CN108584865A - A kind of production method of control method and its ion detector based on the arrangement of overlength molybdenum oxide nanowires array - Google Patents
A kind of production method of control method and its ion detector based on the arrangement of overlength molybdenum oxide nanowires array Download PDFInfo
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- CN108584865A CN108584865A CN201810512799.0A CN201810512799A CN108584865A CN 108584865 A CN108584865 A CN 108584865A CN 201810512799 A CN201810512799 A CN 201810512799A CN 108584865 A CN108584865 A CN 108584865A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B7/00—Microstructural systems; Auxiliary parts of microstructural devices or systems
- B81B7/04—Networks or arrays of similar microstructural devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00023—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems without movable or flexible elements
- B81C1/00031—Regular or irregular arrays of nanoscale structures, e.g. etch mask layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B2201/00—Specific applications of microelectromechanical systems
- B81B2201/02—Sensors
Abstract
The present invention relates to the production methods of a kind of control method based on the arrangement of overlength molybdenum oxide nanowires array and its ion detector, including：To the arrangement of overlong nanowire, the making of ion detector further includes the steps that the design of microchannel and preparation and device assemble for the preparation of overlength molybdenum oxide nanowires, the preparation of electrode, dielectrophoresis.It is interelectrode lengthy and jumbled that the method had both solved the problems, such as that nano wire friendship different in size was disorderly arranged in, also improve and optimize nano wire microelectrode over-assemble stability.Come to carry out a responsive type detection to different ions in combination with the novel chips laboratory such as microchannel.The present invention, which both can be applicable in microchannel, forms effective array detection different ions concentration, it can also be used among the preparation of hydrogen sensitive element, can effectively improve the performance of hydrogen sensing.
Description
Technical field
The invention belongs to field of inorganic nano material, exist in particular for a kind of overlength orthorhombic phase molybdenum trioxide nano wire
The production method of the control method and its ion detector of effective arrangement form array on microelectrode.
Background technology
Dielectrophoresis technology is a kind of novel effective technology for manipulating small molecule and nano material, and this technology is
Dielectrophoresis technology is successfully improved to by traditional electrophoretic techniques, in contrast dielectrophoresis technology to the collection of particle with detach
Aspect has clear advantage, i.e.,：Traditional dielectric swimming and two kinds of control modes of traveling wave dielectrophoresis are integrated, are situated between with tradition
Electrophoresis (DEP, dielectrophoresis) is compared, and traveling wave dielectrophoresis is not necessarily to additional fluid driving equipment, can divide in principle
From a variety of particles, it can realize and detect and be easy to integrate combination with microchip in real time and be used.Dielectrophoresis technology is
In the experiments such as the array arrangement through being widely used in bio-molecular separation and electrodeless nano material, and achieve prodigious
Effect.
From the point of view of a current development trend, dielectrophoresis technology has breached a pass of theoretical property, and constantly into
What row one was deeply changed probes into, and can effectively be separated biological micromolecule using the technology, can also be by nano material
It is moved to designated position in effective dispersion solvent.This technology can also be expanded to various domain variabilities and be used in the future.This
Kind manipulation is technically simple, and effectively equipment is easy to build, while having to the manipulation of biomolecule and inorganic nano material apparent
Controllability.Such as LeungSiu Ling et al. carry out ordered arrangement gold nano grain to study a kind of heat with the method for dielectrophoresis
Sensor (Gold nano-particle-based thermal sensors fabricated using
microspotting and DEP techniques.《Sensors and Actuators A:Physical》,178：32-39
(2012)), this control method is persistently arranged just for one kind of nano particle, and LiuLu et al. has used this technology
A kind of arrangement has been carried out to carbon nanotube, and has tested the ph sensing capabilities (High of this carbon nano pipe array
performance flexible pH sensor based on carboxyl-functionalized and DEP
aligned SWNTs.《Applied Surface Science》, 386：405-411 (2016)), this carbon nanotube has
Effect length can not directly be built at electrode both ends, while also need to a kind of arrangement effect of lasting research carbon nanotube, most
The fruit that terminates is also slightly aobvious lengthy and jumbled.Therefore a kind of reasonable and effective implementing method is needed to make up this shortcoming.
