CN102332375B - Preparation method for carbon nanotube-based dielectric barrier micro-discharge structure - Google Patents
Preparation method for carbon nanotube-based dielectric barrier micro-discharge structure Download PDFInfo
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- CN102332375B CN102332375B CN201110226566.2A CN201110226566A CN102332375B CN 102332375 B CN102332375 B CN 102332375B CN 201110226566 A CN201110226566 A CN 201110226566A CN 102332375 B CN102332375 B CN 102332375B
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Abstract
The invention discloses a preparation method for a carbon nanotube-based dielectric barrier micro-discharge structure. The method specifically comprises the following steps of: preparing a three-dimensional micro-discharge electrode on a substrate; depositing a polymer dielectric thin film on the surface of the microelectrode; forming a dielectric and electrode alternating structure; and depositing a one-dimensional nano-material on the microelectrode not covered by dielectric. The coverage of the surface of the micro-discharge electrode by the dielectric can be effectively improved, the suppression effect of the dielectric on ionization can be enhanced, a short-circuit fault of carbon nanotubes between electrodes can be avoided by the formed alternating dielectric and electrode structure, the working life of a device can be prolonged, and the preparation yield can be improved.
Description
Technical field
what the present invention relates to is a kind of microdischarge devices of microelectronics technology, and specifically, that relate to is a kind of preparation method of the dielectric impedance micro discharge structure based on carbon nano-tube.
Background technology
in daily life, the application of gas discharge is very extensive, such as ozone generator and dielectric barrier discharge light source etc.But under normal temperature atmospheric pressure, gas needs the voltage of several thousand volts even up to ten thousand could form stable electric discharge.By the designs such as the Hui Guohua of Zhejiang University based on aligned carbon nanotube gas discharge structure, the operating voltage of gas dark discharge under atmospheric pressure can be reduced to below 500V, make to utilize the measurement of gas breakdown voltage and discharging current greatly to improve the feasibility of gas qualitative and quantitative detection and practicality.And the self sustaining dark discharge carbon nano tube thin film gas transducer of the designs such as Liu Junhua of Xi'an Communications University can be further down to the operating voltage of gas self sustaining dark discharge below 200V.
through the literature search of prior art is found, Chinese patent " the ionized gas sensor microarray structure based on the microelectronic processing technique " (patent No.: ZL 200510112218.7, publication number CN1808111A), this patent readme is for " to comprise, substrate, microelectrode array, microelectrode bar unit, sensor unit, it is characterized in that, described microelectrode array is arranged on substrate, microelectrode array comprises a plurality of microelectrode bars unit, every pair of adjacent anodic-cathodic bar forms side-wall electrode pair, as producing controllable electric field structure, thereby form a sensor unit, a plurality of sensor units form microelectrode array, whether the plane geometric shape according to the adjacent anodic-cathodic bar in each sensor unit is identical with spacing, sensor unit is divided into and is equal to unit and phase anticoincidence unit, be equal to unit and refer to that the plane geometric shape of the adjacent anodic-cathodic bar in two unit is identical with spacing, phase anticoincidence unit refers to plane geometric shape or the spacing difference of the adjacent anodic-cathodic bar in two unit." this technology application micro-processing technology obtains microelectrode spacing, the electric field astriction in conjunction with monodimension nanometer material under scale effect, has reduced the operating voltage of device widely.But for above-mentioned, pass through the gas molecule of ionization in micro-structural electric field, and consequent gas discharge, all likely because discharging current can not get suppressing, freely increase and then damage device, thereby reducing its useful life and functional reliability.
