CN107969066A - The method for preparing stretchable circuit using oil-water interfaces reaction inkjet printing - Google Patents
The method for preparing stretchable circuit using oil-water interfaces reaction inkjet printing Download PDFInfo
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- CN107969066A CN107969066A CN201711276197.1A CN201711276197A CN107969066A CN 107969066 A CN107969066 A CN 107969066A CN 201711276197 A CN201711276197 A CN 201711276197A CN 107969066 A CN107969066 A CN 107969066A
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- oil
- water
- water interfaces
- inkjet printing
- stretchable circuit
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/12—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using thick film techniques, e.g. printing techniques to apply the conductive material or similar techniques for applying conductive paste or ink patterns
- H05K3/1241—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using thick film techniques, e.g. printing techniques to apply the conductive material or similar techniques for applying conductive paste or ink patterns by ink-jet printing or drawing by dispensing
- H05K3/125—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using thick film techniques, e.g. printing techniques to apply the conductive material or similar techniques for applying conductive paste or ink patterns by ink-jet printing or drawing by dispensing by ink-jet printing
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/0277—Bendability or stretchability details
- H05K1/0283—Stretchable printed circuits
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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Manufacturing Of Printed Wiring (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The present invention provides a kind of method for preparing stretchable circuit using oil-water interfaces reaction inkjet printing, it comprises the following steps:S1, utilize the patterned oil-water interfaces system of inkjet printing structure;Prepared by S2, oil-water interfaces oil-in-water emulsified layer, surfactant is added in the conductive presoma water-base ink in S1, and applies shearing force to oil-water interfaces, obtains stable oil-in-water emulsified layer;The composite construction of S3, oil-water interfaces reaction generation metal parcel elastomeric polymer;S4, the composite construction of the metal obtained using S3 parcel elastomeric polymer form stretchable circuit, and carry out electric conductivity test to the electric property of stretchable circuit, obtain the stretchable circuit of best performance.The present invention, which reacts oil-water interfaces, to be combined with inkjet printing technology, can rapid large-area realize the fine preparation of stretchable circuit, manufacture and be of great significance for flexible extensible electronic device.
Description
Technical field
The present invention relates to application of the printing manufacturing technology in flexible electronic field, and oil-water interfaces are utilized more particularly to one kind
The method that reaction inkjet printing prepares stretchable circuit.
Background technology
In recent years, research of the inkjet printing technology in terms of pattern of functional material has received widespread attention.With it is traditional
Pattern of functional material technology is compared, and inkjet printing technology is that ink is deposited directly to specific region, it is not necessary to mask and exposure
Photoengraving, has saved cost and has greatly reduced pollution.Meanwhile inkjet printing technology be also equipped with flexibly, rapidly, continuously large area
Prepare, environmental suitability is strong, adapts to the advantages such as different substrate materials.
With inkjet printing technology deepening continuously in terms of patterns of high precision preparation research, it is in green plate-making, monocrystalline
Film, transistor, histoorgan, solar cell, biochip, RFID antenna and sensor etc. achieve it is important into
Exhibition.It is that conductive material (metal nanoparticle, carbon material, conductive presoma etc.) is scattered or molten that inkjet printing, which prepares electronic circuit,
Solution is made conductive ink in a solvent, and the profit printer spray orifice that computerizeds control sprays conductive ink droplet, realizes and schemes in substrate surface
Caseization deposits, and obtains required conductive pattern.But the conductive material of inkjet printing and base material are incorporated in certain bending
Easily destroyed under curvature, conductive material is easily produced slight crack or peeling from base material.Meanwhile conductive material is higher
Hardness and brittleness tend not to meet application requirement of the electronic circuit at stretchable aspect.
At present, the energy of man-machine interface, information fusion play increasingly with interacting in terms of human life quality is improved
Important effect, flexible extensible electronic device is in fields such as wearable, Flexible Displays, life medical treatment, Internet of Things, intelligent apparatuses
Application demand constantly increases.Therefore, inkjet printing prepares when one kind bends, folds and stretches under external force and remains to protect
The stretchable circuit for holding stable electrical properties has important research meaning and application value.