Invention content
The present situation of cell and small inorganic nano material is detached based on dielectrophoresis technology, the purpose of the present invention is to provide
A kind of manipulation means of ordered arrangement overlong nanowire, and attempt to make ion detector with this technology to improve detection
Efficiency.Both it is interelectrode lengthy and jumbled to have solved the problems, such as that nano wire friendship different in size was disorderly arranged in, has also improved and optimizes nano wire and exist
The stability of microelectrode over-assemble.Come to carry out a sensitivity to different ions in combination with the novel chips laboratory such as microchannel
Type detects.The present invention, which both can be applicable in microchannel, forms effective array detection different ions concentration, it can also be used in hydrogen
Among the preparation of sensing element, the performance of hydrogen sensing can be effectively improved.
In order to achieve the above objectives, technical solution provided by the invention is：
A kind of control method based on the arrangement of overlength molybdenum oxide nanowires array, which is characterized in that include the following steps：
Step 1, the preparation of overlength molybdenum oxide nanowires：
Using conventional hydrothermal synthesis technology, using water under the high temperature and pressure of 180~220 DEG C of two molybdic acid hydrate sodium and nitric acid
Deionized water is added in thermal synthesis in ptfe autoclave first, make the volume of water account for reaction kettle volume 60%~
80%, magneton is added, is placed on magnetic stirring apparatus and is stirred, then by two molybdic acid hydrate sodium and concentrated nitric acid according to molar ratio
It is 8：1~10：1 amount, which is added in reaction kettle, is mixed 30~60min, finally puts on metal reaction kettle outside and is placed in
8~12h is kept the temperature in hydro-thermal baking oven at 180~220 DEG C, finally wash repeatedly sample with deionized water and is dried, obtaining appearance is
The molybdenum oxide nanowires of white powder.
Step 2, the preparation of electrode：
After quartz glass plate is cleaned, drying, titanium/platinum microelectrode, designing mask are produced using photoetching process on it
Version electrode length is 10mm, and the spacing between two electrodes is 10 μm.
Step 3, arrangement of the dielectrophoresis to overlong nanowire：
3.1) preparation of dielectrophoresis laboratory apparatus：Using one, pc computers, CCD, light microscope, probe base, power
Pc computers and CCD and light microscope are connected together and constitute a real-time observation device, by work(by generator, power amplifier
Rate generator links together with power amplifier and constitutes output source, directly connects output source when being manipulated to nano wire
It is connected on probe base and output is provided.
3.2) weigh appropriate molybdenum trioxide nano-wire powder and deionized water is added and obtain certain density molybdenum oxide nanometer
Line dispersion liquid, and ultrasound makes dispersion liquid full and uniform；
3.3) the molybdenum oxide nanowires dispersion liquid for taking 8~10 μ L steps 3.2) to obtain is obtained using pipettor drop in step 2
The electrode center arrived, is joined using power generator and power amplifier 210~300s of extra electric field, and using dielectric appropriate
Electrode, is finally placed among clean culture dish and waits for that water droplet is evaporated naturally, be placed in annealing furnace and carry out annealing reinforcement by number manipulation
The connectivity of nano wire and electrode obtains the molybdenum oxide nanowires array of ordered arrangement.
Further, the molybdenum oxide nanowires powder in the step 3.2) mixes the molybdenum oxide generated with deionized water
Nanowire dispersion a concentration of 5 × 10-5~2 × 10-4mol/L。
Further, the ultrasonic time in the step 3.2) is 5~10min.
Further, use the time of power generator and power amplifier extra electric field for 150 in the step 3.3)
~300s.
Further, the dielectric parameter used in the step 3.3) for the different gradient alternating voltages of 1~7v, 1~
The different gradient a-c cycles of 10KHz.
Further, it is 200~300 DEG C that the temperature range annealed in annealing furnace is placed in the step 3.3).
The production method of a kind of ion detector using above-mentioned overlength molybdenum oxide nanowires array, which is characterized in that also
Include the following steps：
Step 4：The design and preparation of microchannel：
4.1) substrate cleans：It is that 20 × 20 × 2mm quartz glass plates are sequentially placed into acetone, ethyl alcohol, deionized water to take thickness
It is cleaned by ultrasonic 20~30min respectively, last deionized water is outwelled after ultrasound is complete, ethyl alcohol is added；
4.2) photoetching making microchannel mother matrix：It is placed on after taking the quartz glass plate after cleaning to be dried up with nitrogen on baking platform
90~110 DEG C of 5~8min of baking, remove 5~10min of postcooling, SU-8 photoresists, wherein sol evenning machine are coated on sol evenning machine
Rotating speed is to turn 40s with 850~950rpm, is painted with after glue on drying platform to be warming up to 100 after 65~80 DEG C of 20~25min of baking
~120 DEG C of 120~140min of baking, remove and cool down 10~12min or so again, take the microchannel mask plate that designed in advance is good
18~20s is exposed on litho machine, the wherein width in the mainstream channel of microchannel mask plate is 200 μm, and cavity is a diameter of
The cylinder of 4mm, after having exposed again on drying platform to be warming up to 85~100 DEG C of bakings 50 after 65~80 DEG C of 20~25min of baking
Then~60min cools down 10~12min and develops in developer solution 5~15min, nitrogen drying is rinsed with isopropanol after taking-up,
Finally enhance the connectivity of photoresist on drying platform with 120~135 DEG C of 120~140min of post bake.
