CN103769025A - Microbubble generator and preparation method thereof - Google Patents
Microbubble generator and preparation method thereof Download PDFInfo
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- CN103769025A CN103769025A CN201410017876.7A CN201410017876A CN103769025A CN 103769025 A CN103769025 A CN 103769025A CN 201410017876 A CN201410017876 A CN 201410017876A CN 103769025 A CN103769025 A CN 103769025A
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- 238000001259 photo etching Methods 0.000 claims abstract description 16
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- 238000004528 spin coating Methods 0.000 claims abstract description 7
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 62
- 229910052759 nickel Inorganic materials 0.000 claims description 31
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 22
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- 238000005566 electron beam evaporation Methods 0.000 claims description 10
- 238000000137 annealing Methods 0.000 claims description 6
- 238000005253 cladding Methods 0.000 claims description 6
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- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 4
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Abstract
The invention discloses a microbubble generator and a preparation method thereof. The microbubble generator comprises a substrate, two electrodes and a carbon nano tube, wherein each of the two electrodes comprises graphene; the carbon nano tube is connected with the two electrodes through the graphene and is used as a heating component. The preparation method comprises the following steps of performing spin-coating on the surface of a metal foil, on which the graphene grows, with PMMA (polymethyl methacrylate); removing the metal foil, transferring the graphene protected by the PMMA to the substrate, and performing thermal treatment to enable the graphene to be tightly combined with the substrate; removing the PMMA; performing photoetching and reaction ion etching to obtain the two graphene electrodes; and covering the substrate with Cu2O nano particles serving as a catalyst, and with a hydrocarbon as a carbon source, growing a horizontal orientated carbon nano tube perpendicular to the graphene electrodes under the temperature of 800-950 DEG C through a low-pressure CVD (chemical vapor deposition) technology. The power consumption of the microbubble generator is reduced, and the service life of the microbubble generator is effectively prolonged; furthermore, the microbubble generator is simple in structure and flexible in design and has good high-frequency response and intensive integration potential.
Description
Technical field
The invention belongs to micro-electromechanical system field, more specifically, relate to a kind of microbubble generator and preparation method thereof.
Background technology
Microbubble generator is made up of substrate, heating element heater and electrode three parts, and the huge Joule heat that is fixed on interelectrode heating element heater generation makes heating liquid and produces bubble.Microbubble generator is not only the core of the hot sprayed printed system of hot bubble type, is widely used in MEMS field and microfluid system but also can be used as bubble actuators, bubble valve and bubble kinetic pump etc.For example, microbubble generator produces bubble and drives liquid to flow in capillary channel, is used for microorganism hybrid system, and catches microbe granular etc. as actuator.
Existing microbubble generator all adopts or part adopts metal material, and the power consumption of device is higher, and meanwhile, because metal material is easily subject to electrochemical corrosion under liquid environment, the service life of device is not long.
Summary of the invention
For above defect or the Improvement requirement of prior art, the invention provides a kind of microbubble generator and preparation method thereof, take CNT as heating component, take Graphene as electrode material, overcome conventional metals electrode microbubble generator power consumption high, corrosion-prone shortcoming, reduce the contact resistance of micro-heater, thereby reduce the power consumption of microbubble generator, effectively extend the life-span of microbubble generator, and device architecture is simple, flexible design, there are good high frequency response and intensive integrated potentiality, formerly the system field of making is with a wide range of applications.
For achieving the above object, according to one aspect of the present invention, provide a kind of microbubble generator, it is characterized in that, comprised substrate, two electrodes and CNT; Described two electrodes all comprise Graphene, and described CNT connects described two electrodes by described Graphene, and described CNT is as heating component.
Preferably, described two electrodes are positioned on described substrate, form by Graphene, and electrode spacing is 1~8 μ m, the diameter of described CNT is 1~5nm, and the silicon dioxide film that the contact site cladding thickness of described CNT and described two electrodes is 100~300nm is fixed.
Preferably, described CNT is positioned on described substrate, and the nickel film that described two electrodes cover graphene film by upper and lower surface forms, and covers the two ends of described CNT, and electrode spacing is 1~8 μ m.
