CN106945404A - Hot jet-printing head based on graphene composite structure of carbon nano tube and preparation method thereof - Google Patents
Hot jet-printing head based on graphene composite structure of carbon nano tube and preparation method thereof Download PDFInfo
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- CN106945404A CN106945404A CN201710200069.2A CN201710200069A CN106945404A CN 106945404 A CN106945404 A CN 106945404A CN 201710200069 A CN201710200069 A CN 201710200069A CN 106945404 A CN106945404 A CN 106945404A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2/00—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed
- B41J2/005—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by bringing liquid or particles selectively into contact with a printing material
- B41J2/01—Ink jet
- B41J2/135—Nozzles
- B41J2/16—Production of nozzles
- B41J2/1601—Production of bubble jet print heads
Abstract
The invention discloses a kind of hot jet-printing head based on graphene composite structure of carbon nano tube and preparation method thereof, the surface planarisation technique of zanjon is filled using ICP techniques and PDMS, main channel, ink jet chambers are prepared in silicon chip substrate, enter ink passage, nozzle, inkjet channel；Using anode linkage technique, using graphene fragment as intermediate layer, substrate of glass and silicon chip substrate are bonded.Main channel is connected with ink jet chambers by entering ink passage, and ink feed channel depth is less than ink jet chambers depth；Nozzle is arranged on ink jet chambers bottom；CNT graphene composite structure microbubble generator array and CNT array of temperature sensor are prepared in the region of the corresponding ink jet chambers of substrate of glass, and towards ink jet chambers setting.The shower nozzle feed liquor closes reliable, bond strength height, is difficult to pollute spray printing chamber, and precision is easily controllable during preparation.
Description
Technical field
The invention belongs to MEMS thermal jet print technical field, more particularly, to one kind based on graphene-carbon nanometer
Hot jet-printing head of pipe composite construction and preparation method thereof.
Background technology
Spray printing imaging technique has become large format Digital printing, digital photos printing, digital printing, color digital and drawn a design
And the preferred color hard copy technology of the colored output system of home and office intranets, acquisition be widely applied with huge business into
Work(.In addition to inkjet printing, the differential that Printing techniques can also provide non-contacting plurality of liquid is matched somebody with somebody, have widely should
With for example：Biofluid printing, making liquid crystal display colored filter, digitized manufacturing system PCB, drug injection and fuel note
Enter etc..It is expected to build integrated system (such as bioengineered tissue, big planar flexible flat device with sophisticated functions
Deng) provide it is a kind of from bottom to top, simple and effective embodiment.In a foreseeable future, high reliability, low cost of manufacture and
Micro- sprayed printed system of high-performance (high graphical quality, high frequency response and high spatial resolution) will be paid close attention to and
Commercial field and other special dimensions are used widely.
In existing Printing techniques, bubble type spray printing is a kind of easy Printing techniques based on micro-heater.Microbubble
Generator is the core of hot sprayed printed system, and the micro-heater based on traditional metal materials is mostly used at present, and power consumption is larger.Metal
CNT (CNT) is a kind of excellent microwave conductor, and the turn-on frequency of the CNT of single wall has report up to THz in theory
Road actually reaches GHz.
It is the topmost function of jet-printing head to produce spray printing liquid.Jet-printing head includes liquid-supplying system and injection liquid is produced
System.Liquid-supplying system, which ensures to provide to jet-printing head micro chamber according to certain pressure (static pressure), treats spray printing liquid；And spray printing liquid
Body generation system is actually a kind of pulse generation system, i.e., according to certain working frequency (digit pulse) in microcavity
Indoor one pulse (dynamic pressure) of generation, so as to will treat that spray printing liquid is extruded away from nozzle, forms spray printing drop.
In various driving sources, thermal spray printing is simple due to manufacture craft, be most application prospect method it
One, it has the advantages of very high spatial resolution, high-frequency response and low cost.Thermal technology is micro- using being produced on
Microheater in chamber, by electric pulse control, heating raises fluid temperature, so that the liquid gas of heater surfaces
Change and produce bubble, liquid is extruded away and forms injection drop by the pressure produced with bubble parameters from nozzle.Thermal spray printing
Device architecture is simple, and miniaturization is easy, it is possible to achieve higher nozzle integrated level, while cost of manufacture is relatively low.
Patent ZL201010160465.5《Jet-printing head based on double-carbon nanotube microbubble generator and preparation method thereof》
Disclose jet-printing head based on double-carbon nanotube microbubble generator and preparation method thereof.The program has following deficiency：
(1) carbon nano-tube tiny bubble generator uses metal electrode, there is Schottky barrier therebetween, contact resistance compared with
Greatly.
(2) microfluidic structures use the method that wet etching and dry etching are combined, and are difficult to control machining accuracy.
(3) enter ink passage identical with the chamber depth of sprayed printed unit, bubble valve close feed liquor exist closing loosely
Problem.
(4) double microbubble generators and microfluidic structures use ultra-violet curing bonding method, and bond strength is restricted；And
And spray printing chamber is easily polluted in the coating of uv-curable glue.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, the present invention is intended to provide a kind of feed liquor closes reliable, bonding
Intensity is high, be difficult pollution spray printing chamber, hot stamping shower nozzle easy to process and preparation method thereof.
To achieve the above object, the invention provides a kind of hot jet-printing head based on graphene-carbon nano tube composite structure,
Including：Substrate of glass, silicon chip substrate, main channel, enter ink passage, ink jet chambers, nozzle, inkjet channel, CNT-graphene
Composite construction microbubble generator array, CNT array of temperature sensor；Main channel, enter ink passage, ink jet chambers and be
The cavity of silicon chip substrate upper surface is opened in, main channel is connected with ink jet chambers by entering ink passage, and ink feed channel depth is small
In ink jet chambers depth；Inkjet channel is the cavity for being arranged on silicon chip substrate lower surface, and inkjet channel is located at the ink jet chambers back side；
Nozzle is arranged on ink jet chambers bottom, connection ink jet chambers and inkjet channel；CNT-graphene composite structure microbubble hair
Raw device array and CNT array of temperature sensor are prepared in the region of the corresponding ink jet chambers of substrate of glass, and towards ink-jet chamber
Room is set；Substrate of glass and silicon chip substrate is seamless is bonded together.
