CN102403175A - Method for depositing medium barrier layer on micro-nano electrode - Google Patents
Method for depositing medium barrier layer on micro-nano electrode Download PDFInfo
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- CN102403175A CN102403175A CN2011103464536A CN201110346453A CN102403175A CN 102403175 A CN102403175 A CN 102403175A CN 2011103464536 A CN2011103464536 A CN 2011103464536A CN 201110346453 A CN201110346453 A CN 201110346453A CN 102403175 A CN102403175 A CN 102403175A
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Abstract
The invention discloses a method for depositing a medium barrier layer on a micro-nano electrode, which comprises the following steps of: preparing a three-dimensional micro discharge electrode on a substrate; and carrying out electrophoretic deposition of a carbon nano tube on the surface of the micro electrode and simultaneously forming a magnesium oxide medium covering layer. The inhibition effect of a medium on an ionization current is improved and the service life is prolonged by improving the medium coverage of the surfaces of the carbon nano tube and the micro discharge electrode. The method has simple preparation steps and low preparation cost.
Description
Technical field
What the present invention relates to is a kind of microdischarge devices of microelectronics technology, specifically, relate to be a kind of on the micro-nano electrode method on deposition medium barrier layer.
Background technology
The character of gas ionization characteristic and gas has substantial connection, and gas with various has different critical discharge voltages and critical discharging current, and then can be used as the foundation of difference gas with various composition and concentration.As gas sensor, it is short that the type transducer has the response time, highly sensitive, recovers advantage such as fast.But the animating electrode physical dimension with the conventional method preparation is bigger, and the operating voltage of kilovolt has limited the application aspect transducer greatly on the needs.Development along with the micro-nano technology; Occurred the micron of monodimension nanometer material such as CNT and the micro-processing technology preparation micro-nano discharge electrode structure that forms of combination of electrodes intermittently; Can the operating voltage of gas discharge under the atmospheric pressure be reduced to below tens volts, make and utilize gas discharge characteristic that the feasibility and the practicality of gas qualitative and quantitative analysis are improved greatly.
It is too fast that but this type of device still exists discharging current to change, and the ionization degree is difficult to control problem, thereby reduce the useful life and the functional reliability of device.Therefore, how when reducing the ionization threshold voltage, degree of ionization being constrained to is the subject matter of essential solution in this type of device application.
Dielectric barrier discharge (DBD) structure is through adding dielectric in sparking electrode surface and space; The ionization electric charge of generation is gathered at dielectric surface; Produce an internal electric field in the opposite direction, thereby make the total electric field intensity decreases between electrode gap and stop discharge with extra electric field.When apply reverse add field intensity after, begin a new discharge cycle again.Therefore, through the DBD structure can suppress freely increasing of ionization current effectively from restriction, thereby obtain more stable ionized state, increase the useful life of device.
People such as Wu Jiahao have proposed a kind of CNT dielectric impedance gas sensor (" A MEMS-based ionization gas sensor using carbon nanotubes and dielectric barrier ", Proceedings of the 3 based on the micro mechanical technology preparation
RdIEEE Int.Conf.on Nano/Micro Engineered and Molecular Systems; The 824-827 page or leaf); The formation of this transducer is that the parallel three-dimensional micro-electrode that one or more pairs of spacings are micro-meter scale is set on dielectric base such as glass; Utilize sidewall relative between electrode as region of discharge, and further reduce the ionization threshold voltage at the electrode surface deposition of carbon nanotubes through electrophoresis method.In order to suppress the destruction that excessive ionization electric current produces device,, constitute CNT dielectric barrier discharge structure at the surface coverage dielectric layer of the microelectrode that deposits CNT.Its result of study shows that this technology can effectively limit freely increasing of discharging current, improves the working life of device.But in said preparation of devices, dielectric layer is to adopt the sputtering method deposition, needs special-purpose film deposition equipment, and preparation cost is higher relatively.And general sputter deposition is relatively poor to the covering power of three-dimensional microstructures, has influenced the integrality that medium covers on the side-wall electrode.
Summary of the invention
The present invention is directed to the deficiency and the defective of prior art; Provide a kind of on the micro-nano electrode method on deposition medium barrier layer, adopt electrophoresis method, on electrode, form dielectric layer in the deposition of carbon nanotubes; Thereby improved the medium coverage effect effectively; Improved the performance and the job stability of device, and the step that simplifies the operation, preparation cost reduced.
The present invention realizes through following technical scheme; The present invention adopts electrophoretic deposition method, in carbon nano-tube electrophoretic liquid, adds excessive magnesium nitrate, through separating out in electrophoretic deposition CNT process; And follow-up heat treatment, form dielectric film on the microelectrode surface.