Step 5：Device assembles：
Other than taking front to do top electrode and carrying out the electrode of array arranging nano-wire by DEP and wipe electrode with cotton swab
Partial nano wire, and in 200~300 DEG C of high temperature air annealing to reinforce nano wire crystallinity and the connection between electrode
Property, it takes the ready-made PDMS microchannels in front to be placed on together among plasma cleaning instrument, opens vacuum pump, screw exhaust rotation
Button starts timing after the appearance of pink light, mark is directed at the cross on the channels PDMS according to substrate after being taken out after 2~4 minutes
Compressed after alignment fitting and keep 12~so that substrate is permanently bonded together with PDMS for 24 hours.
The purpose that is reached of the present invention is with advantageous effect：
(1) a kind of single batch of overlong nanowire is introduced into electrode both ends, connects to reducing by more nano wires and brings
Crystal boundary contact problems are to influence detection efficiency；
(2) at the same manipulate more nano wires be arranged separately on electrode both ends formed array, to promote nano material pair
Application efficiency in terms of gas sensing property and other biological；
(3) nano-wire array that different arrangements can be manipulated out according to different electrode shapes, to reach demand；
(4) be subject to the application of microchannel, make whole device improved in terms of biological detection it is prodigious can anti-interference.
(5) the overlength MoO prepared3Even millimeter is controllable, and made respectively to nano wire from nanometer to micron
Nanowire diameter it is relatively uniform, this is above to provide a great convenience in the utilization of dielectrophoresis technology, while its overlength is received
Rice noodles also provide feasibility for single build in Different electrodes spacing.
(6) this manipulation technology strengthens the contact force between metal-oxide semiconductor (MOS) and metal, that is, solves nanometer
Line friendship different in size is disorderly arranged in interelectrode lengthy and jumbled problem, also improves and optimizes nano wire in the steady of microelectrode over-assemble
It is qualitative.Come to carry out a responsive type detection to different ions in combination with the novel chips laboratory such as microchannel.The present invention both may be used
It applies and forms effective array detection different ions concentration in microchannel, it can also be used to prepare it in hydrogen sensitive element
In, the performance of hydrogen sensing can be effectively improved.
Description of the drawings
Attached drawing 1 is the scanning electron microscope schematic diagram of molybdenum oxide nanowires provided in an embodiment of the present invention；
Attached drawing 2 is electrode mask plate figure (left side) designed in the present invention and makes the reality after electrode by the mask plate
Object figure (right side)；
Attached drawing 3 is the test device figure of intermediary's electrophoresis manipulation overlength molybdenum oxide nanowires of the present invention；
Attached drawing 4 is the scanning electron microscope schematic diagram to nano wire manipulation result in the present invention；
Attached drawing 5 is the scanning type of the different dispersion liquid concentration influences that nano-wire array arranges between electrode in the present invention
Electron microscope schematic diagram；
Attached drawing 6 is the scanning type electricity of the different alternating voltage influences that nano-wire array arranges between electrode in the present invention
Sub- microscope schematic diagram；
Attached drawing 7 is the scanning type electricity of the different a-c cycle influences that nano-wire array arranges between electrode in the present invention
Sub- microscope schematic diagram；
Attached drawing 8 is microchannel mask shape (left side) used in the present invention, device pictorial diagram after making (in) with
And graphical three-dimensional schematic diagram (right side)；
Attached drawing 9 is the conductance figure of the units test blank control group and sample sets for detecting ion in the present invention.
Specific implementation mode
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention
Content is not limited solely to the following examples.Those skilled in the art can make various modifications or changes to the present invention, these
Equivalent form is equally listed by the application within the scope of claims limited.