Further, single graphene-carbon nano tube composite structure microbubble generator includes：It is arranged on substrate of glass table
A pair of first Graphene electrodes in face；Connect the first CNT of a pair of first Graphene electrodes；By the first CNT two
End is fixed on a pair of the oneth SiO in a pair of first Graphene electrodes and substrate of glass2Mask layer.
Further, Single Carbon Nanotubes temperature sensor includes：It is arranged on a pair of metal electrodes of glass basic surface
Or a pair of second Graphene electrodes；Connect the second CNT of a pair of metal electrodes or a pair of second Graphene electrodes；By
Two CNT two ends are fixed in a pair of metal electrodes and substrate of glass, or in a pair of second Graphene electrodes and substrate of glass
A pair of the 2nd SiO2Mask layer.
Further, the intermediate layer of substrate of glass and the seamless bonding of silicon chip substrate is graphene fragment.
To achieve these goals, present invention also offers a kind of preparation method of foregoing hot jet-printing head, including following step
Suddenly：
(1) graphene-carbon nano tube composite structure microbubble generator array, CNT temperature are prepared on the glass substrate
Spend sensor array；
(2) the surface planarisation technique of zanjon is filled using ICP techniques and PDMS, is prepared in silicon chip substrate main logical
Road, ink jet chambers, enter ink passage, nozzle, inkjet channel；
(3) use anode linkage technique, using graphene fragment as intermediate layer, substrate of glass that step (1) is obtained and
The silicon chip substrate bonding that step (2) is obtained.
Further, CNT temperature sensor uses metal electrode, and step (1) includes following sub-step：
(1.1) magnetron sputtering and stripping technology are used, graphene-carbon nano tube composite structure is prepared on the glass substrate micro-
First test electrode of bubble generator array, the second test electrode of CNT array of temperature sensor, and carbon nanometer
The metal electrode of pipe array of temperature sensor；First test electrode, the second test electrode, the thickness of metal electrode for 100~
200nm；The spacing of metal electrode is 1~6 μm, and width is 1~5 μm；Metal electrode is identical with the second test number of electrodes, one by one
Correspondence connection；
(1.2) graphene of CVD growth on Copper Foil is transferred to by substrate of glass using spin coating PMMA wet method shifting process
On, the RIE etchings through photoetching and oxygen prepare the first stone of CNT-graphene composite structure microbubble generator array
Black alkene electrode；The spacing of first Graphene electrodes is 1~6 μm, and width is 1~5 μm, the first Graphene electrodes and the first test electricity
Number of poles is identical, connects one to one；
(1.3) AC signal of loading 1MHz, 16V on electrode are tested in microbubble generator, then CNT is suspended
Drop is between a pair of first Graphene electrodes of each graphene-carbon nano tube composite structure microbubble generator, and often
Between a pair of metal electrodes of individual CNT array of temperature sensor, by the micro- gas of each graphene-carbon nano tube composite structure
The first CNT in bubble generator is connected with corresponding a pair of first Graphene electrodes；By each CNT TEMP
The second CNT in device is connected with corresponding a pair of metal electrodes；
(1.4) it is the first of 60~200nm in the junction sputtering thickness of the first CNT and the first Graphene electrodes
SiO2Mask layer, in the junction of the second CNT and metal electrode, the 2nd SiO that sputtering thickness is 60~200nm2Mask
Layer.
Further, CNT temperature sensor does electrode using graphene, and step (1) includes following sub-step：
(1.1) using magnetron sputtering and stripping technology, graphene-carbon nano tube is prepared in substrate of glass after cleaning and is answered
Close the first test electrode, the second test electrode of CNT array of temperature sensor of structure microbubble generator array；The
One test electrode, the second test thickness of electrode are 100~200nm；
(1.2) graphene of CVD growth on Copper Foil is transferred to by substrate of glass using spin coating PMMA wet method shifting process
On, the RIE etchings through photoetching and oxygen prepare the first stone of graphene-carbon nano tube composite structure microbubble generator array
Second Graphene electrodes of black alkene electrode and CNT array of temperature sensor；First Graphene electrodes and the first test electricity
Number of poles is identical, connects one to one；Second Graphene electrodes are identical with the second test number of electrodes, connect one to one；
(1.3) 1MHz, 16V AC signal are loaded on test electrode, then carbon nano tube suspension is dropped in into each stone
Between a pair of first Graphene electrodes of black alkene-composite structure of carbon nano tube microbubble generator, and each CNT temperature
Between a pair of second Graphene electrodes for spending sensor array, each graphene-carbon nano tube composite structure microbubble is occurred
The first CNT in device is connected with corresponding a pair of first Graphene electrodes；By in each CNT temperature sensor
Second CNT is connected with corresponding a pair of second Graphene electrodes；
(1.4) it is the first of 60~200nm in the junction sputtering thickness of the first CNT and the first Graphene electrodes
SiO2Mask layer, in the second CNT and the junction of the second Graphene electrodes, sputtering thickness is the second of 60~200nm
SiO2Mask layer.