According to another aspect of the present invention, a kind of preparation method of microbubble generator is provided, it is characterized in that, comprise the steps: that (1) has the metal foil surface spin coating PMMA of Graphene in growth; (2) remove metal forming, the Graphene of PMMA protection is transferred on substrate, heat treatment is combined closely Graphene and substrate; (3) remove PMMA; (4) obtain two Graphene electrodes by photoetching and reactive ion etching; (5) on substrate, cover Cu
2o nano particle, uses Cu
2o nano particle is made catalyst, and hydrocarbon is made carbon source, adopts low pressure chemical vapor deposition technique, at 800~950 ℃, and the horizontal orientation CNT vertical with Graphene electrodes of growing; (6) by photoetching and reactive ion etching, remove unnecessary CNT, make the two ends of CNT contact respectively two Graphene electrodes; (7) adopt electron beam evaporation and stripping technology, cover silicon dioxide film in the contact site of CNT and two Graphene electrodes and be fixed, complete the preparation of microbubble generator.
Preferably, in described step (2), described heat treatment temperature is 150 ℃, and the time is 10min.
Preferably, the spacing of described two Graphene electrodes is 1~8 μ m.
Preferably, the thickness of described silicon dioxide film is 100~300nm.
According to another aspect of the present invention, a kind of preparation method of microbubble generator is provided, it is characterized in that, comprise the steps: that (1) covers Cu on substrate
2o nano particle; (2) use Cu
2o nano particle is made catalyst, and hydrocarbon is made carbon source, adopts low pressure chemical vapor deposition technique, at Grown horizontal orientation CNT; (3) by photoetching and reactive ion etching, retain the CNT as microbubble generator heating component, remove unnecessary CNT; (4) adopt electron beam evaporation and stripping technology, cover successively the amorphous carbon film of two electrode patterns and the nickel film of two electrode patterns at the two ends of CNT; (5) annealing, maximum temperature is 800~850 ℃, cooldown rate is 10~25 ℃/s, makes amorphous carbon dissolve in nickel film, forms graphene film in nickel film upper and lower surface, completes the preparation of microbubble generator.
Preferably, the specific implementation of described step (1) is: the CuCl that substrate is immersed to 0.01~10mmol/L
2alcoholic solution in, take out substrate, after alcohol volatilizees completely, in the air atmosphere of 700 ℃ heated substrate form Cu
2o nano particle.
Preferably, in described step (4), the thickness of the amorphous carbon film of described two electrode patterns is 2nm, and the thickness of the nickel film of described two electrode patterns is 5~20nm, and described two electrode pattern spacing are 1~8 μ m.
In general, the above technical scheme of conceiving by the present invention compared with prior art, has following beneficial effect:
(1) avoid using metal material, respectively take CNT and Graphene as heating component and electrode material, utilize microwave transport properties and the good electric conductivity of Graphene that CNT is good, the contact of formation carbon-to-carbon, reduce the contact resistance of micro-heater, thereby reduced the power consumption of microbubble generator.
(2) carbon-based material stable in properties, is not vulnerable to electrolysis or corrosion, has effectively extended the life-span of microbubble generator.
(3) CNT and Graphene all have good high frequency electric conductivity, and the Schottky barrier of the two contact is lower, and therefore, device has good high frequency electric conductivity, the frequency response that is conducive to improve microbubble generator.
(4) device architecture is simple, flexible design, and the production technology of two-dimensional structure is conducive to improve machining accuracy and the integrated level of microbubble generator.
Accompanying drawing explanation
Fig. 1 is the preparation method's of the microbubble generator of one embodiment of the invention process flow diagram, wherein, and (a) spin coating PMMA; (b) Graphene of PMMA protection is transferred on substrate; (c) remove PMMA; (d) etching obtains Graphene electrodes; (e) level of growth aligned carbon nanotube; (f) remove surplus carbon nanotube; (g) cover silicon dioxide film in the contact site of CNT and Graphene electrodes;
Fig. 2 is the preparation method's of the microbubble generator of another embodiment of the present invention process flow diagram, wherein, and (a) level of growth aligned carbon nanotube; (b) remove surplus carbon nanotube; (c) cover successively amorphous carbon film and nickel film at CNT two ends; (d) form graphene film by annealing in nickel film upper and lower surface.