the people such as Wu Jiahao have proposed a kind of carbon nano-tube dielectric impedance gas sensor of preparing based on micro mechanical technology (" A MEMS-based ionization gas sensor using carbon nanotubes and dielectric barrier ", Proceedings of the 3
rd
iEEE Int. Conf.on Nano/Micro Engineered and Molecular Systems, 824-827 page), the formation of this transducer is that the parallel three-dimensional micro-electrode that one or more pairs of spacing are micro-meter scale is set in the dielectric base such as glass, utilize sidewall relative between electrode as region of discharge, and at electrode surface deposition of carbon nanotubes, further reduce ionization threshold voltage by electrophoresis method.Destruction device being produced in order to suppress excessive ionization electric current, at the surface coverage dielectric layer that deposits the microelectrode of carbon nano-tube, forms carbon nano-tube dielectric barrier discharge structure.Its result of study shows, this technology can effectively limit freely increasing of discharging current, improves the working life of device.But, in the preparation of described device, dielectric layer adopts sputtering method deposition on electrode after electrophoresis carbon nano-tube, because electrode spacing is micro-meter scale, electrode surface deposition of carbon nanotubes with and subsequent medium overwrite procedure in, carbon pipe is easy to remain between electrode, causes inter-electrode short-circuit, cannot normally work.In addition, the method is not suitable for the dielectric barrier discharge structure that preparation consists of organic media.
Summary of the invention
the present invention is directed to shortcomings and deficiencies of the prior art, a kind of preparation method of the dielectric impedance micro discharge structure based on carbon nano-tube is provided, obtain being alternately placed with at electrode surface the dielectric impedance micro discharge structure of medium and carbon nano-tube, can effectively improve the performance of carbon nano-tube DBD microdischarge devices, improve qualification rate and the job stability of device.
the present invention is achieved by the following technical solutions, the present invention adopts high temperature polymer as dielectric material, by spin coating and photoetching method, form and patterned media film, an electrode surface overwrite media in electrode pair only, finally electrophoresis deposition of carbon nanotubes on the electrode covering without medium.Colloid spin coating method has good spreadability, be conducive to form continuous, fine and close deielectric-coating on the sidewall of three-diemsnional electrode, not only strengthened the restriction of medium to ionization, and because carbon nano-tube is deposition after medium forms, can effectively avoid remaining in the problem that carbon nano-tube in electrode gap causes direct short-circuit.
the preparation method of a kind of dielectric impedance micro discharge structure based on carbon nano-tube of the present invention, specifically comprises the steps:
step 1. is prepared three-dimensional micro discharge electrode on substrate;
adopt surperficial high insulating material as substrate, comprise glass, High Resistivity Si and other insulating material.
adopt conventional photoetching, thin film deposition, photoresist lift off method to prepare the plating seed layer of micro discharge electrode.
adopt the method for mask plating, electroplate three-dimensional micro discharge electrode in above-mentioned Seed Layer, plated material is the metals such as nickel, gold, copper.
step 2. is at micro discharge electrode surface coat polymers dielectric film;
adopt polymer sol, by the method for spin coating, overlie polymer dielectric film on above-mentioned micro discharge electrode.
step 3. forms medium and electrode alternating structure;
utilize photoresist as mask layer, by photoetching, developing method, graphical to dielectric film, graphical after only an electrode surface in micro discharge electrode pair be coated with dielectric film.
step 4. deposits monodimension nanometer material on the microelectrode of overwrite media not.
adopt electrophoresis method deposition of carbon nanotubes on the electrode of overwrite media not.
the above micro discharge electrode, is the K-A electrode pair that one or more pairs of parallel microelectrodes form, and the material good by electric conductivity makes.
described three-dimensional micro discharge electrode pair is of a size of width 20um, length 2000um, spacing 10-20um, height 5-15um.
described polymeric media film, its material is organic media material, is preferably polyimides, the thickness of dielectric film is 4-6um.
described medium and electrode alternating structure, be anodic-cathodic centering, only has overwrite media on an electrode, and another is metal electrode.
described monodimension nanometer material, a kind of in carbon nano-tube, silicon carbide nanometer line, silicon nanowires, zinc oxide nanowire.
the parameter of described electrophoresis method is: the carbon nano-tube weight percent concentration in electrophoresis solution is: 0.1%, and solvent is acetone, and charged auxiliary salt is magnesium nitrate, and weight percent concentration is 0.1%, and electrode cathode is sample, anode is stainless sheet steel.During electrophoretic deposition, apply electric field strength 5-15V/cm, the time is 2-4 minute.
beneficial effect of the present invention is:
1. the dielectric film that adopts spin coating method to prepare has improved the coverage effect of medium on sidewall, has improved the restriction of medium to ionization.