Further, carbon nano tube suspension presses 0.001~0.05mg/ml by CNT and effumability organic solvent
Ratio is mixed；
Further, the step of main channel, ink jet chambers are prepared in step (2), enter ink passage, nozzle is as follows：
(2.1) it is using standard cleaning technique that twin polishing Wafer Cleaning is clean as silicon chip substrate, in silicon chip substrate
Surface magnetic control sputtering metal mask layer；
(2.2) the spin coating photoresist on metal mask layer, main channel and nozzle are obtained by exposure, development on a photoresist
Figure, corrodes the metallic film obtained with main channel and nozzle figure with ceric ammonium nitrate solution, and with metallic film and photoetching
Glue is mask, and main channel and nozzle are etched in silicon chip substrate upper surface with ICP lithographic methods；Residual photoetching is removed with acetone
Glue, ammonium ceric nitrate removes kish film；
(2.3) main channel obtained with PDMS filling steps (2.2) and nozzle, utilize step (2.1), the side of (2.2)
Method etches ink jet chambers, and residual photoresist is removed with acetone, and ammonium ceric nitrate removes kish film；
(2.4) ink jet chambers obtained with PDMS filling steps (2.3), then sputtered metal film, spin coating photoresist；
(2.5) etched using step (2.1), the method for (2.2) into ink passage；Removed and led with oxygen plasma lithographic method
The PDMS of filling in passage, nozzle and ink jet chambers；
(2.6) using step (2.1) method is sputtered again, photoetching and wet etching are carried in silicon chip substrate lower surface
The metallic film of inkjet channel figure, and using the metallic film and photoresist as mask, with ICP lithographic methods under silicon chip substrate
Surface etch goes out inkjet channel；
(2.7) acetone removes residual photoresist, and ammonium ceric nitrate removes kish film.
Further, the anode linkage technique in intermediate layer, including following sub-step are used as using graphene fragment in step (3)
Suddenly：
(3.1) graphene fragment is transferred to step (2) with spin coating PMMA wet method shifting process or step (2.7) is obtained
Silicon chip substrate surface white space；
(3.2) substrate of glass for obtaining step (1) is fixed on clean transparent glass plate, is aligned as litho machine
Mask plate；
(3.3) the substrate of glass alignment that the silicon chip substrate and step (3.2) obtained step (3.1) with litho machine is obtained is simultaneously
Laminating, makes the spray corresponding with CNT array of temperature sensor of CNT-graphene composite structure microbubble generator array
The position of ink chamber, and towards ink jet chambers, obtain hot stamping shower nozzle semi-finished product；
(3.4) the hot stamping shower nozzle semi-finished product that step (3.3) is obtained are placed on stamping machine；
(3.5) temperature of stamping machine is raised to 300~350 DEG C, 600~900V direct currents is passed through to hot stamping shower nozzle semi-finished product
Pressure, continues 10min, completes bonding.
Compared with prior art, advantage for present invention and effect are as follows：
(1) carbon nano-tube tiny bubble generator is with graphene substituted metal electrode, and graphene has higher electron transfer
Rate, band gap is zero, and has similar lattice structure to CNT, is the ideal electrode of CNT.Graphene
Directly contacted with CNT by Van der Waals force, form carbon-to-carbon contact, the Xiao Te lower than metal film electrode can be obtained
Base potential barrier, reduces the contact resistance of microbubble generator, so as to reduce the power consumption of microbubble generator.
(2) CNT temperature sensor is introduced, the environment temperature in ink jet chambers is detected, can be microbubble
Generator realizes that feedback control provides foundation.
(3) ink feed channel depth is smaller than the chamber of sprayed printed unit, can be completely closed when bubble valve closes feed liquor.Due to micro-
Fluidic structures are all processed using ICP techniques, while employing a kind of PDMS (dimethyl silicone polymer) filling zanjons
Surface planarisation technique, obtained microfluidic structures are complete.
(4) anode linkage is carried out using graphene fragment as intermediate layer so that machined the silicon chip of microfluidic structures respectively
With the seamless bonding of substrate of glass of microbubble generator and sensor array.
Brief description of the drawings
Fig. 1 is the schematic cross-sectional view of the invention based on the hot jet-printing head of graphene-carbon nano tube composite structure；
Fig. 2 is graphene-carbon nano tube composite structure microbubble generator and CNT temperature in substrate of glass in Fig. 1
Spend the schematic diagram of sensor；
Fig. 3 is the perspective cross-sectional schematic diagram of silicon chip substrate；
Fig. 4 is the top view of silicon chip substrate；
Fig. 5 is the decomposing schematic representation of graphene-carbon nano tube composite structure microbubble generator；
Fig. 6 is Fig. 5 assembling schematic diagram；
Fig. 7 is the decomposing schematic representation of CNT temperature sensor；
Fig. 8 is Fig. 7 assembling schematic diagram；
Fig. 9 is the anode linkage method schematic diagram that intermediate layer is done with graphene fragment；
Figure 10 (a)~10 (d) is the process flow diagram for the anode linkage method that intermediate layer is done with graphene fragment；
Figure 11 (a)~11 (d) is the preparation method flow chart based on the hot jet-printing head of graphene-carbon nano tube composite structure,
Wherein：
Figure 11 (a) graphene-carbon nano tube composite structures microbubble generator and based on metal electrode CNT temperature
Spend the preparation flow figure of sensor；
The preparation stream of microbubble generator and temperature sensor of the Figure 11 (b) based on graphene-carbon nano tube composite structure
Cheng Tu；
The preparation flow figure of Figure 11 (c) microfluidic structures；
Figure 11 (d) does the anode linkage flow chart in intermediate layer with graphene fragment.
In all of the figs, identical reference is used for representing identical element or structure, wherein：
1- substrate of glass, 2- silicon chip substrates, 3- main channels, 4- enters ink passage, 5- ink jet chambers, 6- nozzles, 7- carbon nanometer
Pipe-graphene composite structure microbubble generator array, the Graphene electrodes of 71- first, the CNTs of 72- first, 73- first
SiO2Mask layer, 8- CNT array of temperature sensor, 81- metal electrodes or the second Graphene electrodes, the carbon of 82- second nanometer
Pipe, the SiO of 83- the 2nd2Mask layer, 9- graphene fragments.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in each embodiment of invention described below
Not constituting conflict each other can just be mutually combined.
The hot jet-printing head based on graphene-carbon nano tube composite structure that the present invention is provided includes microfluidic structures, graphite
Alkene-composite structure of carbon nano tube microbubble generator and CNT temperature sensor；Wherein microfluidic structures are to utilize silicon
Processing technology is produced on silicon chip, by main channel 3, ink jet chambers 5, enters ink passage 4, nozzle 6, inkjet channel (non-label) structure
Into.The cross-section structure of hot jet-printing head as shown in figure 1, including：Substrate of glass 1, silicon chip substrate 2, main channel 3, enter ink passage 4, spray
Ink chamber 5, nozzle 6, inkjet channel, CNT-graphene composite structure microbubble generator array 7, CNT temperature
Sensor array 8.Substrate of glass 1 and silicon chip substrate 2 is seamless is bonded together；Microbubble generator 7 and CNT temperature are passed
Sensor array 8 is prepared in substrate of glass 1, positioned at the top of ink jet chambers 5；Main channel 3 is with ink jet chambers 5 by entering ink passage
4 connections.
