CN103496664A - Method for manufacturing self-support polymer structure with large depth-width ratio - Google Patents
Method for manufacturing self-support polymer structure with large depth-width ratio Download PDFInfo
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- CN103496664A CN103496664A CN201310474535.8A CN201310474535A CN103496664A CN 103496664 A CN103496664 A CN 103496664A CN 201310474535 A CN201310474535 A CN 201310474535A CN 103496664 A CN103496664 A CN 103496664A
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Abstract
The invention discloses a method for manufacturing a self-support polymer structure with a large depth-width ratio. The method comprises the following steps: first, manufacturing a polymer-film or metal-film sacrificial layer on a substrate; then, coating a layer of photoresist on the sacrificial layer to manufacture a microstructure with large depth-width ratio; finally removing the sacrificial layer to obtain the self-support polymer structure with the large depth-width ratio. The method has the beneficial effects that the technical problem that the substrate and the microstructure are not easily stripped in the prior art is solved as the auxiliary sacrificial layer is added between the substrate and the microstructure, and the yield of device is greatly increased. Meanwhile, the method for removing the sacrificial layer is simple, has a low cost, and has an important meaning for effective expansion of a micro-nano processing technology.
Description
Technical field
The present invention relates to the making of polymer architecture in the MEMS device, in particular a kind of preparation method of self-supporting large ratio of height to width polymer architecture.
Background technology
The SU8 negative photoresist is a kind of thick glue of ultraviolet band sensitization, there is mechanical performance, optical characteristics, anticorrosive and heat endurance preferably, be widely used in micro-fluid chip, biochip, micro-optical device, polymeric molds and large ratio of height to width micro-structural etc., become one of important materials of MEMS (MEMS) and related device.Continuous progress along with science and technology, people are more and more stronger to the cognitive desire of microcosmos, in addition, and the diversity of biology and material, traditional method filter separation method can not meet the demands, and the MEMS processing method is that microorganism and material etc. have been carried a kind of good discrete device.
SU8 has biocompatibility preferably, and the SU8 material is after ultraviolet lighting, and heated baking makes its molecule hinge, and material has mechanical performance preferably.The viscosity of SU8 negative photoresist material own is larger, can obtain thicker film, with positive photoresist, compares, and mechanical strength is good, and its elastic modelling quantity is about 4GPa, is difficult for flexural deformation.Along with the fast development of micro-nano process technology, the performance of a lot of micro-nano devices is affected by the depth-width ratio of its structure.The large ratio of height to width micro-nano device, as optics, inertia device and high energy diagnostic device have application comparatively widely in various fields, device performance is widely used it preferably.The SU8 negative photoresist can obtain the film of thickness range from several microns to the hundreds of micron by regulating viscosity and spin coating rotating speed, is the preferential selection that the micro-nano manufacture field is made large ratio of height to width micro-nano structure and device, micro-fluid chip for example, biological cell cultivation etc.But SU8 negative photoresist and substrate after hinge have adhesion preferably, therefore, how to realize discharging photoresist structure from substrate, obtain complete structure or device, be to fail the difficult problem overcome in prior art always.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of self-supporting large ratio of height to width polymer architecture is provided, it is simple that purpose is to provide a kind of technique, and method with low cost realizes discharging photoresist from substrate, obtains complete polymer architecture.
The present invention is achieved by the following technical solutions:
A kind of preparation method of self-supporting large ratio of height to width polymer architecture comprises the following steps:
(1) make sacrifice layer on substrate:
Clean substrate, steam is removed in baking, and after naturally cooling to room temperature, coated polymer film or depositing metal films on substrate, as sacrifice layer;
(2) make the large ratio of height to width micro-structural:
On the described sacrifice layer of step (1), apply photoresist, baking, remove the solvent of photoresist inside, after naturally cooling to room temperature, photoresist exposed, and develops, and finally cleans, and obtains the large ratio of height to width micro-structural;
(3) remove sacrifice layer:
The large ratio of height to width micro-structural that step (2) is obtained is placed in thin polymer film lysate or metal erosion liquid, removes sacrifice layer, obtains self-supporting large ratio of height to width polymer architecture.
Preferably, in described step (1), the method for cleaning substrate is: at first the acetone ultrasonic cleaning is 5 minutes, then uses the alcohol ultrasonic cleaning 5 minutes, last deionized water ultrasonic cleaning 5 minutes.