. by form medium and electrode structure alternately on micro discharge electrode pair, avoid the short trouble of interelectrode carbon nano-tube, improved the working life of device.
because carbon nano-tube is deposited on preparation flow, finally carry out, eliminated the impact of subsequent technique on carbon pipe performance and location, improved qualification rate prepared by device.
Embodiment
below embodiments of the invention are elaborated: the present embodiment is implemented take technical solution of the present invention under prerequisite, provided detailed execution mode and process, but protection scope of the present invention is not limited to following embodiment.
embodiment 1
the present embodiment is implemented under following implementation condition and specification requirement:
1. prepare 3-dimensional metal micro discharge electrode;
adopt the high resistance glass of insulation as substrate, first adopt photoetching process at substrate surface, to form the photoetching offset plate figure of micro discharge electrode, sputtering sedimentation metal seed layer thereon then, obtains Seed Layer electrode structure after removing photoresist with stripping technology.The seed layer materials of selecting is Cu/Ti, Cu thickness 0.12um, and Ti thickness is 0.03um, and electrode width is 20um, and length is 2000um, and electrode spacing is 10um.Then, be prepared with on the sample of Seed Layer, adopting photoetching process, forming photoresist mask plating figure, photoresist height is 10um.Above-mentioned sample is put into Watt Ni deposition liquid, and using it as negative electrode, nickel plate is as anode, and applying electroplating current density is 0.2A/dm
2
, the time is 30 minutes, obtaining is highly the nickel sparking electrode of 5um.
deposition medium film;
on the Ni electrode obtaining in 1 step, spin-on polyimide coating adhesive, turn/min of whirl coating rotating speed 3500, time 45s, is placed on slice, thin piece on hot plate after whirl coating, from 130
0
c is progressively warming up to 170
0
c, hot curing polyimide film.
form medium and electrode alternating structure;
on the polyimide film obtaining in step 2, adopt photoetching process, by exposing, develop, removing photoresist, form polyimides figure, making only has an electrode to cover polyimides in electrode pair.Then, then the polyimides after graphical is further done to imidization and process, design parameter is: 300
0
c, 1 hour, after imidization, the thickness of polyimides was about 6um.
deposition monodimension nanometer material
by the slice, thin piece through after step 3, adopt electrophoresis method on the electrode of overwrite media not, to deposit the carbon nano-tube of certain density.The parameter of electrophoretic deposition is: the carbon nano-tube weight percent concentration in electrophoresis solution is 0.1%, and solvent is acetone, and magnesium nitrate is for charged auxiliary salt, and weight percent concentration is 0.1%, and negative electrode is deposited samples, and anode is stainless sheet steel.During electrophoretic deposition, apply electric field strength 15V/cm, the time is 2 minutes.
the micro discharge electrode electrode spacing that the present embodiment prepares is 10 microns, the electrode surface of overwrite media is distributed with the uniform deielectric-coating of one deck, overlay area accurate positioning, sharpness of border, neat, in another electrode surface even carbon nanotube, distribute, ionization performance to device is tested, the ionization threshold voltage obtaining is 3V, ionization electric current obviously starts to decline when 5V, show that device not only under lower voltage, ionization occurs, and dielectric layer has good inhibitory action to the growth of ionization electric current.
embodiment 2
the present embodiment is implemented under following implementation condition and specification requirement condition:
1. prepare 3-dimensional metal micro discharge electrode;
adopt the high resistance glass of insulation as substrate, first adopt photoetching process at substrate surface, to form the photoetching offset plate figure of sparking electrode, then sputtering sedimentation metal seed layer thereon, removes photoresist with stripping technology, obtains Seed Layer electrode structure.The seed layer materials of selecting is Cu/Ti, Cu thickness 0.12um, and Ti thickness is 0.03um, and electrode width is 20um, and length is 2000um, and electrode spacing is 15um.Then, be prepared with on the sample of Seed Layer, adopting photoetching process, forming photoresist mask plating figure, photoresist height is 15um.Above-mentioned sample is put into Watt Ni deposition liquid, and using it as negative electrode, nickel plate is as anode, and applying electroplating current density is 0.2A/dm
2,
time is 60 minutes, and obtaining deposit thickness is the nickel sparking electrode of 10um.