The specific embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.In addition,, in each embodiment of described the present invention, involved technical characterictic just can combine mutually as long as do not form each other conflict.
CNT (CNT) is the microwave conductor that a kind of structure is good, and the radially phon scattering that one dimension tubular structure causes has limited the radially scattering of CNT, and Axial Thermal conduction makes CNT produce highdensity Joule heat.Graphene is as a kind of two-dimension single layer material, and its band gap is zero, and electric transmission speed is fast, has good electric conductivity.The present invention utilizes microwave transport properties and the good electric conductivity of Graphene that CNT is good, formation carbon-to-carbon contacts, and has reduced the power consumption of microbubble generator, and due to carbon-based material stable in properties, be not vulnerable to electrolysis or corrosion, effectively extended the life-span of microbubble generator.In addition, preparation technology is simple, and has good high frequency response and intensive integrated potentiality, and formerly the system field of making is with a wide range of applications.
Microbubble generator of the present invention comprises: substrate, two electrodes and CNT.Each electrode all comprises Graphene, and CNT connects two electrodes by the Graphene in electrode, as heating component.
As shown in Figure 1, the preparation method of the microbubble generator of one embodiment of the invention comprises the steps:
(1) there is surperficial spin coating one deck polymethyl methacrylate (PMMA) 4 of the metal forming 1 of Graphene 3 in growth, as shown in Fig. 1 (a).
(2) erode metal forming 1 with iron chloride or ammonium persulfate solution; the Graphene 3 that obtains PMMA4 protection, with after washed with de-ionized water, is transferred on the substrate 2 cleaning up by standard CMOS process; heat treatment is combined closely Graphene 3 and substrate 2, as shown in Fig. 1 (b).
(3) acetone soaks and removes PMMA4, obtains transferring to the Graphene 3 on substrate 2, as shown in Fig. 1 (c).
(4) obtain Graphene electrodes 31 and 32 by photoetching and reactive ion etching, as shown in Figure 1 (d) shows.Electrode spacing is 1~8 μ m, and spacing is too small, easily cause inter-electrode short-circuit, and heating part is too little, causes the finite energy of generation, and bubble is too little; Spacing is excessive, and device integrated level reduces.
(5) on substrate 2, cover Cu
2o nano particle, uses Cu
2o nano particle is made catalyst, and hydrocarbon is made carbon source, adopts low pressure chemical vapor deposition technique, and at 800~950 ℃, the horizontal orientation CNT 5 vertical with Graphene electrodes of growing, as shown in Fig. 1 (e).Temperature is too low, and hydrocarbons decompose is incomplete, carbon atom active-energy deficiency, and poor growth, affects the quality of CNT; Excess Temperature, the corrasion of active hydrogen atom is stronger, is unsuitable for the growth of CNT.The diameter of CNT is 1~5nm.
(6) by photoetching and reactive ion etching, remove unnecessary CNT, make the two ends of CNT 6 contact respectively Graphene electrodes 31 and 32, as shown in Fig. 1 (f).
(7) adopt electron beam evaporation and stripping technology, at CNT 6 and the silicon dioxide film 61 and 62 that the contact site cladding thickness of Graphene electrodes 31 and 32 is 100~300nm, as shown in Fig. 1 (g), complete the preparation of microbubble generator.Silicon dioxide film is too thin, is difficult to effective fixed contact and divides; Silicon dioxide film is too thick, stripping technology more complicated, and affect technique integration.
As shown in Fig. 1 (g), the microbubble generator of one embodiment of the invention comprises 2, two Graphene electrodes of substrate 31 and 32, and CNT 6.Substrate 2 is the silicon chip that glass or growth have oxide layer, Graphene electrodes 31 and 32 is positioned on substrate 2, electrode spacing is 1~8 μ m, diameter is that the CNT 6 of 1~5nm connects Graphene electrodes 31 and 32, and CNT 6 is fixed with the silicon dioxide film 61 and 62 that the contact site cladding thickness of Graphene electrodes 31 and 32 is 100~300nm.