A kind of method that on the micro-nano electrode, forms dielectric barrier according to the invention comprises the steps:
Step 1. prepares three-dimensional micro discharge electrode on substrate;
Substrate is a glass, or High Resistivity Si, or pottery or surface deposition have the substrate of insulating material.
Adopt photoetching commonly used, thin film deposition, photoresist lift off method to prepare the plating seed layer of micro discharge electrode.
Adopt the method for mask plating, on above-mentioned Seed Layer, electroplate three-dimensional micro discharge electrode, plated material is metals such as nickel, gold, copper.
Step 2. deposition monodimension nanometer material and dielectric layer
Adopt electrophoresis method, deposition monodimension nanometer material and dielectric layer on above-mentioned three-dimensional micro discharge electrode.Add excessive charged auxiliary salt magnesium nitrate in the electrophoresis liquid, dielectric layer is a magnesia.
The heat treatment of step 3. dielectric layer
The above-mentioned sample that deposits CNT and medium is carried out vacuum heat, obtain stable MgO dielectric layer.
Said micro discharge electrode is the K-A electrode pair that one or more pairs of parallel microelectrodes are formed, and the material good by electric conductivity makes.
Said three-dimensional micro discharge electrode pair is of a size of width 20um, length 2000um, spacing 10-20um, height 5-15um.
Said monodimension nanometer material, a kind of in CNT, silicon carbide nanometer line, silicon nanowires, the zinc oxide nanowire.
The parameter of said electrophoresis method is: the CNT weight percent concentration in the electrophoresis solution is: 0.1%, and solvent is an acetone, and charged auxiliary salt is a magnesium nitrate, and concentration is 1-10 * 10
-4Mol/L, electrode cathode are sample, and anode is a stainless sheet steel.Apply electric field strength 5-15V/cm during electrophoretic deposition, the time is 2-4 minute.
Said dielectric layer heat treatment is: heat treatment under the vacuum, parameter: 300-500 ℃, 1 hour.
Beneficial effect of the present invention is:
1. improved the coverage of dielectric layer, improved the restriction of device the ionization electric current on electrode sidewall and monodimension nanometer material surface.
2. in the electrophoretic deposition CNT, form dielectric layer, help simplifying technology, reduce cost.
3. magnesia has anti-preferably ion bombardment ability, can further improve the working life of device.
Embodiment
Elaborate in the face of embodiments of the invention down: present embodiment provided detailed execution mode and process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.
Embodiment 1
Present embodiment is implemented under following implementation condition and specification requirement:
1. prepare 3-dimensional metal micro discharge electrode;
Adopt insulating glass as substrate, at first adopt photoetching process to form the photoresist figure of micro discharge electrode at substrate surface, sputtering sedimentation metal seed layer above that then obtains the Seed Layer electrode pattern after removing photoresist with stripping technology.The seed layer materials of selecting for use is Cu/Ti, and Cu thickness 0.12um, Ti thickness are 0.03um.On the above-mentioned sample that the Seed Layer electrode pattern arranged, adopt photoetching process, form photoresist mask plating figure, the photoresist height is 10um.Above-mentioned sample is put into a watt nickel plating solution, and as negative electrode, the nickel plate is as anode with it, and applying electroplating current density is 0.2A/dm
2, the time is 30 minutes, and obtaining electrode width is 20um, and length is 2000um, and electrode spacing is 10um, highly is the nickel sparking electrode of 5um.
2. electrophoretic deposition CNT and dielectric layer;
On the Ni electrode that 1 step obtains, adopt the electrophoresis method deposition of carbon nanotubes.The parameter of electrophoretic deposition is: the CNT weight percent concentration in the electrophoresis solution is 0.1%, and solvent is an acetone, and magnesium nitrate concentration is 1 * 10
-4Mol/L, negative electrode are deposited samples, and anode is a stainless sheet steel.Apply electric field strength 15V/cm during electrophoretic deposition, the time is 2 minutes.
3. dielectric layer heat treatment;
To put into vacuum annealing furnace through the sample of 2 steps, carry out thermal decomposition process, 300 ℃ of annealing temperatures, 1 hour time.
The micro discharge electrode spacing that present embodiment prepares is 10 microns, and electrode surface has covered uniform CNT, and the oxidized magnesium crystal grain of carbon nano tube surface coats, but still has kept the pattern of CNT.Ionization performance to device is tested, and the ionization threshold voltage is lower than 10V, and the ionization current peak is less than 10uA, explains that ionization not only takes place under lower voltage device, and dielectric layer has good inhibition effect to the growth of ionization electric current.
