxygen gas plasma stripping to the HOPG micro-structural;
The HF solution of the pure level of commodity in use analysis and ultra-pure water are made into etching liquid, soak at room temperature 10 minutes according to the ratio of volume ratio 1:10.
Comprise the steps: with photoetching process processing micro structure method on highly oriented pyrolytic graphite in the present embodiment
Use the chemical mechanical grinder attenuate and grinding HOPG surface of CETR board CP-4, adjust the depth of parallelism of thickness and the assurance upper and lower surface of HOPG, then to its polishing.
Ultrasonic wave specification during ultrasonic cleaning is: adopt the frequency of 20,000 hertz, and the power of every premium on currency 30w, Hereinafter the same.First HOPG is soaked in ultra-pure water (in this patent to the description of ultra-pure water for details, see the appendix 1) ultrasonic cleaning 10 minutes; Then HOPG successively is soaked in two kinds of liquid of acetone and ethanol, used successively ultrasonic cleaning 5 minutes, wash rear ultra-pure water 1 minute of using; Then hydrogen peroxide, hydrochloric acid and ultra-pure water are prepared washing lotion according to volume ratio 1:2:9, be heated to 80 ℃ and cleaned HOPG approximately 5 minutes; Rinse with ultra-pure water at last and be not less than 1 minute and drying.
In surfacing with the about Al film of 200 nanometers of the method deposit a layer thickness that adopts magnetron sputtering on the HOPG after cleaning;
On the Al of HOPG film, with rotating speed spin coating one deck of 3000rpm approximately the BP212-37 eurymeric photoresist of 2 micron thickness as the mask of HOPG;
First be heated to 110 degrees centigrade on hot plate, soft baking 60 seconds; Then do the exposure mask version with the glass plate of chromium plating, with the ultraviolet ray of wavelength 365 nanometers, exposure intensity 7.5mw/cm
2, 15 seconds time for exposure; Then be heated to 110 degrees centigrade on hot plate, carried out post exposure bake 60 seconds; Then be that 0.5% KOH solution developed 30 seconds with regard to the service property (quality) mark; Be heated at last 110 degrees centigrade on hot plate, post bake 360 seconds.
Concentrated hydrochloric acid and ultra-pure water that commodity in use is analyzed pure level configure the approximately dilute hydrochloric acid solution of 3mol/L, in approximately corrosion approximately after 20 seconds under 20 ℃ of normal temperature, whether the argenteous aluminium that detects by an unaided eye disappears, with can present silver gray even the method on the surface of the HOPG of black confirm whether the Al film is etched fully, this kind method generally can make live width slightly increase, but technique is simple, with low cost.
With oxygen etching HOPG, can process micro-structural on HOPG the ICP etching machine
Soak ultrasonic removal residual photoresist with acetone.This method process costs is simple, with low cost, can avoid removing photoresist with machinery the mechanical-physical of HOPG micro-structural is destroyed and with the chemical depletion of oxygen gas plasma stripping to the HOPG micro-structural;
Commodity in use is analyzed the approximately dilute hydrochloric acid solution of 3mol/L of the concentrated hydrochloric acid of pure level and ultra-pure water configuration, and the silvery white that approximately is dipped to the surface at normal temperature under 20 ℃ disappears fully.
Comprise the steps: with photoetching process processing micro structure method on highly oriented pyrolytic graphite in the present embodiment
Use the chemical mechanical grinder attenuate and grinding HOPG surface of CETR board CP-4, adjust the depth of parallelism of thickness and the assurance upper and lower surface of HOPG, then to its polishing.
Ultrasonic wave specification during ultrasonic cleaning is: adopt the frequency of 20,000 hertz, and the power of every premium on currency 30w, Hereinafter the same.First HOPG is soaked in ultra-pure water ultrasonic cleaning 10 minutes; Then HOPG is soaked in two kinds of liquid of acetone and ethanol, used successively ultrasonic cleaning 5 minutes, wash rear ultra-pure water 1 minute of using; Then hydrogen peroxide, hydrochloric acid and ultra-pure water are prepared washing lotion according to volume ratio 1:2:9, be heated to 80 ℃ and cleaned HOPG approximately 5 minutes; Rinse with ultra-pure water at last and be not less than 1 minute and drying.
In surfacing with the about Ag film of 200 nanometers of the method deposit a layer thickness that adopts magnetron sputtering on the HOPG after cleaning;
On the Ag of HOPG film, with rotating speed spin coating one deck of 3000rpm approximately the BP212-37 eurymeric photoresist of 2 micron thickness as the mask of HOPG;
First be heated to 110 degrees centigrade on hot plate, soft baking 60 seconds; Then do the exposure mask version with the glass plate of chromium plating, with the ultraviolet ray of wavelength 365 nanometers, exposure intensity 7.5mw/cm
2, 15 seconds time for exposure; Then be heated to 110 degrees centigrade on hot plate, carried out post exposure bake 60 seconds; Then be that 0.5% KOH solution developed 30 seconds with regard to the service property (quality) mark; Be heated at last 110 degrees centigrade on hot plate, post bake 360 seconds.
Red fuming nitric acid (RFNA) and ultra-pure water that commodity in use is analyzed pure level configure the approximately dilute nitric acid solution of 6mol/L, in approximately corrosion approximately after 20 seconds under 20 ℃ of normal temperature, whether the argenteous silver that detects by an unaided eye disappears, with can present silver gray even the method on the surface of the HOPG of black confirm whether the Ag film is etched fully, this kind method generally can make live width slightly increase, but technique is simple, with low cost.