Embodiment 1：
Step 1：The preparation of overlength molybdenum oxide nanowires：
Using hydro-thermal synthesis process, with hydrothermal synthesis under the high temperature and pressure of 180 DEG C of two molybdic acid hydrate sodium and nitric acid, first
32.75mL deionized waters are added in the ptfe autoclave of 50ml, magneton is added, is placed on magnetic stirring apparatus and carries out
Stirring, takes the two molybdic acid hydrate sodium of 2.4196g (0.01mol) to be placed in reaction kettle, and the dense nitre of 6.25mL (0.1mol) is added
Acid, it is 10 to make the molar ratio of two molybdic acid hydrate sodium and concentrated nitric acid：1, mixing, which is added in reaction kettle, is mixed 30min, takes out magnetic
Son puts on metal reaction kettle and is placed in 180 DEG C of heat preservation 12h in hydro-thermal baking oven, finally washes repeatedly sample with deionized water, obtain
To the molybdenum oxide nanowires that appearance is white powder.
Step 2：The preparation of electrode：
2.1) substrate cleans：Be 15mm by length and width, the quartz glass plate that thickness is 2mm be sequentially placed into acetone, alcohol,
Respectively it is cleaned by ultrasonic 30min in deionized water under room temperature, outwells last deionized water after ultrasound is complete, be put into after being dried up with nitrogen
70 DEG C of drying 30min, are put into clean culture dish and preserve in baking oven；
Quartz glass is current market sales of product；
Cleaning agent used in quartz glass cleaning is analysis pure acetone, the pure absolute ethyl alcohol of analysis and deionized water；
Ultrasound Instrument is current market sales of product used in being cleaned by ultrasonic；
2.2) photoetching process：It takes the quartz glass plate after cleaning to be put into ethyl alcohol after the leaching several seconds, is placed on after being dried up with nitrogen
It dries and toasts 3-5min on platform, remove postcooling 5min or so, AZ5214 photoresists are coated on sol evenning machine, wherein sol evenning machine turns
Speed toasts 120s after being painted with glue for first turn 6s with 600rpm turns 30s with 2000rpm again on drying platform, and it is left to remove again cooling 5min
The right side, then the electrode mask plate that takes designed in advance good expose 3s on litho machine, and the length of electrode is 10mm, between two electrodes
Spacing be 10 μm, toast 90s on drying platform again after expose, then cooling 3min or so, then in the case of no mask plate
10s is exposed on litho machine, finally develop 60s in developer solution, observation using develop completely after after aobvious 10s as principle, taking-up
Afterwards with deionized water rinse nitrogen drying after again dry platform on post bake 120s；
Experiment AZ5214 photoresists used are the products sold in the market by negtive photoresist；
2.3) sputtering technology：The substrate that photoetching was done in front is taken to use mark under conditions of Ar atmosphere and 80W sputtering powers
Accurate sputtering technology first sputters the platinum that 25s titaniums sputter 80s again on surface；
The DC magnetron sputtering device that the present invention uses is current market sales of equipment；
2.4) stripping of photoresist：It takes the substrate after sputtering to impregnate in acetone, and carries out ultrasonic removal in ultrasonic machine
As soon as falling layer platinum on photoresist and photoresist, the part without photoresist keeps down to form electrode.
AZ5214 photoresists are current market sales of products；
Sol evenning machine used in gluing is current market sales of product；
Baking baking platform used is current market sales of product；
Litho machine used in photoetching is the product of American AB M, Inc. companies.
Step 3：Arrangement of the dielectrophoresis to overlong nanowire：
3.1) quantitative molybdenum oxide nanowires powder is weighed respectively and is separately added into deionized water obtains molybdenum oxide nanowires
Dispersion liquid, ultrasound 5 minutes and stir make dispersion liquid full and uniform；
3.2) pipettor is used to instill quantitative 10 μ L in electrode center, extra electric field 300s, after electrode is placed in it is clean
It waits for that water droplet is evaporated naturally among net culture dish, is placed in the connection that 200 DEG C of annealing 2h in annealing furnace reinforce nano wire and electrode
Property.