Main channel 3, enter ink passage 4, ink jet chambers 5 and be the cavity for being opened in the upper surface of silicon chip substrate 2, the He of main channel 3
Ink jet chambers 5 are connected by entering ink passage 4, and enter the depth of ink passage 4 less than the depth of ink jet chambers 5；Inkjet channel is to be arranged on
The cavity of the lower surface of silicon chip substrate 2, inkjet channel is located at the back side of ink jet chambers 5；Nozzle 6 is arranged on the bottom of ink jet chambers 5, connection
Ink jet chambers 5 and inkjet channel；CNT-graphene composite structure microbubble generator array and CNT TEMP
Device array is prepared in the region of the correspondence ink jet chambers 5 of substrate of glass 1, and is set towards ink jet chambers 5.Substrate of glass 1 and silicon chip
The intermediate layer of the seamless bonding of substrate 2 is graphene fragment 9.
Graphene-carbon nano tube composite structure microbubble generator 7 is used as basic heating element heater, graphene using CNT
Replace traditional metal electrodes, one layer of microbubble generator test electrode connection Graphene electrodes are sputtered using the method for magnetron sputtering
And external source, and sputter one layer of SiO2In Graphene electrodes and CNT contact site, fixed and protective effect is played.It is single
The structure of individual graphene-carbon nano tube composite structure microbubble generator 7 as shown in figs.5 and 6, including：It is arranged on glass
A pair of first Graphene electrodes 71 on the surface of substrate 1；Connect the first CNT 72 of a pair of first Graphene electrodes 71；By
The two ends of one CNT 72 are fixed on a pair of the oneth SiO in a pair of first Graphene electrodes 71 and substrate of glass 12Mask layer
73。
Graphene-carbon nano tube composite structure microbubble generator 7 does electrode using graphene, stable in properties, overcomes
The shortcoming that traditional metal electrodes microbubble generator is easily electrolysed or corroded, effectively extends the life-span of microbubble generator.More
Importantly, Graphene electrodes have higher electron mobility, and band gap is zero, and has similar crystalline substance to CNT
Lattice structure, is the ideal electrode of CNT.Graphene is directly contacted by Van der Waals force with CNT, is formed carbon-to-carbon and is connect
Touch, the Schottky barrier lower than metal film electrode can be obtained, the contact resistance of microbubble generator is reduced, so as to drop
The low power consumption of microbubble generator.
CNT temperature sensor 8 it is same with microbubble generator array preparation in substrate of glass 1, its structure with it is micro-
Bubble generator is identical, and simply its electrode both can also use metal material using grapheme material.CNT temperature
The cellular construction of sensor as shown in Figure 7 and Figure 8, including：It is arranged on a pair of metal electrodes 81 on the surface of substrate of glass 1；Even
Connect the second CNT 82 of a pair of metal electrodes 81 or a pair of second Graphene electrodes 81；The two ends of second CNT 82 are consolidated
It is scheduled on a pair of the 2nd SiO in a pair of metal electrodes 81 and substrate of glass 12Mask layer 83.A pair of metal electrodes 81 is in other realities
It can also be a pair of second Graphene electrodes 81 to apply in example.
Radial direction phon scattering caused by the one-dimensional tubular structure of CNT limits CNT radially to ring around
Border and the heat transfer of substrate, vertically based on heat transfer result in high density Joule heat in CNT.Using carbon nanometer
Pipe is as the sensing element in temperature sensor, and highdensity Joule heat makes it be operated in higher temperature, so as to have higher
Sensitivity.The temperature resistance characteristic of CNT temperature sensor discloses the change of the environment temperature in ink jet chambers, obtains
Environment temperature before and after bubble nucleating and ink-jet in ink jet chambers, contributes to the factor such as heat dissipation caused by analysis water, can be more
The microenvironment situation in sprayed printed unit is understood well, and the feedback for controlling circuit for microbubble generator provides foundation.
The preparation method of above-mentioned hot jet-printing head mainly comprises the following steps：
1st step, prepares graphene-carbon nano tube composite structure microbubble generator, CNT temperature on a glass substrate
Spend sensor array；
2nd step, the surface planarisation technique of zanjon is filled using ICP techniques and PDMS (dimethyl silicone polymer),
Microfluidic structures are prepared on silicon chip；Microfluidic structures include main channel, ink jet chambers, enter ink passage, nozzle, inkjet channel；
3rd step, uses the anode linkage technique using graphene fragment as intermediate layer, by glass and wafer bonding.Bonding
Method is as schemed as shown in 9,10, and graphene fragment 9 is located in the middle of substrate of glass 1 and silicon chip substrate 2, in substrate of glass 1 and silicon chip
Apply high pressure, high temperature on substrate 2 to be bonded.
The preparation of microfluidic structures all employs ICP techniques in the hot jet-printing head preparation method that the present invention is provided, simultaneously
The surface planarisation technique that a kind of PDMS (dimethyl silicone polymer) fills zanjon is additionally used, main channel side is effectively improved
The etching effect of edge, it is ensured that the integrality of each structure.In addition, using the anode linkage using graphene fragment as intermediate layer
Technique so that be prepared for the silicon chip substrate and microbubble generator of microfluidic structures and the substrate of glass reality of sensor array respectively
It is now reliable to be bonded.
More specifically, preparing the above-mentioned hot jet-printing head method based on graphene-carbon nano tube composite structure, its step bag
Include：
Step 1：Graphene-carbon nano tube composite structure microbubble generator and carbon nanometer are prepared in substrate of glass 1
Pipe array of temperature sensor；Wherein, CNT temperature sensor can do electrode using graphene or metal material.