Preferably, in described step (1), the temperature of baking is 150 ℃, and the time of baking is 20 minutes.
Preferably, in described step (1), before the coated polymer film, first by the oxygen rie technology, cooled substrate surface is carried out to modification, coated polymer film again, the oxygen flow of described oxygen rie technology is 30sccm, the reaction time is 10 seconds, radio-frequency power is 40 watts, because the viscosity of photoresist own is larger, poor fluidity, adopt the oxygen rie technology to carry out modification to substrate surface, can improve the wellability of substrate and sacrifice layer, prevent that bubble from appearring in the coating procedure median surface.
Preferably, in described step (1), the material of thin polymer film is polymetylmethacrylate, and coating processes is for revolving Tu technique, and coating thickness is 200～300 nanometers, and described step of revolving Tu technique comprises:
1) revolve Tu PMMA on substrate, the spin coating rotating speed is 500～2000 revolutions per seconds;
2) baking, solidify PMMA, and described baking temperature is 180 ℃, and baking time is 90 seconds.
Preferably, in described step (1), the method for depositing metal films is the ion beam sputter depositing method, and the chamber vacuum degree of described ion beam sputter depositing method is 1.0 * 10
-3～1.3 * 10
-3pa, the ion beam line is 70～80mA, and sedimentation time is 10～15 minutes, and deposit thickness is 200～300 nanometers.
Preferably, in described step (2), photoresist is the SU8 photoresist, and the revolution of coating is 500～2000 revolutions per seconds, and the time of coating is 10～60 seconds, and the thickness of coating is 100～150 microns.
Preferably, in described step (2), the method for baking is: in temperature, be at first to toast 5 minutes under 65 ℃, then be warming up to 95 ℃, toast 20 minutes, the speed of described intensification is 5 ℃/min.
Preferably, in described step (2), adopt the ultraviolet photolithographic technology to be exposed to photoresist, develop, described exposure dose is 150～200J/cm
2the method of described development is: at first baking 3 minutes under 65 ℃, then be warming up to 95 ℃ of bakings 15 minutes, and the speed of described intensification is 5 ℃/min, be placed in again 1-Methoxy-2-propyl acetate PGMEA and develop 10～15 minutes, finally be placed in isopropyl alcohol IPA and clean 5 minutes.
Preferably, in described step (3), the thin polymer film lysate is organic solvent, and the dissolution time of lysate is 5～10min, after dissolving, uses washed with de-ionized water, and nitrogen dries up; Metal erosion liquid is the ferric chloride solution that mass concentration is 0.5%, and the etching time of corrosive liquid is 3～5 minutes, uses successively IPA and washed with de-ionized water after corrosion, and nitrogen dries up.
Principle of the present invention is: at first at treated substrate surface deposition layer of metal film or spin coating one layer of polymeric film, for self-supporting large ratio of height to width structure provides sacrifice layer; Then apply one deck photoresist on the metallic film obtained or thin polymer film, obtain the large ratio of height to width polymer micro-structural; Finally by the method for wet etching (corrosion of thin polymer film lysate) or organic solvent dissolution, remove sacrifice layer, obtain self-supporting large ratio of height to width polymer architecture.
The present invention has the following advantages compared to existing technology: the preparation method that the invention provides a kind of self-supporting large ratio of height to width polymer, the method by adding auxiliary sacrifice layer between substrate and micro-structural, overcome the technical problem that is difficult for peeling off between substrate and micro-structural in the prior art, greatly improved the yield of device, simultaneously, the method of removal sacrifice layer provided by the invention is simple, and cost is low, and effective expansion of micro-nano processing technology is had to important meaning.
The accompanying drawing explanation
Fig. 1 makes the schematic diagram of sacrifice layer on substrate;
Fig. 2 applies the schematic diagram of photoresist on sacrifice layer;
Fig. 3 is the schematic diagram that utilizes the ultraviolet photolithographic method to be exposed to photoresist;
Fig. 4 is for making the schematic diagram of the large ratio of height to width micro-structural obtained;
Fig. 5 is for removing the schematic diagram of the self-supporting large ratio of height to width polymer architecture obtained after sacrifice layer.