Taking the device after annealing to be placed in prevents from shaking from adsorption box, and whole region nanowire alignment situation is by scanning
Formula electron microscope shoots and records；
Using identical additional AC field and a-c cycle, the molybdenum oxide dispersion liquid of various concentration instills 10 μ L dispersions
Liquid, according to the specific implementation parameter of such as table 1, obtains interelectrode nanowire alignment under different dispersion liquid concentrations in electrode center
Situation and in 200 DEG C of air anneal 2h, obtains scanning electron microscope result such as Fig. 5；
Table 1
Embodiment 2：
Step 1：The preparation of overlength molybdenum oxide nanowires：
Using hydro-thermal synthesis process, with hydrothermal synthesis under the high temperature and pressure of 200 DEG C of two molybdic acid hydrate sodium and nitric acid, first
35mL deionized waters are added in the ptfe autoclave of 50ml, magneton is added, is placed on magnetic stirring apparatus and is stirred
It mixes, takes the two molybdic acid hydrate sodium of 2.4196g (0.01mol) to be placed in reaction kettle, and the dense nitre of 5.6mL (0.09mol) is added
Acid, it is 9 to make the molar ratio of two molybdic acid hydrate sodium and concentrated nitric acid：1, mixing, which is added in reaction kettle, is mixed 45min, takes out magnetic
Son puts on metal reaction kettle and is placed in 200 DEG C of heat preservation 10h in hydro-thermal baking oven, finally washes repeatedly sample with deionized water, obtain
To the molybdenum oxide nanowires that appearance is white powder.
Step 2：The preparation of electrode：
2.1) substrate cleans：Be 15mm by length and width, the quartz glass plate that thickness is 2mm be sequentially placed into acetone, alcohol,
Respectively it is cleaned by ultrasonic 30min in deionized water under room temperature, outwells last deionized water after ultrasound is complete, be put into after being dried up with nitrogen
70 DEG C of drying 30min, are put into clean culture dish and preserve in baking oven；
Quartz glass is current market sales of product；
Cleaning agent used in quartz glass cleaning is analysis pure acetone, the pure absolute ethyl alcohol of analysis and deionized water；
Ultrasound Instrument is current market sales of product used in being cleaned by ultrasonic；
2.2) photoetching process：It takes the quartz glass plate after cleaning to be put into ethyl alcohol after the leaching several seconds, is placed on after being dried up with nitrogen
It dries on platform in baking 3-5min, removes postcooling 5min or so, AZ5214 photoresists, wherein sol evenning machine are coated on sol evenning machine
Rotating speed is that first turn 6s with 600rpm turns 30s with 2000rpm again, toasts 120s on drying platform after being painted with glue, removes and cool down 5min again
Left and right, then the electrode mask plate that takes designed in advance good expose 3s on litho machine, and the length of electrode is 10mm, two electrodes it
Between spacing be 10 μm, toast 90s on drying platform again after expose, then cooling 3min or so, then no mask plate the case where
Under 10s is exposed on litho machine, finally develop 60s in developer solution, observation using develop completely after after aobvious 10s as principle, take
After going out with deionized water rinse nitrogen drying after again dry platform on post bake 120s；
Experiment AZ5214 photoresists used are the products sold in the market by negtive photoresist；
2.3) sputtering technology：The substrate that photoetching was done in front is taken to use mark under conditions of Ar atmosphere and 80W sputtering powers
Accurate sputtering technology first sputters the platinum that 25s titaniums sputter 80s again on surface；
The DC magnetron sputtering device that the present invention uses is current market sales of equipment；
2.4) stripping of photoresist：It takes the substrate after sputtering to impregnate in acetone, and carries out ultrasonic removal in ultrasonic machine
As soon as falling layer platinum on photoresist and photoresist, the part without photoresist keeps down to form electrode.
AZ5214 photoresists are current market sales of products；
Sol evenning machine used in gluing is current market sales of product；
Baking baking platform used is current market sales of product；
Litho machine used in photoetching is the product of American AB M, Inc. companies.
Step 3：Arrangement of the dielectrophoresis to overlong nanowire：
3.1) quantitative molybdenum oxide nanowires powder is weighed respectively and is separately added into deionized water obtains molybdenum oxide nanowires
Dispersion liquid, ultrasound 5 minutes and stir make dispersion liquid full and uniform；
3.2) pipettor is used to instill quantitative 10 μ L in electrode center, extra electric field 300s, after electrode is placed in it is clean
It waits for that water droplet is evaporated naturally among net culture dish, is placed in the connectivity that nano wire and electrode are reinforced in 250 DEG C of annealing in annealing furnace.