As shown in fig. 11a, graphene-carbon nano tube is prepared in substrate of glass 1 according to step (1.1)~(1.4) to be combined
Structure microbubble generator array and CNT array of temperature sensor；When CNT temperature sensor 8 uses metal
During electrode, specific sub-step is as follows：
(1.1) magnetron sputtering and stripping technology are used, graphene-carbon nano tube composite structure is prepared in substrate of glass 1
First test electrode (not shown) of microbubble generator array and the second test electricity of CNT array of temperature sensor
Pole (not shown) and metal electrode, the first test electrode, the second test electrode, the thickness of metal electrode are 100~200nm；Gold
The spacing for belonging to electrode is 1~6 μm, and width is 1~5 μm；Metal electrode and the second test number of electrodes are identical, the company of one-to-one corresponding
Connect；
(1.2) graphene of CVD growth on Copper Foil is transferred to by substrate of glass 1 using spin coating PMMA wet method shifting process
On, the RIE etchings through photoetching and oxygen prepare the first stone of CNT-graphene composite structure microbubble generator array
Black alkene electrode；The spacing of first Graphene electrodes is 1~6 μm, and width is 1~5 μm, the first Graphene electrodes and the first test electricity
Number of poles is identical, connects one to one；
(1.3) AC signal of loading 1MHz, 16V on electrode are tested in microbubble generator, then CNT is suspended
Drop is between a pair of first Graphene electrodes of each graphene-carbon nano tube composite structure microbubble generator, and often
Between a pair of metal electrodes of individual CNT array of temperature sensor, carbon nano tube suspension is by CNT and effumability
Organic solvent (such as absolute ethyl alcohol) is mixed in 0.001~0.05mg/ml ratios；By alternating voltage at paired two
Non-uniform electric field is produced between first Graphene electrodes, promotes the first CNT to shifting in the middle of corresponding a pair of first graphenes
It is dynamic, after effumability organic solvent volatilizees, the first carbon in each graphene-carbon nano tube composite structure microbubble generator
Nanotube is connected with corresponding a pair of first Graphene electrodes；Similarly, by the second carbon in each CNT temperature sensor
Nanotube is connected with corresponding a pair of metal electrodes；The purpose for preparing carbon nano tube suspension is CNT is in suspension
State, so as to move freely；
(1.4) it is the first of 60~200nm in the junction sputtering thickness of the first CNT and the first Graphene electrodes
SiO2Mask layer, in the junction of the second CNT and metal electrode, the 2nd SiO that sputtering thickness is 60~200nm2Mask
Layer.
As shown in figure 11b, in another embodiment, CNT temperature sensor can also do electrode with graphene, this
When, step 1 includes following sub-step：
(1.1) using magnetron sputtering and stripping technology, graphene-carbon nano tube is prepared in substrate of glass after cleaning and is answered
Close structure microbubble generator array first tests the second of electrode (not shown) and CNT array of temperature sensor
Electrode (not shown) is tested, the first test electrode, the second test thickness of electrode are 100~200nm；
(1.2) graphene of CVD growth on Copper Foil is transferred to by substrate of glass using spin coating PMMA wet method shifting process
On, the RIE etchings through photoetching and oxygen prepare the first stone of graphene-carbon nano tube composite structure microbubble generator array
Second Graphene electrodes of black alkene electrode and CNT array of temperature sensor；First Graphene electrodes and the first test electricity
Number of poles is identical, connects one to one；Second Graphene electrodes are identical with the second test number of electrodes, connect one to one；
(1.3) 1MHz, 16V AC signal are loaded on test electrode, then carbon nano tube suspension is dropped in into each stone
Between a pair of first Graphene electrodes of black alkene-composite structure of carbon nano tube microbubble generator, and each CNT temperature
Between a pair of second Graphene electrodes for spending sensor array, carbon nano tube suspension is organic molten by CNT and effumability
Agent (such as absolute ethyl alcohol) is mixed in 0.001~0.05mg/ml ratios；By alternating voltage in two paired the first stones
Non-uniform electric field is produced between black alkene electrode, promotes the first CNT to movement in the middle of corresponding a pair of first graphenes, treats
After the volatilization of effumability organic solvent, the first carbon in each graphene-carbon nano tube composite structure microbubble generator is received
Mitron is connected with corresponding a pair of first Graphene electrodes；Similarly, the second carbon in each CNT temperature sensor is received
Mitron is connected with corresponding a pair of second Graphene electrodes；
(1.4) it is the first of 60~200nm in the junction sputtering thickness of the first CNT and the first Graphene electrodes
SiO2Mask layer, in the second CNT and the junction of the second Graphene electrodes, sputtering thickness is the second of 60~200nm
SiO2Mask layer.
Step 2：Microfluidic structures are prepared in silicon chip substrate 2.
Microfluidic structures enter ink passage 4 by main channel 3, and ink jet chambers 5, nozzle 6 is constituted, all using ICP technique systems
It is standby；Meanwhile, the surface planarisation technique that a kind of PDMS (dimethyl silicone polymer) fills zanjon is additionally used, is effectively improved
The etching effect at main channel edge, it is ensured that the integrality of the geometric figure of each structure.
As shown in fig. 11c, the concrete technology step for preparing microfluidic structures is as follows：
(2.1) it is using standard cleaning technique that twin polishing Wafer Cleaning is clean as silicon chip substrate, in silicon chip substrate
Surface magnetic control sputtering metal mask layer；
(2.2) the spin coating photoresist on metal mask layer, main channel and nozzle are obtained by exposure, development on a photoresist
Figure, corrodes the metallic film obtained with main channel and nozzle figure with ceric ammonium nitrate solution, and with metallic film and photoetching
Glue is mask, and main channel and nozzle are etched in silicon chip substrate upper surface with ICP lithographic methods；Residual photoetching is removed with acetone
Glue, ammonium ceric nitrate removes kish film；
(2.3) main channel obtained with PDMS filling steps (2.2) and nozzle, utilize step (2.1), the side of (2.2)
Method etches ink jet chambers, and residual photoresist is removed with acetone, and ammonium ceric nitrate removes kish film；
(2.4) ink jet chambers obtained with PDMS filling steps (2.3), then sputtered metal film, spin coating photoresist；
(2.5) etched using step (2.1), the method for (2.2) into ink passage；Removed and led with oxygen plasma lithographic method
The PDMS of filling in passage, nozzle and ink jet chambers；
(2.6) using step (2.1) method is sputtered again, photoetching and wet etching are carried in silicon chip substrate lower surface
The metallic film of inkjet channel figure, and using the metallic film and photoresist as mask, with ICP lithographic methods under silicon chip substrate
Surface etch goes out inkjet channel；
(2.7) acetone removes residual photoresist, and ammonium ceric nitrate removes kish film.