Composite conducting slurry needs to add substantial amounts of viscoelastic material to reach good electric conductivity with tensility, this
Obviously it cannot meet the rheological property requirement of ink-jet printing ink, be difficult to realize the fine system of stretchable circuit in practical applications
It is standby.Therefore, develop that a kind of by inkjet printing conductive ink to be directly realized by conductive material and elastomeric polymer in circuit compound
Method, realizes that the fine of stretchable circuit is prepared with important research meaning and using valency for flexible, quick, large area
Value.
The content of the invention
The defects of in order to overcome the prior art, the present invention provide one kind and are prepared and can be drawn using oil-water interfaces reaction inkjet printing
The method of circuit is stretched, it utilizes the liquid elastomer prepolymer oiliness substrate of reproducibility, and conductive presoma water-base ink, builds grease
Inkjet printing system is reacted, interfacial reaction is carried out in the oil-water interfaces emulsion layer of formation, realizes that metal wraps up elastomeric polymer
Composite construction, inkjet printing prepares stretchable circuit.
What the present invention was realized in:The present invention provides one kind and prepares stretchable electricity using oil-water interfaces reaction inkjet printing
The method on road, it comprises the following steps:
S1, using inkjet printing build patterned oil-water interfaces system, prepares reproducibility liquid prepolymer oiliness substrate,
In reproducibility liquid prepolymer oiliness substrate surface inkjet printing conduction presoma water-base ink, patterned oil-water interfaces are built
System;
Prepared by S2, oil-water interfaces oil-in-water emulsified layer, surface-active is added in the conductive presoma water-base ink in S1
Agent, and shearing force is applied to oil-water interfaces, obtain stable oil-in-water emulsified layer;
S3, oil-water interfaces reaction generation metal composite structure, the oil-in-water emulsified layer of the stabilization obtained to S2 apply temperature
Control, the reduction reaction generation that metal ion occurs in water-oil interface for conductive presoma water-base ink and surfactant are continuous
Metal layer, after curing to reproducibility liquid prepolymer oiliness substrate, obtain metal parcel elastomeric polymer composite junction
Structure;
S4, the composite construction of the metal obtained using S3 parcel elastomeric polymer form stretchable circuit, and to stretchable
The electric property of circuit carries out electric conductivity test, and carries out multi-drawing to circuit, and the electric conductivity in drawing process is carried out
Test, and then by varying the control parameter in preparation process, obtain the stretchable circuit of best performance.
Preferably, shearing force is applied to oil-water interfaces using micro- ultrasound in S2.
Preferably, be changed in S3 between 30 DEG C to 90 DEG C temperature regulation and control, obtain with different electric properties can
Stretch circuit.
Preferably, interfacial reaction temperature, reactant concentration and kinds of surfactants regulation and control metal composite are utilized in S4
The composition and thickness of structure, obtain the relation of the metal composite structure and its electric property of oil-water interfaces reaction generation, selection is most
The stretchable circuit of excellent gain of parameter best performance.
Preferably, in S4 at 70 DEG C, the electric property of the metal composite structure is stablized the most, and prepared structure is the most
Homogeneous, conductivity is consistent under stretching condition, is reduced or is reduced temperature, the metal composite conductive structure of formation, with drawing
The change for having electric property is stretched, and temperature departure is bigger, electric property is bigger with the change of level of stretch.
Preferably, the preparation of reproducibility liquid prepolymer oiliness substrate comprises the following steps in S1:
Elastomeric prepolymer is chosen, then makes mass fraction of the reducing agent in liquid prepolymer oiliness substrate be by a certain percentage
8%-12%, is subject to the viscoelastic fluid flow behavior for not influencing substrate;
The reducing agent of the functional group containing reproducibility is added thereto, obtains mixture, prepared by spin coating or extrusion said mixture
Reproducibility liquid elastomer prepolymer oiliness substrate.