Taking the device after annealing to be placed in prevents from shaking from adsorption box, and whole region nanowire alignment situation is by scanning
Formula electron microscope shoots and records；
Using identical additional a-c cycle and dispersion liquid concentration, different AC fields instills 10 μ L dispersion liquids in electricity
It is extremely central, according to the specific implementation parameter of such as table 2, obtain under different alternating voltages interelectrode nanowire alignment situation and
250 DEG C of air anneal 1.5h obtain scanning electron microscope result such as Fig. 6；
Table 2
Embodiment 3：
Step 1：The preparation of overlength molybdenum oxide nanowires：
Using hydro-thermal synthesis process, with hydrothermal synthesis under the high temperature and pressure of 220 DEG C of two molybdic acid hydrate sodium and nitric acid, first
38mL deionized waters are added in the ptfe autoclave of 50ml, magneton is added, is placed on magnetic stirring apparatus and is stirred
It mixes, takes the two molybdic acid hydrate sodium of 2.4196g (0.01mol) to be placed in reaction kettle, and the concentrated nitric acid of 5mL (0.08mol) is added,
It is 8 to make the molar ratio of two molybdic acid hydrate sodium and concentrated nitric acid：60min is mixed in 1 addition reaction kettle, takes out magneton, puts on gold
Belong to reaction kettle and be placed in 220 DEG C of heat preservation 8h in hydro-thermal baking oven, finally washes repeatedly sample with deionized water, it is white to obtain appearance
The powdered molybdenum oxide nanowires of color.
Step 2：The preparation of electrode：
2.1) substrate cleans：Be 15mm by length and width, the quartz glass plate that thickness is 2mm be sequentially placed into acetone, alcohol,
Respectively it is cleaned by ultrasonic 30min in deionized water under room temperature, outwells last deionized water after ultrasound is complete, be put into after being dried up with nitrogen
70 DEG C of drying 30min, are put into clean culture dish and preserve in baking oven；
Quartz glass is current market sales of product；
Cleaning agent used in quartz glass cleaning is analysis pure acetone, the pure absolute ethyl alcohol of analysis and deionized water；
Ultrasound Instrument is current market sales of product used in being cleaned by ultrasonic；
2.2) photoetching process：It takes the quartz glass plate after cleaning to be put into ethyl alcohol after the leaching several seconds, is placed on after being dried up with nitrogen
It dries on platform in baking 3-5min, removes postcooling 5min or so, AZ5214 photoresists, wherein sol evenning machine are coated on sol evenning machine
Rotating speed is that first turn 6s with 600rpm turns 30s with 2000rpm again, toasts 120s on drying platform after being painted with glue, removes and cool down 5min again
Left and right, then the electrode mask plate that takes designed in advance good expose 3s on litho machine, and the length of electrode is 10mm, two electrodes it
Between spacing be 10 μm, toast 90s on drying platform again after expose, then cooling 3min or so, then no mask plate the case where
Under 10s is exposed on litho machine, finally develop 60s in developer solution, observation using develop completely after after aobvious 10s as principle, take
After going out with deionized water rinse nitrogen drying after again dry platform on post bake 120s；
Experiment AZ5214 photoresists used are the products sold in the market by negtive photoresist；
2.3) sputtering technology：The substrate that photoetching was done in front is taken to use mark under conditions of Ar atmosphere and 80W sputtering powers
Accurate sputtering technology first sputters the platinum that 25s titaniums sputter 80s again on surface；
The DC magnetron sputtering device that the present invention uses is current market sales of equipment；
2.4) stripping of photoresist：It takes the substrate after sputtering to impregnate in acetone, and carries out ultrasonic removal in ultrasonic machine
As soon as falling layer platinum on photoresist and photoresist, the part without photoresist keeps down to form electrode.
AZ5214 photoresists are current market sales of products；
Sol evenning machine used in gluing is current market sales of product；
Baking baking platform used is current market sales of product；
Litho machine used in photoetching is the product of American AB M, Inc. companies.
Step 3：Arrangement of the dielectrophoresis to overlong nanowire：
3.1) quantitative molybdenum oxide nanowires powder is weighed respectively and is separately added into deionized water obtains molybdenum oxide nanowires
Dispersion liquid, ultrasound 5 minutes and stir make dispersion liquid full and uniform；
3.2) pipettor is used to instill quantitative 10 μ L in electrode center, extra electric field 300s, after electrode is placed in it is clean
It waits for that water droplet is evaporated naturally among net culture dish, is placed in the connectivity that nano wire and electrode are reinforced in 300 DEG C of annealing in annealing furnace.