Step 3：Substrate of glass is bonded with silicon chip.The anode linkage method using graphene fragment as intermediate layer is used,
So that the seamless bonding of the substrate of glass of silicon chip and microbubble generator and sensor array for being prepared for microfluidic structures respectively.
As illustrated in fig. 11d, the anode linkage technique using graphene fragment as intermediate layer, including following sub-steps are used：
(3.1) graphene is transferred to the silicon chip substrate for being prepared for microfluidic structures with spin coating PMMA wet method shifting process
Surface white space；
(3.2) graphene-carbon nano tube composite structure bubble generator, CNT array of temperature sensor will be prepared for
Substrate of glass be fixed on clean transparent glass plate, the mask plate being aligned as litho machine；
(3.3) the substrate of glass alignment that the silicon chip substrate and step (3.2) obtained step (3.1) with litho machine is obtained is simultaneously
Laminating, makes the spray corresponding with CNT array of temperature sensor of CNT-graphene composite structure microbubble generator array
The position of ink chamber, and towards ink jet chambers, obtain hot stamping shower nozzle semi-finished product；Script litho machine is used in photoetching, this step
It is aligned using litho machine；
(3.4) heat that the silicon chip substrate 2 of 1/ graphene fragment of substrate of glass 9/ after the alignment for obtaining step (3.3) is constituted
Print shower nozzle semi-finished product are placed on stamping machine；
(3.5) temperature of stamping machine is raised to 300~350 DEG C, is passed through 600~900V DC voltages, continue 10min, it is complete
Into bonding.
To make those skilled in the art more fully understand the present invention, with reference to microbubble of the specific embodiment to the present invention
The preparation method of generator is described in detail.
【Embodiment 1】
(1) quartz glass is cleaned, by graphene-carbon nano tube composite structure as substrate using quartz glass
Microbubble generator, CNT array of temperature sensor are prepared on quartz glass, and its process is：
(1.1) magnetron sputtering is used, the nickel film that thickness is 100nm is formed, existing stripping technology formation nickel electrode is utilized；
The nickel electrode spacing of temperature sensor is 2 μm, and width is 4 μm；
(1.2) graphene of CVD growth on Copper Foil is transferred to by substrate of glass using spin coating PMMA wet method shifting process,
RIE etchings through photoetching and oxygen prepare the Graphene electrodes of microbubble generator；The spacing of Graphene electrodes is 2 μm, wide
Spend for 4 μm；
(1.3) CNT and anhydrous ethanol solvent are mixed in 0.001mg/ml ratios, makes CNT equal through ultrasound
It is even scattered；By 1MHz, 16V alternating voltage is loaded into the nickel electrode on glass, with microsyringe by carbon nano tube suspension
Drip between electrode, when solvent is evaporated completely full-time, electrode is connected and be positioned between electrode by CNT, is now removed and is powered up
；
(1.4) magnetron sputtering is used, the silicon dioxide film that thickness is 60nm is formed；
(2) technique in following processes and table 1 makes microfluidic structures in silicon chip substrate：
(2.1) silicon chip substrate, front magnetron sputtering are totally regard twin polishing Wafer Cleaning as using standard cleaning technique
One layer of Cr film；
(2.2) by main channel and nozzle pattern transfer to photoresist after positive spin coating photoresist, exposure imaging, nitric acid is used
Cerium ammonium salt solution corrodes the Cr films for obtaining main channel and nozzle figure, and using Cr and photoresist as mask, is etched with ICP lithographic methods
Main channel and nozzle, acetone remove residual photoresist, and ammonium ceric nitrate removes residual Cr films；
(2.3) main channel formed after etching and nozzle, then one layer of Cr film of front sputtering, spin coating photoetching are filled with PDMS
Glue, photoetching and wet etching obtain the Cr films of ink jet chambers figure again, and using Cr films and photoresist as mask, are etched with ICP
Method etches ink jet chambers, and residual photoresist is removed with acetone, and ammonium ceric nitrate removes residual Cr films；；
(2.4) ink jet chambers formed after etching, then one layer of Cr film of front sputtering, spin coating photoresist are filled with PDMS；
(2.5) photoetching, wet etching obtain the Cr films of ink feed passageway pattern again, using Cr films and photoresist as mask, use
ICP lithographic methods are etched into ink passage, and residual photoresist is removed with acetone, and ammonium ceric nitrate removes residual Cr films, uses oxygen plasma
Lithographic method removes the PDMS of filling in main channel, nozzle and ink jet chambers；
(2.6) in silicon chip reverse side one layer of Cr film of sputtering, one layer of photoresist of spin coating, photoetching, wet etching obtain reverse side again
The Cr films of structure graph, and using Cr films and photoresist as mask, inverse layer structure is etched with ICP lithographic methods；
(2.7) residual photoresist is removed with acetone, ammonium ceric nitrate removes kish film, completes the system of microfluidic structures
It is standby.
The technological parameter of table 1ICP etchings
(3) silicon chip and microbubble generator and the substrate of glass anode key of sensor array of microfluidic structures will be prepared for
Close, its process is：
(3.1) graphene is transferred to the silicon chip surface for being prepared for microfluidic structures with spin coating PMMA wet method shifting process
White space；
(3.2) glass of graphene-carbon nano tube composite structure bubble generator, CNT temperature sensor will be prepared for
Glass substrate is fixed on clean transparent glass plate, the mask plate being aligned as litho machine；
(3.3) substrate of glass is aligned with the silicon chip with microfluidic structures with litho machine；
(3.4) substrate of glass after alignment/graphene/silicon piece is placed on stamping machine；
(3.5) temperature is raised to 350 DEG C, is passed through 900V DC voltages, continue 10min.