The specific embodiment
Below embodiments of the invention are elaborated, the present embodiment is implemented take technical solution of the present invention under prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
The making flow chart that Fig. 1～Fig. 5 is the present embodiment comprises the following steps:
1, make sacrifice layer on substrate:
At first, get a slice silicon chip 1 as substrate, be placed in the acetone soln ultrasonic cleaning 5 minutes, the remaining acetone of deionized water rinsing, nitrogen dries up, and then is placed in the alcoholic solution ultrasonic cleaning 5 minutes, the deionized water rinsing residual alcohol, nitrogen dries up, then is placed in deionized water for ultrasonic cleaning 5 minutes, and nitrogen dries up;
Then, silicon chip 1 is placed on the hot platform of 150 ℃ to baking 20 minutes, removes the steam in cleaning process;
Finally, the copper metal film that is 200 nanometers in silicon chip 1 surface deposition a layer thickness by the ion beam sputter depositing method, the energy of described ion beam sputtering is 400eV, and the ion beam line is 80mA, and the chamber vacuum degree is 1.0 * 10
-3pa, sedimentation time is 15 minutes, after having deposited, obtains copper sacrificial metal layer 2 as shown in Figure 1.
2, make the large ratio of height to width micro-structural:
At first, on copper sacrificial metal layer 2, the method that Tu technique is revolved in utilization applies one deck SU82100 photoresist 3, then is placed in baking oven and toasts, and removes the solvent in photoresist 3, in temperature, be to toast 3 minutes under 65 ℃, then be warming up to 95 ℃, toast 20 minutes, the speed wherein heated up is 5 ℃/min, naturally cool to room temperature, obtain structure as shown in Figure 2;
Then, as shown in Figure 3, by the ultraviolet photolithographic method, SU82100 photoresist 3 is exposed, wherein 4 is photo etched mask, and described exposure adopts the i line passage contact exposure that wavelength is 365 nanometers, and exposure dose is 200J/cm
2, after exposure, be placed in baking oven and toast, make silicon chip 1 and SU82100 photoresist 3 hinges.Be to toast 5min under 65 ℃ in temperature, then be warming up to 95 ℃, toast 15 minutes, the speed wherein heated up is 5 ℃/min, naturally cools to room temperature;
Finally, the total after baking is placed in to PGMEA solution, develops 15 minutes, then be placed in IPA cleaning 5 minutes, nitrogen dries up, and obtains structure as shown in Figure 4, is the large ratio of height to width micro-structural.
3, remove sacrifice layer:
The above-mentioned micro-structural that obtains is placed in to the ferric chloride solution that mass percent is 0.5%, corrode 10 minutes, remove sacrifice layer, make the SU82100 photoresist 3 in micro-structural separate with substrate 1, as shown in Figure 5, obtain self-supporting large ratio of height to width polymer architecture, finally, described self-supporting large ratio of height to width polymer architecture is taken out from solution, after washed with de-ionized water, dry up with nitrogen.
In the present embodiment, while using the sacrifice layer 2 of ion beam sputter depositing method deposited copper metallic film, the chamber vacuum degree of ion beam sputter depositing is 1.3 * 10
-3pa, the ion beam line is 70mA, and sedimentation time is 10 minutes, and deposit thickness is 300 nanometers; Exposure dose photoresist 3 exposed by the ultraviolet photolithographic method is 150J/cm
2, developing time is 10 minutes; The ferric chloride solution that is 0.5% by mass percent is removed the sacrifice layer 2 of copper metal film, and etching time is 5 minutes, and other step is with embodiment 1.
In the present embodiment, sacrifice layer 2 material selection polymer P MMA, utilize mechanical method of revolving Tu to be coated on the surface of silicon substrate 1, the thickness applied is 200 nanometers, the rotating speed that revolves Tu is 2000 rev/mins, and then baking is solidified polymer P MMA, and described baking temperature is 180 ℃, baking time is 90 seconds, and described PMMA selects PMMA950K.
The method of removing sacrifice layer is: the micro-structural obtained is placed in to acetone, PMMA is dissolved in acetone, corrode 5 minutes, then take out from acetone, use successively IPA and washed with de-ionized water, nitrogen dries up, and obtains self-supporting large ratio of height to width polymer architecture.
Other step is with embodiment 1.
Embodiment 4
In the present embodiment, sacrifice layer 2 material selection polymer P MMA, the coating thickness that utilizes machinery to revolve the Tu method is 300 nanometers, revolving the Tu rotating speed is 500 revolutions per seconds; While removing sacrifice layer, the time of acetone corrosion is 3 minutes, and other step is with embodiment 3.