With oxygen etching HOPG, can process micro-structural on HOPG the ICP etching machine;
Soak ultrasonic removal residual photoresist with acetone.This method process costs is simple, with low cost, can avoid with machinery remove photoresist to the mechanical-physical of HOPG micro-structural destroy and with oxygen gas plasma stripping to the HOPG micro-structural chemical depletion;
Commodity in use is analyzed the approximately dilute nitric acid solution of 6mol/L of the red fuming nitric acid (RFNA) of pure level and ultra-pure water configuration, and the silvery white that approximately is dipped to the surface at normal temperature under 20 ℃ disappears fully.
Claims (3)
1. with the method for photoetching process processing micro structure on highly oriented pyrolytic graphite, it is characterized in that, comprise the following steps:
Step 1: surfacing, use grinder to grind the HOPG surface, to its polishing;
Step 2: surface clean;
Step 3: deposit one deck SiO
2Film or metallic film are as the mask of HOPG;
Step 4: gluing, the uniform photoresist of spin coating a layer thickness is as SiO
2The mask of film or metallic film;
Step 5: photoetching;
Step 6: the mask of graphical HOPG:
If the mask of HOPG is silica, use hydrofluoric acid or potassium hydroxide, concentrated ammonia liquor wet etching pattern mask layer, perhaps use fluorine sulfide as the method pattern mask layer of reacting gas etching; If the mask of HOPG is metal, according to can corroding metal but can not dissolve the suitable corrosive liquid pattern mask layer of principle preparation of photoresist and graphite;
Step 7: dry etching HOPG:
Step 8: remove photoresist:
After etching finishes, to soak with acetone, residual photoresist is removed in ultrasonic cleaning;
Step 9: the mask of removing HOPG: use the operation the same with the 6th step to remove the mask of residual HOPG, obtain the HOPG that the surface has the micro-structural of design configuration.
2. the method with photoetching process processing micro structure on highly oriented pyrolytic graphite as claimed in claim 1, it is characterized in that, in described step 2, the process of surface clean is: first HOPG is soaked in pure water, adopt the frequency of 20,000 hertz to 200,000 hertz, every premium on currency is not less than the power of 30w, and ultrasonic cleaning is not less than 5 minutes; Then HOPG is soaked in successively in two kinds of liquid of acetone and ethanol, ultrasonic cleaning is not less than 5 minutes, washes to be not less than 1 minute with pure water rinsing afterwards; Then hydrogen peroxide, hydrochloric acid and pure water are prepared washing lotion according to volume ratio 1:1:6～1:2:50,50 ℃ to 80 ℃ of heating-up temperature scopes are cleaned HOPG and are not less than 5 minutes; Be not less than 1 minute with pure water rinsing at last and drying.
3. the method with photoetching process processing micro structure on highly oriented pyrolytic graphite as claimed in claim 1, it is characterized in that, in described step 7, the detailed process of dry etching HOPG is: with MEMS industry various dry etching equipments commonly used, comprise drum type brake, flat, the following current plasma, planar tripolar, reactive ion etching (RIE), deep reaction ion etching (DRIE), electron cyclotron accelerates concussion (ECR), distributed ECR, inductively coupled plasma etching (ICP) or magnetic intensified response ion etching (MERIE) and other dry etching equipment, use oxygen or fluorocarbon gases etching HOPG, go out to have the micro-structural of design configuration in the HOPG Surface Machining.
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Cited By (7)
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| CN105675684A (en) * | 2016-03-16 | 2016-06-15 | 临沂大学 | Preparation method of multi-hole-height oriented pyrolytic graphite electrode with hole diameter controllable |
| CN107665810A (en) * | 2017-09-11 | 2018-02-06 | 中国科学院微电子研究所 | The stripping means of nano-grade size photoresist on a kind of semiconductor |
| CN107857234A (en) * | 2017-11-01 | 2018-03-30 | 西安交通大学 | A kind of ecr ion lithography Surface Texture simultaneously accurately controls texture measures |
| CN108892099A (en) * | 2018-06-25 | 2018-11-27 | 武汉大学 | A method of coining ultra-thin materials prepare uniform outer surface micro-structure |
| CN109827700A (en) * | 2019-03-04 | 2019-05-31 | 温州大学 | A kind of double-disk graphite-based pressure resistance type pliable pressure sensor and its manufacture craft |
| CN113788452A (en) * | 2021-08-31 | 2021-12-14 | 上海交通大学 | Processing method of fine micro-nano glass structure |
| WO2022000120A1 (en) * | 2020-06-28 | 2022-01-06 | 深圳清华大学研究院 | Manufacturing method for graphite island sliding block arrays |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105675684A (en) * | 2016-03-16 | 2016-06-15 | 临沂大学 | Preparation method of multi-hole-height oriented pyrolytic graphite electrode with hole diameter controllable |
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| CN107857234A (en) * | 2017-11-01 | 2018-03-30 | 西安交通大学 | A kind of ecr ion lithography Surface Texture simultaneously accurately controls texture measures |
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| CN108892099A (en) * | 2018-06-25 | 2018-11-27 | 武汉大学 | A method of coining ultra-thin materials prepare uniform outer surface micro-structure |
| CN109827700A (en) * | 2019-03-04 | 2019-05-31 | 温州大学 | A kind of double-disk graphite-based pressure resistance type pliable pressure sensor and its manufacture craft |
| WO2022000120A1 (en) * | 2020-06-28 | 2022-01-06 | 深圳清华大学研究院 | Manufacturing method for graphite island sliding block arrays |
| CN113788452A (en) * | 2021-08-31 | 2021-12-14 | 上海交通大学 | Processing method of fine micro-nano glass structure |
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Application publication date: 20130529 |