【Embodiment 2】
(1) glass is cleaned, will be answered based on graphene-carbon nano tube as substrate using Pyrex7740 types glass
The microbubble generator and temperature sensor for closing structure are prepared on quartz glass, and its process is：
(1.1) magnetron sputtering is used, the titanium film that thickness is 200nm is formed, the formation titanium test of existing stripping technology is utilized
Electrode；
(1.2) passed through using the graphene of CVD growth on spin coating PMMA wet method shifting process transfer Copper Foil to substrate of glass
The RIE etchings of photoetching and oxygen prepare the Graphene electrodes of microbubble generator and temperature sensor；The spacing of graphene
For 6 μm, width is 5 μm；
(1.3) CNT and anhydrous ethanol solvent are mixed in 0.05mg/ml ratios, makes CNT uniform through ultrasound
It is scattered；By 1MHz, 16V alternating voltage is loaded between the Ti electrode on glass, with microsyringe by carbon nano tube suspension
Drip between electrode, when solvent is evaporated completely full-time, electrode is connected and be positioned between electrode by CNT, is now removed and is powered up
；
(1.4) magnetron sputtering is used, the silicon dioxide film that thickness is 200nm is formed；
(2) microfluidic structures are prepared using method in the same manner as in Example 1；
(3) silicon chip and the seamless key of the substrate of glass of microbubble generator and sensor array of microfluidic structures will be prepared for
Close, its process is：
(3.1) graphene is transferred to the silicon chip surface for being prepared for microfluidic structures with spin coating PMMA wet method shifting process
White space；
(3.2) glass of graphene-carbon nano tube composite structure bubble generator, CNT temperature sensor will be prepared for
Glass substrate is fixed on clean transparent glass plate, the mask plate being aligned as litho machine；
(3.3) substrate of glass is aligned with the silicon chip with microfluidic structures with litho machine；
(3.4) substrate of glass after alignment/graphene/silicon piece is placed on stamping machine；
(3.5) temperature is raised to 300 DEG C, is passed through 600V DC voltages, continue 10min.
As it will be easily appreciated by one skilled in the art that the foregoing is only presently preferred embodiments of the present invention, it is not used to
The limitation present invention, any modification, equivalent and the improvement made within the spirit and principles of the invention etc., it all should include
Within protection scope of the present invention.
Claims (10)
1. a kind of hot jet-printing head based on graphene-carbon nano tube composite structure, it is characterised in that including：Substrate of glass, silicon chip
Substrate, main channel, enter ink passage, ink jet chambers, nozzle, inkjet channel, CNT-graphene composite structure microbubble and occur
Device array, CNT array of temperature sensor；
Main channel, enter ink passage, ink jet chambers and be the cavity for being opened in silicon chip substrate upper surface, main channel and ink jet chambers are logical
Cross into ink passage connection, and ink feed channel depth is less than ink jet chambers depth；Inkjet channel is to be arranged on silicon chip substrate lower surface
Cavity, inkjet channel be located at the ink jet chambers back side；Nozzle is arranged on ink jet chambers bottom, and connection ink jet chambers and ink-jet are logical
Road；
CNT-graphene composite structure microbubble generator array and CNT array of temperature sensor are prepared in glass
The region of substrate correspondence ink jet chambers, and set towards ink jet chambers；
Substrate of glass and silicon chip substrate is seamless is bonded together.
2. a kind of hot jet-printing head based on graphene-carbon nano tube composite structure as claimed in claim 1, it is characterised in that
Single graphene-carbon nano tube composite structure microbubble generator includes：It is arranged on a pair of first graphite of glass basic surface
Alkene electrode；Connect the first CNT of a pair of first Graphene electrodes；First CNT two ends are fixed on a pair first
A pair of the oneth SiO in Graphene electrodes and substrate of glass2Mask layer.
3. a kind of hot jet-printing head based on graphene-carbon nano tube composite structure as claimed in claim 1, it is characterised in that
Single Carbon Nanotubes temperature sensor includes：It is arranged on a pair of metal electrodes or a pair of second graphene electricity of glass basic surface
Pole；Connect the second CNT of a pair of metal electrodes or a pair of second Graphene electrodes；Second CNT two ends are fixed
In a pair of metal electrodes and substrate of glass, or a pair of the 2nd SiO in a pair of second Graphene electrodes and substrate of glass2Mask
Layer.
4. a kind of hot jet-printing head based on graphene-carbon nano tube composite structure as described in claim 1-3 any one, its
It is characterised by, the intermediate layer of substrate of glass and the seamless bonding of silicon chip substrate is graphene fragment.
5. the preparation method of the hot stamping shower nozzle described in a kind of claim 1, it is characterised in that comprise the following steps：
(1) graphene-carbon nano tube composite structure microbubble generator array, CNT temperature is prepared on the glass substrate to pass
Sensor array；
(2) the surface planarisation technique of zanjon is filled using ICP techniques and PDMS, main channel, spray are prepared in silicon chip substrate
Ink chamber, enter ink passage, nozzle, inkjet channel；
(3) anode linkage technique is used, using graphene fragment as intermediate layer, the substrate of glass and step that step (1) is obtained
(2) the silicon chip substrate bonding obtained.