Taking the device after annealing to be placed in prevents from shaking from adsorption box, and whole region nanowire alignment situation is by scanning
Formula electron microscope shoots and records；
Using identical additional AC field and dispersion liquid concentration, different a-c cycles instills 10 μ L dispersion liquids in electricity
It is extremely central, according to the specific implementation parameter of such as table 3, obtain under different a-c cycles interelectrode nanowire alignment situation and
300 DEG C of air anneal 1h obtain scanning electron microscope result such as Fig. 7.
Table 3
The making of ion detector
Embodiment 1,2,3 is combined and obtains optimum array and arranges and apply to step 4.2)
The making and assembling of step 4 device：
4.1) photoetching making microchannel mother matrix：It is placed on and is dried on platform at 100 DEG C after taking the glass slide after cleaning to be dried up with nitrogen
Toast 5min, remove postcooling 5min, coat SU-8 photoresists on sol evenning machine, wherein spin coating machine speed be with 850~
950rpm turns 40s, is painted with after glue on drying platform to be warming up to 100 DEG C of baking 120min after 70 DEG C of baking 20min, removes again cold
But 10~12min or so, the microchannel mask plate for taking designed in advance good expose 20s on litho machine, and wherein microchannel is covered
The width in the mainstream channel of diaphragm plate is 200 μm, and cavity is the cylinder of a diameter of 4mm, and the microchannel mask plate of design is shown in attached drawing
8 left figures, after having exposed again dry platform on 70 DEG C baking 20min after be warming up to 100 DEG C baking 50min, then cool down 10~
12min develops 5~15min in developer solution, and nitrogen drying is rinsed again on drying platform with 135 DEG C of post bakes with isopropanol after taking-up
120min。
Experiment SU-8 photoresists used are the products sold in the market by negtive photoresist；
4.2) it takes front to do top electrode and carries out the electrode of array arranging nano-wire by DEP and wipe electrode with cotton swab
With the nano wire of outer portion, and in 300 DEG C of high temperature air annealing to reinforce nano wire crystallinity and the connection between electrode
Property, it takes the ready-made PDMS microchannels in front to be placed on together among plasma cleaning instrument, opens vacuum pump, screw exhaust rotation
Button starts timing after the appearance of pink light, is directed at mark pair after being taken out after 4 minutes with the cross on the channels PDMS according to substrate
It is compressed after quasi- fitting and keeps 12h that substrate is made permanently to be bonded together with PDMS.
Step 5 is tested
Setting does the mask plate used in electrode with reference to figure 2, and electrode length 10mm, interelectrode spacing is 10 μm, mask
Plate appearance and size is that length and width are 30mm.The mask plate used in microchannel is done with reference to figure 8, sets mainstream channel width as b=
200 μm, mask plate appearance and size is that length and width are 30mm, goes out in water filling port and injects deionized water using the tasselled of 20 μ L/min
And the solion of various concentration, the resistance data of ammeter test are shown by LabVIEW softwares and are recorded in electricity in real time
On brain, as shown in Figure 9.
It should be noted that it will be understood by those of ordinary skill in the art that, technical scheme of the present invention can be carried out
Modification or equivalent replacement, without departing from the objective and range of technical solution of the present invention, the right that should all cover in the present invention is wanted
It asks in range.
Claims (7)
1. a kind of control method based on the arrangement of overlength molybdenum oxide nanowires array, which is characterized in that include the following steps：
Step 1, the preparation of overlength molybdenum oxide nanowires：
Using conventional hydrothermal synthesis technology, closed using hydro-thermal under the high temperature and pressure of 180~220 DEG C of two molybdic acid hydrate sodium and nitric acid
At, deionized water is added in ptfe autoclave first, the volume of water is made to account for reaction kettle volume 60%~80%, addition
Magneton is placed on magnetic stirring apparatus and is stirred, and is then 8 according to molar ratio by two molybdic acid hydrate sodium and concentrated nitric acid：1~10：1
Amount be added reaction kettle in be mixed 30~60min, finally put on metal reaction kettle outside and be placed in hydro-thermal baking oven
180~220 DEG C of 8~12h of heat preservation, finally wash repeatedly sample with deionized water and dry, and it is white powder to obtain appearance
Molybdenum oxide nanowires；
Step 2, the preparation of electrode：
After quartz glass plate is cleaned, drying, titanium/platinum microelectrode, designing mask version electricity are produced using photoetching process on it
Pole length is 10mm, and the spacing between two electrodes is 10 μm；
Step 3, arrangement of the dielectrophoresis to overlong nanowire：
3.1) preparation of dielectrophoresis laboratory apparatus：Occurred using one, pc computers, CCD, light microscope, probe base, power
Pc computers and CCD and light microscope are connected together and constitute a real-time observation device, power is sent out by device, power amplifier
Raw device links together with power amplifier constitutes output source, and output source is directly connected to spy when being manipulated to nano wire
Output is provided on needle pedestal；
3.2) weigh appropriate molybdenum trioxide nano-wire powder and deionized water is added and obtain certain density molybdenum oxide nanowires point
Dispersion liquid, and ultrasound makes dispersion liquid full and uniform；
3.3) the molybdenum oxide nanowires dispersion liquid for taking 8~10 μ L steps 3.2) to obtain drips the electricity obtained in step 2 using pipettor
It is extremely central, it is manipulated using power generator and power amplifier 210~300s of extra electric field, and using dielectric parameter appropriate,
Finally electrode is placed among clean culture dish and waits for that water droplet is evaporated naturally, be placed in annealing furnace carry out annealing reinforce nano wire with
The connectivity of electrode obtains the molybdenum oxide nanowires array of ordered arrangement.