As shown in Figure 2, the preparation method of the microbubble generator of another embodiment of the present invention comprises the steps:
(1) on the substrate 2 cleaning up by standard CMOS process, cover Cu
2o nano particle.
(2) use Cu
2o nano particle is made catalyst, and hydrocarbon is made carbon source, adopts low pressure chemical vapor deposition technique, level of growth aligned carbon nanotube 7 on substrate 2, as shown in Figure 2 (a) shows.
(3) by photoetching and reactive ion etching, retain the CNT 8 as microbubble generator heating component, remove unnecessary CNT, as shown in Fig. 2 (b).
(4) adopt electron beam evaporation and stripping technology, cover successively the amorphous carbon film 81 and 82 and nickel film 91 and 92 of two electrode patterns at the two ends of CNT 8, as shown in Figure 2 (c).
The thickness of amorphous carbon film 81 and 82 is about 2nm.The thickness of nickel film 91 and 92 is 5~20nm, and nickel film is too thin, can not guarantee that all carbon atoms can dissolve among nickel film; Nickel film is too thick, and the amount of carbon atom of separating out in cooling procedure is limited, can not form continuous graphite alkene film, and technique integrated level is reduced.Electrode pattern spacing is 1~8 μ m, and spacing is too small, easily cause inter-electrode short-circuit, and heating part is too little, causes the finite energy of generation, and bubble is too little; Spacing is excessive, and technique integrated level is not high.
(5) annealing, maximum temperature is 800~850 ℃, cooldown rate is 10~25 ℃/s, makes amorphous carbon dissolve in nickel film, forms graphene film in nickel film upper and lower surface, completes the preparation of microbubble generator, as shown in Figure 2 (d) shows.
Temperature is too low, and the solubility of carbon atom in nickel is not high, can not dissolve in completely in nickel film; Excess Temperature, the evaporation of nickel film is serious, and impact cooling forms graphene film.Cooldown rate is too low, and too much carbon atom is separated out the thicker graphene film of formation, lack of homogeneity; Cooldown rate is too high, and the carbon number of separating out is limited, can not form continuous graphene film.
As shown in Figure 2 (d) shows, the microbubble generator of another embodiment of the present invention comprises substrate 2, CNT 8 and two electrodes.Substrate 2 is the silicon chip that glass or growth have oxide layer, and CNT 8 is positioned on substrate 2, and two electrode spacings are 1~8 μ m, the two ends of coated carbon nanotube 8, and the nickel film that each electrode covers graphene film by upper and lower surface forms.
For making those skilled in the art understand better the present invention, below in conjunction with specific embodiment, the preparation method of microbubble generator of the present invention is elaborated.
Embodiment 1
The preparation method of microbubble generator comprises the steps:
(1) there is the PMMA of the about 200nm of copper foil surface spin coating thick layer of single-layer graphene in growth.
(2) erode metal forming with the ammonium persulfate solution of 0.5mol/L; obtain the Graphene of PMMA protection, with after washed with de-ionized water 3 times, be transferred on the substrate cleaning up by standard CMOS process; after drying up, at 150 ℃, toast 10min, Graphene and substrate are combined closely.
(3) in acetone, soak 1h and remove PMMA, obtain transferring to the Graphene on substrate.
(4) by photoetching and oxygen plasma reactive ion etching, obtain two Graphene electrodes, electrode spacing is 1 μ m.
(5) cover Cu
2o nano particle, uses Cu
2o nano particle is made catalyst, and methane gas is made carbon source, adopts low pressure chemical vapor deposition technique, is warming up to 800 ℃ with the speed of 50 ℃/s, the growth horizontal orientation CNT vertical with Graphene electrodes at 800 ℃, and the diameter of CNT is 1nm.
(6) by photoetching and oxygen plasma reactive ion etching, remove unnecessary CNT, make the two ends of CNT contact respectively two Graphene electrodes.
(7) adopt electron beam evaporation and stripping technology, the silicon dioxide film that is 100nm at the contact site cladding thickness of CNT and two Graphene electrodes, completes the preparation of microbubble generator.