deposition medium film;
on the Ni electrode obtaining in 1 step, spin-on polyimide coating adhesive, turn/min of whirl coating rotating speed 4000, time 45s, is placed on slice, thin piece on hot plate after whirl coating, from 130
0
c is progressively warming up to 170
0
c, hot curing polyimide film.
form medium and electrode alternating structure;
on the polyimide film obtaining in step 2, adopt photoetching process, by exposing, develop, removing photoresist, form polyimides figure, making only has an electrode surface to cover polyimides in electrode pair.And then the polyimides after graphical is further done to imidization and process, design parameter is: 300
0
c, 1 hour, after imidization, the thickness of polyimides was 5um.
deposition monodimension nanometer material
by the slice, thin piece through after step 3, adopt electrophoresis method on the electrode of overwrite media not, to deposit the carbon nano-tube of certain density.The parameter of electrophoretic deposition is: the carbon nano-tube weight percent concentration in electrophoresis solution is: 0.1%, and solvent is acetone, and magnesium nitrate is for charged auxiliary salt, and weight percent concentration is 0.1%, and negative electrode is deposited samples, anode is stainless sheet steel.During electrophoretic deposition, apply electric field strength 10V/cm, the time is 3 minutes.
the micro discharge electrode spacing that the present embodiment prepares is 15 microns, the electrode surface deielectric-coating of overwrite media is even, overlay area accurate positioning, sharpness of border, neat is distributed with carbon nano-tube on another electrode surface and sidewall, and the ionization performance of device is tested, the ionization threshold voltage obtaining is 6V, ionization electric current obviously starts to decline at 10V, show that device not only under lower voltage, ionization occurs, and medium has good inhibitory action to the growth of ionization electric current.
embodiment 3
the present embodiment is implemented under following implementation condition and specification requirement condition:
1. prepare 3-dimensional metal micro discharge electrode;
adopt the high resistance glass of insulation as substrate, first adopt photoetching process at substrate surface, to form the photoetching offset plate figure of sparking electrode, then sputtering sedimentation metal seed layer thereon, removes photoresist with stripping technology, obtains Seed Layer electrode structure.The seed layer materials of selecting is Cu/Ti, Cu thickness 0.12um, and Ti thickness is 0.03um, and electrode width is 20um, and length is 2000um, and electrode spacing is 20um.Then, depositing on the sample of Seed Layer, adopting photoetching process, forming photoresist mask plating figure, photoresist height is 20um.Above-mentioned sample is put into Watt Ni deposition liquid, and using it as negative electrode, nickel plate is as anode, and applying electroplating current density is 0.2A/dm
2
, the time is 90 minutes, obtaining is highly the nickel sparking electrode of 15um.
deposition medium film;
on the Ni electrode obtaining in 1 step, spin-on polyimide coating adhesive, turn/min of whirl coating rotating speed 4500, time 45s, is placed on slice, thin piece on hot plate after whirl coating, from 130
0
c is progressively warming up to 170
0
c, hot curing polyimide film.
form medium and electrode alternating structure;
on the polyimide film obtaining in step 2, adopt photoetching process, by exposing, develop, removing photoresist, form polyimides figure, make an electrode in electrode pair cover polyimides.Again the polyimides after graphical is further done to imidization and process, design parameter is: 300
0
c, 1 hour, after imidization, the thickness of polyimides was 4um.
deposition monodimension nanometer material
by the slice, thin piece through after step 3, adopt electrophoresis method on the electrode of overwrite media not, to deposit the carbon nano-tube of certain density.The parameter of electrophoretic deposition is: the carbon nano-tube weight percent concentration in electrophoresis solution is: 0.1%, and solvent is acetone, and magnesium nitrate is as charged auxiliary salt, and weight percent concentration is 0.1%, and negative electrode is for being deposited as sample, and anode is stainless sheet steel.During electrophoretic deposition, apply electric field strength 5V/cm, the time is 4 minutes.
the micro discharge electrode electrode spacing that the present embodiment prepares is 20 microns, the electrode surface deielectric-coating of overwrite media is even, overlay area accurate positioning, sharpness of border, neat, on another electrode surface and sidewall, be distributed with carbon nano-tube, device ionization performance is tested, the ionization threshold voltage obtaining is 10V, ionization electric current obviously starts to decline at 15V, result shows that device not only under lower voltage, ionization occurs, and medium has good inhibitory action to the growth of ionization electric current.