2. the control method according to claim 1 based on the arrangement of overlength molybdenum oxide nanowires array, it is characterised in that：Institute
State the molybdenum oxide nanowires powder in step 3.2) mixed with deionized water generate molybdenum oxide nanowires dispersion liquid concentration be 5 ×
10-5~2 × 10-4mol/L。
3. the control method according to claim 1 based on the arrangement of overlength molybdenum oxide nanowires array, it is characterised in that：Institute
It is 5~10min to state the ultrasonic time in step 3.2).
4. the control method according to claim 1 based on the arrangement of overlength molybdenum oxide nanowires array, it is characterised in that：Institute
Stating in step 3.3) uses the time of power generator and power amplifier extra electric field for 150~300s.
5. the control method according to claim 1 based on the arrangement of overlength molybdenum oxide nanowires array, it is characterised in that：Institute
The dielectric parameter used in step 3.3) is stated as the different gradient alternating voltages of 1~7v, the different gradients exchange of 1~10KHz is frequently
Rate.
6. the control method according to claim 1 based on the arrangement of overlength molybdenum oxide nanowires array, it is characterised in that：Institute
It is 200~300 DEG C to state the temperature range for being placed in step 3.3) and annealing in annealing furnace.
7. a kind of ion detector using the overlength molybdenum oxide nanowires array as described in claim 1~6 any one
Production method, which is characterized in that further include following steps：
Step 4：The design and preparation of microchannel：
4.1) substrate cleans：It is that 20 × 20 × 2mm quartz glass plates are sequentially placed into acetone, ethyl alcohol, deionized water respectively to take thickness
It is cleaned by ultrasonic 20~30min, last deionized water is outwelled after ultrasound is complete, ethyl alcohol is added；
4.2) photoetching making microchannel mother matrix：Be placed on after taking the quartz glass plate after cleaning to be dried up with nitrogen dry on platform 90~
110 DEG C of 5~8min of baking, remove 5~10min of postcooling, SU-8 photoresists are coated on sol evenning machine, wherein spin coating machine speed is
Turn 40s with 850~950rpm, is painted with after glue on drying platform to be warming up to 100~120 DEG C after 65~80 DEG C of 20~25min of baking
120~140min is toasted, removes and cools down 10~12min or so again, the microchannel mask plate for taking designed in advance good is in litho machine
18~20s of upper exposure, the wherein width in the mainstream channel of microchannel mask plate are 200 μm, and cavity is the cylinder of a diameter of 4mm
Shape, after having exposed again on drying platform to be warming up to 85~100 DEG C of 50~60min of baking after 65~80 DEG C of 20~25min of baking, so
10~12min of postcooling develops 5~15min in developer solution, nitrogen drying is rinsed with isopropanol after taking-up, finally on drying platform
Enhance the connectivity of photoresist with 120~135 DEG C of 120~140min of post bake；
Step 5：Device assembles：
It takes front to do top electrode and carries out the electrode of array arranging nano-wire by DEP and wipe electrode with cotton swab with outer portion
Nano wire, and in 200~300 DEG C of high temperature air annealing to reinforce nano wire crystallinity and the connectivity between electrode, before taking
The ready-made PDMS microchannels in face are placed among plasma cleaning instrument together, are opened vacuum pump, are screwed exhaust knob, wait for pink
Light starts timing after occurring, after being directed at mark alignment fitting with the cross on the channels PDMS according to substrate after being taken out after 2~4 minutes
Compress and keep 12~so that substrate is permanently bonded together with PDMS for 24 hours.
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| CN109972087A (en) * | 2019-04-15 | 2019-07-05 | 华东师范大学 | A kind of preparation method of microelectrode deposition mask |
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