Embodiment 2
The preparation method of microbubble generator comprises the steps:
(1) there is the PMMA of the about 200nm of copper foil surface spin coating thick layer of single-layer graphene in growth.
(2) erode metal forming with the ammonium persulfate solution of 0.5mol/L; obtain the Graphene of PMMA protection, with after washed with de-ionized water 4 times, be transferred on the substrate cleaning up by standard CMOS process; after drying up, at 150 ℃, toast 10min, Graphene and substrate are combined closely.
(3) in acetone, soak 1h and remove PMMA, obtain transferring to the Graphene on substrate.
(4) by photoetching and oxygen plasma reactive ion etching, obtain two Graphene electrodes, electrode spacing is 8 μ m.
(5) cover Cu
2o nano particle, uses Cu
2o nano particle is made catalyst, and methane gas is made carbon source, adopts low pressure chemical vapor deposition technique, is warming up to 950 ℃ with the speed of 50 ℃/s, the growth horizontal orientation CNT vertical with Graphene electrodes at 950 ℃, and the diameter of CNT is 5nm.
(6) by photoetching and oxygen plasma reactive ion etching, remove unnecessary CNT, make the two ends of CNT contact respectively two Graphene electrodes.
(7) adopt electron beam evaporation and stripping technology, the silicon dioxide film that is 300nm at the contact site cladding thickness of CNT and two Graphene electrodes, completes the preparation of microbubble generator.
Embodiment 3
The preparation method of microbubble generator comprises the steps:
(1) growth cleaning up by standard CMOS process there is is the silicon chip substrate of oxide layer immerse the CuCl of 0.01mmol/L
2alcoholic solution in, take out substrate, after alcohol volatilizees completely, substrate is put into CVD boiler tube, in air atmosphere, at 700 ℃, add thermosetting Cu
2o nano particle.
(2) use Cu
2o nano particle is made catalyst, and methane gas is made carbon source, adopts low pressure chemical vapor deposition technique, with 50 ℃/
sspeed be warming up to 800 ℃, level of growth aligned carbon nanotube at 800 ℃.
(3) by photoetching and reactive ion etching, retain the CNT 8 as microbubble generator heating component, remove unnecessary CNT.
(4) adopt electron beam evaporation and stripping technology, cover successively amorphous carbon film and the nickel film of two electrode patterns at the two ends of CNT, the thickness of each amorphous carbon film is 2nm, and the thickness of each nickel film is 5nm, and electrode pattern spacing is 1 μ m.
(5) annealing, maximum temperature is 850 ℃, cooldown rate be 10 ℃/
s, make amorphous carbon dissolve in nickel film, form graphene film in nickel film upper and lower surface, complete the preparation of microbubble generator.
Embodiment 4
The preparation method of microbubble generator comprises the steps:
(1) growth cleaning up by standard CMOS process there is is the silicon chip substrate of oxide layer immerse the CuCl of 10mmol/L
2alcoholic solution in, take out substrate, after alcohol volatilizees completely, substrate is put into CVD boiler tube, in air atmosphere, at 700 ℃, add thermosetting Cu
2o nano particle.
(2) use Cu
2o nano particle is made catalyst, and acetylene gas is made carbon source, adopts low pressure chemical vapor deposition technique, is warming up to 800 ℃, level of growth aligned carbon nanotube at 800 ℃ with the speed of 50 ℃/s.
(3) by photoetching and reactive ion etching, retain the CNT 8 as microbubble generator heating component, remove unnecessary CNT.
(4) adopt electron beam evaporation and stripping technology, cover successively amorphous carbon film and the nickel film of two electrode patterns at the two ends of CNT, the thickness of each amorphous carbon film is 2nm, and the thickness of each nickel film is 20nm, and electrode pattern spacing is 8 μ m.
(5) annealing, maximum temperature is 800 ℃, cooldown rate be 25 ℃/
s, make amorphous carbon dissolve in nickel film, form graphene film in nickel film upper and lower surface, complete the preparation of microbubble generator.