Claims (10)
1. a preparation method for the dielectric impedance micro discharge structure based on carbon nano-tube, comprises the steps:
Step 1 is prepared three-dimensional micro discharge electrode on substrate;
Step 2, the method by spin coating is at micro discharge electrode surface deposited polymer dielectric film; Described polymeric media film is polyimides;
On the three-dimensional micro discharge electrode obtaining in step 1, spin-on polyimide coating adhesive, is placed on slice, thin piece on hot plate after whirl coating, from 130 ℃, is progressively warming up to 170 ℃, hot curing polyimide film;
Step 3, forms medium and electrode alternating structure: utilize photoresist as mask layer, by photoetching, developing method, graphical to dielectric film, graphical after only an electrode surface in micro discharge electrode pair be coated with dielectric film;
On the polyimide film obtaining in step 2, adopt photoetching process, by exposing, develop, removing photoresist, form polyimides figure, making only has an electrode to cover polyimides in electrode pair, then, then the polyimides after graphical is further done to imidization and process, design parameter is: 300 ℃, and 1 hour;
Step 4 deposits monodimension nanometer material on the micro discharge electrode of overwrite media not;
The above micro discharge electrode is the K-A electrode pair of one or more pairs of parallel microelectrodes compositions.
2. the preparation method of the dielectric impedance micro discharge structure based on carbon nano-tube according to claim 1, it is characterized in that, described step 1, is specially: adopt the method for photoetching, thin film deposition, photoresist lift off, prepare the plating seed layer of micro discharge electrode pattern on substrate; Adopt the method for mask plating, in above-mentioned Seed Layer, electroplate three-dimensional micro discharge electrode.
3. the preparation method of the dielectric impedance micro discharge structure based on carbon nano-tube according to claim 1 and 2, is characterized in that, described substrate is glass, or High Resistivity Si, or surface deposition has the substrate of insulating material.
4. the preparation method of the dielectric impedance micro discharge structure based on carbon nano-tube according to claim 1 and 2, is characterized in that, described micro discharge electrode, and the anodic-cathodic pair for one or more pairs of parallel microelectrodes form, is made by electric conducting material.
5. the preparation method of the dielectric impedance micro discharge structure based on carbon nano-tube according to claim 1 and 2, is characterized in that, described three-dimensional micro discharge electrode pair is of a size of width 20um, length 2000um, spacing 10-20um, height 5-15um.
6. the preparation method of the dielectric impedance micro discharge structure based on carbon nano-tube according to claim 1, is characterized in that, the thickness of described polymeric media film is 4-6um.
7. the preparation method of the dielectric impedance micro discharge structure based on carbon nano-tube according to claim 1, is characterized in that, described monodimension nanometer material is a kind of in carbon nano-tube, silicon carbide nanometer line, silicon nanowires, zinc oxide nanowire.
8. according to the preparation method of the dielectric impedance micro discharge structure based on carbon nano-tube described in claim 1 or 7, it is characterized in that, described monodimension nanometer material is carbon nano-tube.
9. the preparation method of the dielectric impedance micro discharge structure based on carbon nano-tube according to claim 1, is characterized in that, described step 4, is specially: adopt electrophoresis method at the micro discharge electrode surface deposition monodimension nanometer material of overwrite media not.
10. the preparation method of the dielectric impedance micro discharge structure based on carbon nano-tube according to claim 9, it is characterized in that, the parameter of described electrophoresis method is: the carbon nano-tube weight percent concentration in electrophoresis solution is 0.1%, solvent is acetone, charged auxiliary salt is magnesium nitrate, weight percent concentration is 0.1%, and electrode cathode is sample, and anode is stainless sheet steel; During electrophoretic deposition, apply electric field strength 5-15V/cm, the time is 2-4 minute.
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