6. preparation method as claimed in claim 5, it is characterised in that CNT temperature sensor uses metal electrode, step
Suddenly (1) includes following sub-step：
(1.1) magnetron sputtering and stripping technology are used, graphene-carbon nano tube composite structure microbubble is prepared on the glass substrate
First test electrode of generator array, the second test electrode of CNT array of temperature sensor, and CNT temperature
Spend the metal electrode of sensor array；First test electrode, the second test electrode, the thickness of metal electrode are 100~200nm；
The spacing of metal electrode is 1~6 μm, and width is 1~5 μm；Metal electrode is identical with the second test number of electrodes, the company of one-to-one corresponding
Connect；
(1.2) graphene of CVD growth on Copper Foil is transferred in substrate of glass using spin coating PMMA wet method shifting process, passed through
The RIE etchings of photoetching and oxygen prepare the first graphene of CNT-graphene composite structure microbubble generator array
Electrode；The spacing of first Graphene electrodes is 1~6 μm, and width is 1~5 μm, the first Graphene electrodes and the first test number of electrodes
Amount is identical, connects one to one；
(1.3) AC signal of loading 1MHz, 16V on electrode are tested in microbubble generator, then carbon nano tube suspension is dripped
Between a pair of first Graphene electrodes of each graphene-carbon nano tube composite structure microbubble generator, and each carbon
Between a pair of metal electrodes of nanotube array of temperature sensor, each graphene-carbon nano tube composite structure microbubble is sent out
The first CNT in raw device is connected with corresponding a pair of first Graphene electrodes；By in each CNT temperature sensor
The second CNT connected with corresponding a pair of metal electrodes；
(1.4) the first SiO for being 60~200nm in the junction sputtering thickness of the first CNT and the first Graphene electrodes2Cover
Film layer, in the junction of the second CNT and metal electrode, the 2nd SiO that sputtering thickness is 60~200nm2Mask layer.
7. preparation method as claimed in claim 5, it is characterised in that CNT temperature sensor does electricity using graphene
Pole, step (1) includes following sub-step：
(1.1) use in magnetron sputtering and stripping technology, substrate of glass after cleaning and prepare graphene-carbon nano tube composite junction
First test electrode of structure microbubble generator array, the second test electrode of CNT array of temperature sensor；First surveys
It is 100~200nm to try electrode, the second test thickness of electrode；
(1.2) graphene of CVD growth on Copper Foil is transferred in substrate of glass using spin coating PMMA wet method shifting process, passed through
The RIE etchings of photoetching and oxygen prepare the first graphene of graphene-carbon nano tube composite structure microbubble generator array
Second Graphene electrodes of electrode and CNT array of temperature sensor；First Graphene electrodes and the first test number of electrodes
Amount is identical, connects one to one；Second Graphene electrodes are identical with the second test number of electrodes, connect one to one；
(1.3) load 1MHz on test electrode, 16V AC signal, then by carbon nano tube suspension drop in each graphene-
Between a pair of first Graphene electrodes of composite structure of carbon nano tube microbubble generator, and each CNT TEMP
Between a pair of second Graphene electrodes of device array, by each graphene-carbon nano tube composite structure microbubble generator
First CNT is connected with corresponding a pair of first Graphene electrodes；By the second carbon in each CNT temperature sensor
Nanotube is connected with corresponding a pair of second Graphene electrodes；
(1.4) the first SiO for being 60~200nm in the junction sputtering thickness of the first CNT and the first Graphene electrodes2Cover
Film layer, in the second CNT and the junction of the second Graphene electrodes, the 2nd SiO that sputtering thickness is 60~200nm2Mask
Layer.
8. preparation method as claimed in claims 6 or 7, it is characterised in that carbon nano tube suspension is by CNT with easily waving
Hair property organic solvent is mixed in 0.001~0.05mg/ml ratios.
9. the preparation method as described in claim 5 or 7, it is characterised in that main channel, ink jet chambers are prepared in step (2), are entered
The step of ink passage, nozzle, is as follows：
(2.1) it is using standard cleaning technique that twin polishing Wafer Cleaning is clean as silicon chip substrate, in silicon chip substrate upper surface
Magnetron sputtering metal mask layer；
(2.2) the spin coating photoresist on metal mask layer, main channel and nozzle figure are obtained by exposure, development on a photoresist
Shape, corrodes the metallic film obtained with main channel and nozzle figure with ceric ammonium nitrate solution, and with metallic film and photoresist
For mask, main channel and nozzle are etched in silicon chip substrate upper surface with ICP lithographic methods；Residual photoresist is removed with acetone,
Ammonium ceric nitrate removes kish film；
(2.3) main channel obtained with PDMS filling steps (2.2) and nozzle, are carved using step (2.1), the method for (2.2)
Lose ink jet chambers, residual photoresist is removed with acetone, ammonium ceric nitrate removes kish film；
(2.4) ink jet chambers obtained with PDMS filling steps (2.3), then sputtered metal film, spin coating photoresist；
(2.5) etched using step (2.1), the method for (2.2) into ink passage；Removed with oxygen plasma lithographic method main logical
The PDMS of filling in road, nozzle and ink jet chambers；
(2.6) sputtered again using step (2.1) method, photoetching and wet etching obtain carrying ink-jet in silicon chip substrate lower surface
The metallic film of passageway pattern, and using the metallic film and photoresist as mask, with ICP lithographic methods in silicon chip substrate lower surface
Etch inkjet channel；
(2.7) acetone removes residual photoresist, and ammonium ceric nitrate removes kish film.
10. the preparation method as described in claim 5 or 9, it is characterised in that step is used as centre in (3) using graphene fragment
The anode linkage technique of layer, including following sub-step：
(3.1) graphene fragment is transferred to the silicon that step (2) or step (2.7) are obtained with spin coating PMMA wet method shifting process
The white space of piece substrate surface；
(3.2) substrate of glass for obtaining step (1) is fixed on clean transparent glass plate, the mask being aligned as litho machine
Version；
(3.3) substrate of glass that the silicon chip substrate and step (3.2) obtained step (3.1) with litho machine is obtained is aligned and pasted
Close, make the ink-jet corresponding with CNT array of temperature sensor of CNT-graphene composite structure microbubble generator array
The position of chamber, and towards ink jet chambers, obtain hot stamping shower nozzle semi-finished product；
(3.4) the hot stamping shower nozzle semi-finished product that step (3.3) is obtained are placed on stamping machine；
(3.5) temperature of stamping machine is raised to 300~350 DEG C, 600~900V DC voltages is passed through to hot stamping shower nozzle semi-finished product,
Continue 10min, complete bonding.
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