Preferably, the substrate of initiator preparation is uniformly added in S1 for the dimethyl silicone polymer by thermohardening type, is needed
Want under normal pressure, precuring 7-8 minutes is carried out in 70 DEG C of baking oven, obtain certain viscoelastic mobility substrate.
Preferably, structure patterning oil-water interfaces system comprises the following steps in S1:
The surface tension matching of ink-jet ink and printed substrates is adjusted, prepared conductive precursor ink injection is beaten
Print machine print cartridge, using fine nozzle, in the pattern of mobility oil phase reduction substrate surface inkjet printing setting, finishing patterns
Oil-water interfaces structure.
Preferably, elastomeric prepolymer is uniformly to add initiator by the dimethyl silicone polymer of thermohardening type to prepare.
Preferably, the reducing agent in S1 is the compound containing aldehyde radical.
Compared with prior art, the invention has the advantages that:
The present invention is the liquid elastomer prepolymer oiliness substrate using reproducibility, and conductive presoma water-base ink, builds oil
Water reacts inkjet printing system, and interfacial reaction is carried out in the oil-water interfaces emulsion layer of formation, realizes that metal wraps up flexible polymer
The composite construction of thing, inkjet printing prepare stretchable circuit.The present invention reacts oil-water interfaces to be combined with inkjet printing technology,
Can rapid large-area realize the fine preparation of stretchable circuit, be of great significance for the manufacture of flexible extensible electronic device.
At the same time, it is proposed that a kind of composite construction prepares the method with regulation and control, has greatly improved the efficiency for preparing Stretch material, has been one
The new method of kind high performance material manufacture.
Brief description of the drawings
Fig. 1 is the flow chart that the present invention prepares stretchable circuit methods;
Fig. 2 is that inkjet printing builds oil-water interfaces reaction system schematic diagram in the embodiment of the present invention;
Fig. 3 is that metal composite structure lifts the stretchable impact of performance figure of circuit in the embodiment of the present invention.
Embodiment
Below with reference to the attached drawing exemplary embodiment that the present invention will be described in detail, feature and aspect.It is identical attached in attached drawing
Icon note represents functionally the same or similar element.Although the various aspects of embodiment are shown in the drawings, unless special
Do not point out, it is not necessary to attached drawing drawn to scale.
The present invention provides a kind of method for preparing stretchable circuit using oil-water interfaces reaction inkjet printing, it includes following
Step:
S1, using inkjet printing build patterned oil-water interfaces system, prepares reproducibility liquid prepolymer oiliness substrate,
In reproducibility liquid prepolymer oiliness substrate surface inkjet printing conduction presoma water-base ink, patterned oil-water interfaces are built
System.
The preparation of reproducibility liquid prepolymer oiliness substrate comprises the following steps in S1:
Elastomeric prepolymer is chosen, then makes mass fraction of the reducing agent in liquid prepolymer oiliness substrate be by a certain percentage
8%-12%, is subject to the viscoelastic fluid flow behavior for not influencing substrate;The reducing agent of the functional group containing reproducibility is added thereto, is obtained
To mixture, spin coating or extrusion said mixture prepare reproducibility liquid elastomer prepolymer oiliness substrate.
Preferably, the substrate of initiator preparation is uniformly added in S1 for the dimethyl silicone polymer by thermohardening type, is needed
Want under normal pressure, precuring 7-8 minutes is carried out in 70 DEG C of baking oven, obtain certain viscoelastic mobility substrate.
Prepared by S2, oil-water interfaces oil-in-water emulsified layer, surface-active is added in the conductive presoma water-base ink in S1
Oil-water interfaces using micro- ultrasound and are applied shearing force, obtain stable oil-in-water emulsified layer by agent.
S3, oil-water interfaces reaction generation metal composite structure, the oil-in-water emulsified layer of the stabilization obtained to S2 apply temperature
Control, the reduction reaction generation that metal ion occurs in water-oil interface for conductive presoma water-base ink and surfactant are continuous
Metal layer, after curing to reproducibility liquid prepolymer oiliness substrate, obtain metal parcel elastomeric polymer composite junction
Structure;Temperature regulation and control are changed in S3 between 30 DEG C to 90 DEG C, obtain the stretchable circuit with different electric properties.