Embodiment 2
Present embodiment is implemented under following implementation condition and specification requirement condition:
1. prepare 3-dimensional metal micro discharge electrode;
The high resistance glass that adopts insulation is as substrate, at first adopts photoetching process to form the photoresist figure of sparking electrode at substrate surface, and sputtering sedimentation metal seed layer is above that removed photoresist with stripping technology then, obtains the Seed Layer electrode structure.The seed layer materials of selecting for use is Cu/Ti, and Cu thickness 0.12um, Ti thickness are 0.03um.Then, have in preparation on the sample of Seed Layer, adopt photoetching process, form photoresist mask plating figure, the photoresist height is 15um.Above-mentioned sample is put into a watt nickel plating solution, and as negative electrode, the nickel plate is as anode with it, and applying electroplating current density is 0.2A/dm
2, the time is 60 minutes, and obtaining electrode width is 20um, and length is 2000um, and electrode spacing is 15um, highly is the nickel sparking electrode of 10um.
2. electrophoretic deposition CNT and dielectric layer;
On the Ni electrode that step 1 obtains, adopt the electrophoresis method deposition of carbon nanotubes.The parameter of electrophoretic deposition is: the CNT weight percent concentration in the electrophoresis solution is 0.1%, and solvent is an acetone, and magnesium nitrate concentration is 5 * 10
-4Mol/L, negative electrode are deposited samples, and anode is a stainless sheet steel.Apply electric field strength 10V/cm during electrophoretic deposition, the time is 3 minutes.
3. dielectric layer heat treatment;
To pass through the sample of step 2 and put into vacuum annealing furnace, carry out thermal decomposition process, 400 ℃ of annealing temperatures, 1 hour time.
The micro discharge electrode electricity die opening that present embodiment prepares is 15 microns, and electrode surface covers uniform CNT, and the oxidized magnesium crystal grain of carbon nano tube surface coats, but still keeps the CNT pattern.Ionization performance to device is tested, and the ionization threshold voltage is lower than 10V, and the ionization current peak is less than 10uA, explains that ionization not only takes place under lower voltage device, and dielectric layer has good inhibition effect to the growth of ionization electric current.
Embodiment 3
Present embodiment is implemented under following implementation condition and specification requirement condition:
1. prepare 3-dimensional metal micro discharge electrode;
Adopt surface deposition the silicon chip of silicon oxide layer as substrate, at first adopt photoetching process to form the photoresist figure of sparking electrode at substrate surface, sputtering sedimentation metal seed layer is above that removed photoresist with stripping technology then, obtains the Seed Layer electrode structure.The seed layer materials of selecting for use is Cu/Ti, and Cu thickness 0.12um, Ti thickness are 0.03um.Then, depositing on the sample of Seed Layer, adopting photoetching process, forming photoresist mask plating figure, the photoresist height is 20um.Above-mentioned sample is put into a watt nickel plating solution, and as negative electrode, the nickel plate is as anode with it, and applying electroplating current density is 0.2A/dm
2, the time is 90 minutes, and obtaining electrode width is 20um, and length is 2000um, and electrode spacing is 20um, highly is the nickel sparking electrode of 15um.
2. electrophoretic deposition CNT and dielectric layer;
On the Ni electrode that step 1 obtains, adopt the electrophoresis method deposition of carbon nanotubes.The parameter of electrophoretic deposition is: the CNT weight percent concentration in the electrophoresis solution is 0.1%, and solvent is an acetone, and magnesium nitrate concentration is 10 * 10
-4Mol/L, negative electrode are deposited samples, and anode is a stainless sheet steel.Apply electric field strength 5V/cm during electrophoretic deposition, the time is 4 minutes.
3. dielectric layer heat treatment;
To pass through the sample of step 2 and put into vacuum annealing furnace, carry out thermal decomposition process.500 ℃ of annealing temperatures, 1 hour time.
The micro discharge electrode electricity die opening that present embodiment prepares is 20 microns, and electrode surface covers uniform CNT, and the oxidized magnesium crystal grain of carbon nano tube surface coats, but still presents the CNT pattern.Ionization performance to device is tested, and the ionization threshold voltage is lower than 10V, and the ionization current peak is less than 10uA, explains that ionization not only takes place under lower voltage device, and dielectric layer has good inhibition effect to the growth of ionization electric current.
Although content of the present invention has been done detailed introduction through above-mentioned preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple modification of the present invention with to substitute all will be conspicuous.Therefore, protection scope of the present invention should be limited appended claim.
Claims (9)
1. the method on a deposition medium barrier layer on the micro-nano electrode comprises the steps:
Step 1, the three-dimensional micro discharge electrode of preparation on substrate;
Step 2 adopts electrophoresis method, and the deposition monodimension nanometer material also forms dielectric layer simultaneously on above-mentioned three-dimensional micro discharge electrode, adds excessive charged auxiliary salt magnesium nitrate in the electrophoresis liquid, and dielectric layer is a magnesia;
Step 3, dielectric layer heat treatment.