The present invention, respectively take CNT and Graphene as heating component and electrode material, makes the two form carbon-to-carbon contact, has reduced the power consumption of microbubble generator, due to carbon-based material stable in properties, has effectively extended the life-span of microbubble generator.In addition, CNT and Graphene all have good high frequency electric conductivity, and the Schottky barrier of the two contact is lower, and therefore, device has good high frequency electric conductivity.
Those skilled in the art will readily understand; the foregoing is only preferred embodiment of the present invention; not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a microbubble generator, is characterized in that, comprises substrate, two electrodes and CNT; Described two electrodes all comprise Graphene, and described CNT connects described two electrodes by described Graphene, and described CNT is as heating component.
2. microbubble generator as claimed in claim 1, it is characterized in that, described two electrodes are positioned on described substrate, form by Graphene, electrode spacing is 1~8 μ m, the diameter of described CNT is 1~5nm, and the silicon dioxide film that the contact site cladding thickness of described CNT and described two electrodes is 100~300nm is fixed.
3. microbubble generator as claimed in claim 1, is characterized in that, described CNT is positioned on described substrate, and the nickel film that described two electrodes cover graphene film by upper and lower surface forms, and covers the two ends of described CNT, and electrode spacing is 1~8 μ m.
4. the preparation method of microbubble generator as claimed in claim 1, is characterized in that, comprises the steps:
(1) there is the metal foil surface spin coating PMMA of Graphene in growth;
(2) remove metal forming, the Graphene of PMMA protection is transferred on substrate, heat treatment is combined closely Graphene and substrate;
(3) remove PMMA;
(4) obtain two Graphene electrodes by photoetching and reactive ion etching;
(5) on substrate, cover Cu
2o nano particle, uses Cu
2o nano particle is made catalyst, and hydrocarbon is made carbon source, adopts low pressure chemical vapor deposition technique, at 800~950 ℃, and the horizontal orientation CNT vertical with Graphene electrodes of growing;
(6) by photoetching and reactive ion etching, remove unnecessary CNT, make the two ends of CNT contact respectively two Graphene electrodes;
(7) adopt electron beam evaporation and stripping technology, cover silicon dioxide film in the contact site of CNT and two Graphene electrodes and be fixed, complete the preparation of microbubble generator.
5. the preparation method of microbubble generator as claimed in claim 4, is characterized in that, in described step (2), described heat treatment temperature is 150 ℃, and the time is 10min.
6. the preparation method of the microbubble generator as described in claim 4 or 5, is characterized in that, the spacing of described two Graphene electrodes is 1~8 μ m.
7. the preparation method of the microbubble generator as described in any one in claim 4 to 6, is characterized in that, the thickness of described silicon dioxide film is 100~300nm.
8. the preparation method of microbubble generator as claimed in claim 1, is characterized in that, comprises the steps:
(1) on substrate, cover Cu
2o nano particle;
(2) use Cu
2o nano particle is made catalyst, and hydrocarbon is made carbon source, adopts low pressure chemical vapor deposition technique, at Grown horizontal orientation CNT;
(3) by photoetching and reactive ion etching, retain the CNT as microbubble generator heating component, remove unnecessary CNT;
(4) adopt electron beam evaporation and stripping technology, cover successively the amorphous carbon film of two electrode patterns and the nickel film of two electrode patterns at the two ends of CNT;
(5) annealing, maximum temperature is 800~850 ℃, cooldown rate is 10~25 ℃/s, makes amorphous carbon dissolve in nickel film, forms graphene film in nickel film upper and lower surface, completes the preparation of microbubble generator.
9. the preparation method of microbubble generator as claimed in claim 8, is characterized in that, the specific implementation of described step (1) is: the CuCl that substrate is immersed to 0.01~10mmol/L
2alcoholic solution in, take out substrate, after alcohol volatilizees completely, in the air atmosphere of 700 ℃ heated substrate form Cu
2o nano particle.
10. the preparation method of microbubble generator as claimed in claim 8 or 9, it is characterized in that, in described step (4), the thickness of the amorphous carbon film of described two electrode patterns is 2nm, the thickness of the nickel film of described two electrode patterns is 5~20nm, and described two electrode pattern spacing are 1~8 μ m.
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