S4, the composite construction of the metal obtained using S3 parcel elastomeric polymer form stretchable circuit, and to stretchable
The electric property of circuit carries out electric conductivity test, and carries out multi-drawing to circuit, and the electric conductivity in drawing process is carried out
Test, and then by varying the control parameter in preparation process, obtain the stretchable circuit of best performance.
The group of interfacial reaction temperature, reactant concentration and kinds of surfactants regulation and control metal composite structure is utilized in S4
Into and thickness, obtain the relation of metal composite structure and its electric property of oil-water interfaces reaction generation, select optimized parameter to obtain
Obtain the stretchable circuit of best performance.
In S4 at 70 DEG C, the electric property of the metal composite structure is stablized the most, and prepared structure is the most homogeneous, draws
Conductivity is consistent under the conditions of stretching, and is reduced or is reduced temperature, the metal composite conductive structure of formation, as stretching has electricity
The change of performance is learned, and temperature departure is bigger, electric property is bigger with the change of level of stretch.
With reference to the Content Implementation of attached drawing Fig. 1, the embodiment during the present invention will be described in detail.
The specific implementation method of the preparation of conductive presoma water-base ink is to be directed to different conductive metal materials, such as gold,
Silver, copper, select different conductive presomas is soluble in water to form conductive presoma water-base ink.Selected according to " coalescence rate theory "
The stronger surfactant of hydrophily is selected to be added in conductive presoma water-base ink as emulsifying agent.
The specific implementation method of the preparation of reproducibility liquid elastomer prepolymer oiliness substrate is to choose different types of elasticity
Prepolymer, such as the dimethyl silicone polymer of thermohardening type, uniformly adds initiator, then add thereto containing reduction by a certain percentage
The reducing agent of property functional group, such as compound containing aldehyde radical.Spin coating or extrusion said mixture prepare reproducibility liquid elastomer pre-polymerization
Thing oiliness substrate, the precuring regular hour, obtains different viscoelastic mobility substrates.
It is specifically real with reference to attached drawing Fig. 2 the present invention also provides the method that inkjet printing builds patterned oil-water interfaces system
It is to adjust the surface tension matching of ink-jet ink and printed substrates to apply content, and prepared conductive precursor ink injection is beaten
Print machine print cartridge, using fine nozzle, reduces the pattern set by substrate surface inkjet printing computer, i.e., in mobility oil phase
The oil-water interfaces structure of finishing patterns.In Fig. 2,1 is conductive presoma water-base ink, and 2 be reproducibility liquid elastomer prepolymer
Oiliness substrate, 3 be emulsion layer, and 4 be the conductive presoma of water phase, and 5 reduce substrate for oil phase.
Specific implementation method prepared by the oil-in-water emulsified layer that oil-water interfaces are stablized is the profit under micro- ultrasonic mechanical shear stress
Make conductive precursor water solution that emulsification occur to the oiliness substrate of mobility with emulsifying agent, form oil-in-water emulsion layer.
So as to form in continuous water phase the emulsion layer for including a large amount of oiliness drops at oil-water interfaces.
The specific implementation method that generation metal composite structure is reacted using oil-water interfaces is control grease system temperature, makes to lead
The reduction reaction that metal ion occurs with reducing agent on oil-water interfaces for electric presoma generates continuous metal layer.Finally, pre-
After polymers cures, based on oil-water interfaces emulsion layer and interfacial reaction, the composite construction that metal wraps up elastomeric polymer is realized.Cause
This, metal composite structure is that the continuous cured elasticity of metal layer parcel of interfacial reaction generation occurs by oil-water interfaces emulsion layer to gather
What compound was formed.