2. according to claim 1 on the micro-nano electrode method on deposition medium barrier layer, it is characterized in that said step 1 is specially: adopt the method for photoetching, thin film deposition, photoresist lift off, the plating seed layer of preparation micro discharge electrode pattern on substrate; Adopt the method for mask plating, on above-mentioned Seed Layer, electroplate three-dimensional micro discharge electrode.
3. according to claim 1 and 2 on the micro-nano electrode method on deposition medium barrier layer, it is characterized in that said substrate is a glass, or High Resistivity Si, or pottery or surface deposition have the substrate of insulating material.
4. according to claim 1 and 2 on the micro-nano electrode method on deposition medium barrier layer, it is characterized in that, said micro discharge electrode, right for the anodic-cathodic that one or more pairs of parallel microelectrodes are formed, make by electric conducting material.
5. according to claim 4 on the micro-nano electrode method on deposition medium barrier layer, it is characterized in that said three-dimensional micro discharge electrode pair is of a size of width 20um, length 2000um, spacing 10-20um, height 5-15um.
6. according to claim 1 on the micro-nano electrode method on deposition medium barrier layer, it is characterized in that said one-dimensional material is a kind of in CNT, silicon carbide nanometer line, silicon nanowires, the zinc oxide nanowire.
7. according to claim 6 on the micro-nano electrode method on deposition medium barrier layer, it is characterized in that said one-dimensional material is a CNT.
8. according to claim 1 on the micro-nano electrode method on deposition medium barrier layer; It is characterized in that the parameter of said electrophoresis method is: the CNT weight percent concentration in the electrophoresis solution is 0.1%, and solvent is an acetone; Charged auxiliary salt is a magnesium nitrate, and concentration is 1-10 * 10
-4Mol/L, electrode cathode are sample, and anode is a stainless sheet steel; Apply electric field strength 5-15V/cm during electrophoretic deposition, the time is 2-4 minute.
9. according to claim 1 on the micro-nano electrode method on deposition medium barrier layer, it is characterized in that said dielectric layer heat treatment is: heat treatment under the vacuum condition, parameter: 300-500 ℃, 1 hour.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102933015A (en) * | 2012-11-16 | 2013-02-13 | 上海交通大学 | Polarization-enhanced discharge electrode formed by one-dimensional nanostructures |
| CN103079328A (en) * | 2012-12-31 | 2013-05-01 | 云南航天工业有限公司 | Dielectric barrier discharge electrode and manufacture method of dielectric barrier discharge electrode |
| CN109782103A (en) * | 2019-03-11 | 2019-05-21 | 潘元志 | The alignment methods and system of probe and pin of electronic device |
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| CN1617954A (en) * | 2001-11-30 | 2005-05-18 | 北卡罗来纳-查佩尔山大学 | Deposition method for nanostructure materials |
| US6902658B2 (en) * | 2001-12-18 | 2005-06-07 | Motorola, Inc. | FED cathode structure using electrophoretic deposition and method of fabrication |
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| CN1617954A (en) * | 2001-11-30 | 2005-05-18 | 北卡罗来纳-查佩尔山大学 | Deposition method for nanostructure materials |
| US6902658B2 (en) * | 2001-12-18 | 2005-06-07 | Motorola, Inc. | FED cathode structure using electrophoretic deposition and method of fabrication |
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| JIAHAO WU ET AL: "A MEMS-Based Ionization Gas Sensor Using Carbon Nanotubes and Dielectric Barrier", 《NANO/MICRO ENGINEERED AND MOLECULAR SYSTEMS, 2008. NEMS 2009. 4TH IEEE INTERNATIONAL CONFERENCE ON》, 8 January 2008 (2008-01-08) * |
| SANUK PIMANPANG ET ALL: "Influences of magnesium particles incorporated on electrophoretically multiwall carbon nanotube film on dye-sensitized solar cell performance", 《SYNTHETIC METALS》, vol. 159, no. 1920, 15 August 2009 (2009-08-15), pages 1996 - 2000 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102933015A (en) * | 2012-11-16 | 2013-02-13 | 上海交通大学 | Polarization-enhanced discharge electrode formed by one-dimensional nanostructures |
| CN103079328A (en) * | 2012-12-31 | 2013-05-01 | 云南航天工业有限公司 | Dielectric barrier discharge electrode and manufacture method of dielectric barrier discharge electrode |
| CN103079328B (en) * | 2012-12-31 | 2015-10-07 | 云南航天工业有限公司 | A kind of medium blocking discharge electrode and preparation method thereof |
| CN109782103A (en) * | 2019-03-11 | 2019-05-21 | 潘元志 | The alignment methods and system of probe and pin of electronic device |
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Application publication date: 20120404 |