Claims (10)
1. the preparation method of a self-supporting large ratio of height to width polymer architecture, is characterized in that, comprises the following steps:
(1) make sacrifice layer on substrate:
Clean substrate, steam is removed in baking, and after naturally cooling to room temperature, coated polymer film or depositing metal films on substrate, as sacrifice layer;
(2) make the large ratio of height to width micro-structural:
On the described sacrifice layer of step (1), apply photoresist, baking, remove the solvent of photoresist inside, after naturally cooling to room temperature, photoresist exposed, and develops, and finally cleans, and obtains the large ratio of height to width micro-structural;
(3) remove sacrifice layer:
The large ratio of height to width micro-structural that step (2) is obtained is placed in thin polymer film lysate or metal erosion liquid, removes sacrifice layer, obtains self-supporting large ratio of height to width polymer architecture.
2. the preparation method of a kind of self-supporting large ratio of height to width polymer architecture as claimed in claim 1, it is characterized in that, in described step (1), the method for cleaning substrate is: at first the acetone ultrasonic cleaning is 5 minutes, then use the alcohol ultrasonic cleaning 5 minutes, last deionized water ultrasonic cleaning 5 minutes.
3. the preparation method of a kind of self-supporting large ratio of height to width polymer architecture as claimed in claim 1, is characterized in that, in described step (1), the temperature of baking is 150 ℃, and the time of baking is 20 minutes.
4. the preparation method of a kind of self-supporting large ratio of height to width polymer architecture as claimed in claim 1, it is characterized in that, in described step (1), before the coated polymer film, first by the oxygen rie technology, cooled substrate surface is carried out to modification, then the coated polymer film, the oxygen flow of described oxygen rie technology is 30sccm, reaction time is 10 seconds, and radio-frequency power is 40 watts.
5. the preparation method of a kind of self-supporting large ratio of height to width polymer architecture as described as claim 1 or 4, it is characterized in that, in described step (1), the material of thin polymer film is polymetylmethacrylate, coating processes is for revolving Tu technique, coating thickness is 200～300 nanometers, and described step of revolving Tu technique comprises:
1) revolve Tu PMMA on substrate, the spin coating rotating speed is 500～2000 revolutions per seconds;
2) baking, solidify PMMA, and described baking temperature is 180 ℃, and baking time is 90 seconds.
6. the preparation method of a kind of self-supporting large ratio of height to width polymer architecture as claimed in claim 1, it is characterized in that, in described step (1), the method for depositing metal films is the ion beam sputter depositing method, and the chamber vacuum degree of described ion beam sputter depositing method is 1.0 * 10
-3～1.3 * 10
-3pa, the ion beam line is 70～80mA, and sedimentation time is 10～15 minutes, and deposit thickness is 200～300 nanometers.
7. the preparation method of a kind of self-supporting large ratio of height to width polymer architecture as claimed in claim 1, it is characterized in that, in described step (2), photoresist is the SU8 negative photoresist, the revolution applied is 500～2000 revolutions per seconds, the time applied is 10～60 seconds, and the thickness of coating is 100～150 microns.
8. the preparation method of a kind of self-supporting large ratio of height to width polymer architecture as claimed in claim 1, is characterized in that, in described step (2), the method of baking is: in temperature, be at first to toast 5 minutes under 65 ℃, then be warming up to 95 ℃, toast 20 minutes, the speed of described intensification is 5 ℃/min.
9. the preparation method of a kind of self-supporting large ratio of height to width polymer architecture as claimed in claim 1, is characterized in that, in described step (2), adopts the ultraviolet photolithographic technology to be exposed to photoresist, develops, and described exposure dose is 150～200J/cm
2the method of described development is: at first baking 3 minutes under 65 ℃, then be warming up to 95 ℃ of bakings 15 minutes, and the speed of described intensification is 5 ℃/min, be placed in again 1-Methoxy-2-propyl acetate PGMEA and develop 10～15 minutes, finally be placed in isopropyl alcohol IPA and clean 5 minutes.
10. the preparation method of a kind of self-supporting large ratio of height to width polymer architecture as claimed in claim 1, is characterized in that, in described step (3), the thin polymer film lysate is organic solvent, the dissolution time of lysate is 5～10min, after dissolving, uses washed with de-ionized water, and nitrogen dries up; Metal erosion liquid is the ferric chloride solution that mass concentration is 0.5%, and the etching time of corrosive liquid is 3～5 minutes, uses successively IPA and washed with de-ionized water after corrosion, and nitrogen dries up.
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