The stretchable circuit of structure metal composite structure and electronic device are also needed in the implementation of the present invention, content is embodied
It is the composition and thickness using the factors such as interfacial reaction temperature, reactant concentration, kinds of surfactants regulation and control metal composite structure
Degree.The metal composite structure of oil-water interfaces reaction generation and the relation of performance are obtained, lifts the application performance of stretchable circuit.Base
In oil-water interfaces reaction inkjet printing metal composite structure prepare stretchable circuit, realize electronic circuit labels, electronic skin,
Application in the stretchable electronic device such as Flexible Displays.
Specific embodiment:
1. dimethyl silicone polymer substrate is mixed into formic acid leaf-alcohol ester as reducing agent liquid oil phase substrate.
2. 30% ammonia aqueous solution is diluted five times, slowly to nitre by silver nitrate with 10% concentration obtained aqueous solution
It is added dropwise in sour silver solution, until precipitation disappears after occurring again, stops dropwise addition and obtain corresponding silver-colored ammonia precursor ink.
3. using ink-jet printing apparatus into row line print, to oiliness can precuring liquid substrate carry out precuring processing,
At 70 degrees Celsius, kept for 8 minutes under normal pressure.
Reacted 4. the oil-water interfaces system of ink jet printing is placed on 30 DEG C to 90 DEG C of warm table, obtain metal
The different stretchable circuit of composite construction.
5. changing content silver-colored in ink-jet precursor ink, controlled respectively from 5%-20% mass fractions, ink jet printing
Temperature parameter, obtains the different stretchable circuit of metal composite structure.
6. changing the type of the surfactant in ink-jet ink, such as polyethylene glycol, ethylene glycol, glycol monoethyl ether, divide
Not Zuo Wei surfactant, temperature, content silver-colored in precursor ink are controlled in ink jet printing, metal composite structure is obtained and differs
The stretchable circuit of sample.Fig. 3 is that metal composite structure lifts the stretchable impact of performance figure of circuit in the embodiment of the present invention.
7. for temperature at 70 DEG C, for precursor ink mass concentration 10%, surfactant is the condition of polyethylene glycol
The stretchable circuit of ink jet printing of formation, circuit is bent, stretchable excellent performance, as the printed electronic under stress condition
Skin device.
8 for temperature at 50 DEG C, for precursor ink mass concentration 20%, surfactant is the condition shape of polyethylene glycol
Into the stretchable circuit of ink jet printing, circuit is bent, has micro-nano composite conductive layers, as flexible super capacitor
Collector and electrode activation material, all print prepare flexible super capacitor.
Finally it should be noted that:Above-described embodiments are merely to illustrate the technical scheme, rather than to it
Limitation;Although the present invention is described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that:
It can still modify the technical solution described in previous embodiment, or to which part or all technical characteristic into
Row equivalent substitution;And these modifications or substitutions, the essence of appropriate technical solution is departed from various embodiments of the present invention technical side
The scope of case.
Claims (10)
- A kind of 1. method for preparing stretchable circuit using oil-water interfaces reaction inkjet printing, it is characterised in that:It includes following Step:S1, utilize the patterned oil-water interfaces system of inkjet printing structure:Reproducibility liquid prepolymer oiliness substrate is prepared, also Originality liquid prepolymer oiliness substrate surface inkjet printing conduction presoma water-base ink, builds patterned oil-water interfaces body System;It is prepared by S2, oil-water interfaces oil-in-water emulsified layer:Surfactant is added in conductive presoma water-base ink in S1, and Shearing force is applied to oil-water interfaces, obtains stable oil-in-water emulsified layer;The composite construction of S3, oil-water interfaces reaction generation metal parcel elastomeric polymer:The oil-in-water breast of the stabilization obtained to S2 Change layer and apply temperature control, the reduction of metal ion occurs in water-oil interface for conductive presoma water-base ink and surfactant Reaction generates continuous metal layer, and after curing to reproducibility liquid prepolymer oiliness substrate, it is poly- to obtain metal parcel elasticity The composite construction of compound;S4, the composite construction of the metal obtained using S3 parcel elastomeric polymer form stretchable circuit, and to stretchable circuit Electric property carry out electric conductivity test, and to circuit carry out multi-drawing, the electric conductivity in drawing process is tested, And then by varying the control parameter in preparation process, obtain the stretchable circuit of best performance.
- 2. the method according to claim 1 for preparing stretchable circuit using oil-water interfaces reaction inkjet printing, its feature It is:Shearing force is applied to oil-water interfaces using micro- ultrasound in S2.
- 3. the method according to claim 1 for preparing stretchable circuit using oil-water interfaces reaction inkjet printing, its feature It is:Temperature regulation and control are changed in S3 between 30 DEG C to 90 DEG C, obtain the stretchable circuit with different electric properties.
- 4. the method according to claim 1 for preparing stretchable circuit using oil-water interfaces reaction inkjet printing, its feature It is:The composition of interfacial reaction temperature, reactant concentration and kinds of surfactants regulation and control metal composite structure is utilized in S4 And thickness, the relation of the metal composite structure and its electric property of oil-water interfaces reaction generation is obtained, selects optimized parameter to obtain The stretchable circuit of best performance.
- 5. the method according to claim 4 for preparing stretchable circuit using oil-water interfaces reaction inkjet printing, its feature It is:In S4 at 70 DEG C, the electric property of obtained metal composite structure is stablized the most, and conductivity keeps one under stretching condition Cause.
- 6. the method according to claim 1 for preparing stretchable circuit using oil-water interfaces reaction inkjet printing, its feature It is:The preparation of reproducibility liquid prepolymer oiliness substrate comprises the following steps in S1:Elastomeric prepolymer is chosen, then makes mass fraction of the reducing agent in liquid prepolymer oiliness substrate be 8%- by a certain percentage 12%, it is subject to the viscoelastic fluid flow behavior for not influencing substrate;The reducing agent of the functional group containing reproducibility is added thereto, obtains mixture, and spin coating or extrusion said mixture prepare reduction Property liquid elastomer prepolymer oiliness substrate.
- 7. the method according to claim 1 for preparing stretchable circuit using oil-water interfaces reaction inkjet printing, its feature It is:The substrate of initiator preparation is uniformly added, it is necessary under normal pressure for the dimethyl silicone polymer by thermohardening type in S1, Precuring 7-8 minutes is carried out in 70 DEG C of baking oven, obtains that there is viscoelastic mobility substrate.
- 8. the method according to claim 1 for preparing stretchable circuit using oil-water interfaces reaction inkjet printing, its feature It is:Structure patterning oil-water interfaces system comprises the following steps in S1:The surface tension matching of ink-jet ink and printed substrates is adjusted, by prepared conductive precursor ink injection printer Print cartridge, in the pattern of mobility oil phase reduction substrate surface inkjet printing setting, the oil-water interfaces structure of finishing patterns.
- 9. the method according to claim 1 for preparing stretchable circuit using oil-water interfaces reaction inkjet printing, its feature It is:Elastomeric prepolymer is uniformly to add initiator by the dimethyl silicone polymer of thermohardening type to prepare.
- 10. the method according to claim 1 for preparing stretchable circuit using oil-water interfaces reaction inkjet printing, its feature It is:Reducing agent in S1 is the compound containing aldehyde radical.
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CN109080281A (en) * | 2018-08-10 | 2018-12-25 | 齐鲁工业大学 | The method for preparing flexible transparent conducting film based on the fine inkjet printing of wellability substrate |
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WO2004020065A3 (en) * | 2002-08-28 | 2005-04-28 | Mt Technologies Inc | Microfluidic affinity system using polydimethylsiloxane and a surface modification process |
CN103219243A (en) * | 2012-09-28 | 2013-07-24 | 复旦大学 | Manufacturing method of patterning metal lines |
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Effective date of registration: 20221222 Address after: Room 3115, No. 135, Ward Avenue, Ping'an Street, Changqing District, Jinan, Shandong 250300 Patentee after: Shandong Jiqing Technology Service Co.,Ltd. Address before: 250353 No. 3501, Daxue Road, Jinan City, Shandong Province Patentee before: Qilu University of Technology |