CN106211606B - A kind of the heat ultrasound sintering method and its device of the compound ink of nano silver/graphene - Google Patents

A kind of the heat ultrasound sintering method and its device of the compound ink of nano silver/graphene Download PDF

Info

Publication number
CN106211606B
CN106211606B CN201610576017.0A CN201610576017A CN106211606B CN 106211606 B CN106211606 B CN 106211606B CN 201610576017 A CN201610576017 A CN 201610576017A CN 106211606 B CN106211606 B CN 106211606B
Authority
CN
China
Prior art keywords
sintering
graphene
nano silver
compound ink
heat
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201610576017.0A
Other languages
Chinese (zh)
Other versions
CN106211606A (en
Inventor
王福亮
朱海新
何虎
李军辉
朱文辉
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Central South University
Original Assignee
Central South University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Central South University filed Critical Central South University
Priority to CN201610576017.0A priority Critical patent/CN106211606B/en
Publication of CN106211606A publication Critical patent/CN106211606A/en
Application granted granted Critical
Publication of CN106211606B publication Critical patent/CN106211606B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00Apparatus or processes for manufacturing printed circuits
    • H05K3/10Apparatus 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
    • H05K3/12Apparatus 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
    • H05K3/1283After-treatment of the printed patterns, e.g. sintering or curing methods
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/52Electrically conductive inks
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00Printed circuits
    • H05K1/02Details
    • H05K1/09Use of materials for the conductive, e.g. metallic pattern
    • H05K1/092Dispersed materials, e.g. conductive pastes or inks
    • H05K1/097Inks comprising nanoparticles and specially adapted for being sintered at low temperature
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2203/00Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
    • H05K2203/02Details related to mechanical or acoustic processing, e.g. drilling, punching, cutting, using ultrasound
    • H05K2203/0285Using ultrasound, e.g. for cleaning, soldering or wet treatment

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Dispersion Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)

Abstract

The invention discloses the ultrasonic sintering methods of heat and its device of a kind of compound ink of nano silver/graphene, by nano silver powder and graphene dispersion in mixed organic solvents, the compound ink of nano silver/graphene that configuration quality percentage is 0.01%~90%;The highly viscous compound ink of nano silver/graphene is extruded from packing element by air pressure, is scribbled by Glue dripping head and forms the flexible base board with conducting channel on flexible substrates;Between the flexible base board with conducting channel of drying is placed on two layers of PDMS protection plastics, applies pressure and reach 3~30MPa of desirable value;Heating temperature is 60~160 DEG C;Then, under conditions of 3~30MPa, 60 160 DEG C, carry out hot pressing pre-sintering, sintering time is 1 10 minutes, heat ultrasound sintering is carried out under conditions of 3 30MPa, 60 160 DEG C, sintering time is 1 10 minutes, passes through ultrasound, the effect of pressure and temperature, it realizes the solid-state diffusion between nano silver/graphene, prepares the flexible circuit with excellent conductive performance and mechanical deflection performance.

Description

A kind of the heat ultrasound sintering method and its device of the compound ink of nano silver/graphene
Technical field
The present invention relates to the conducting channel preparation methods in a kind of flexible electronic field, and nanometer is used more particularly to a kind of High intensity, the low resistance flexible circuit preparation method of the compound ink of silver/graphite alkene.The invention further relates to a kind of realization nanometers The device of the ultrasonic sintering method of heat of the compound ink of silver/graphite alkene.
Background technology
Wearable intelligent equipment is the developing direction in electronics industry future, and flexible electronic technology is key technology therein. Flexible electronic can be summarized as being that organic/inorganic materials electronic device is produced on flexibility/Drawability plastics or metal sheet New electronic technology, with its unique flexibility/ductility and efficient, low cost manufacturing technique, in information, the energy, medical treatment, state Anti- equal fields have wide application prospect.It is the main development side of flexible circuit using nano metal ink as the paper substrate circuit of medium One of to, it disperses nano metal powder in organic solvent, to prepare conductive ink, passes through ink jet printing, deposition sputtering plating Ink is deposited on paper base plate by the modes such as film and spray gun spraying prepares circuit.For this purpose, each research institution proposes a variety of preparations The method of nano-metal particle conductive ink and flexible circuit.Chinese patent CN 1437200 proposes a kind of according to nanometer silver granuel Sub- self assembly and low temperature fusion welding property, the method that filling epoxy resin reduces colloid viscosity;Chinese patent CN 104877464A are carried A kind of method preventing nano-metal particle reunion using surfactant is gone out.
But the conducting channel prepared with simple nano metal (being mostly nano silver) ink, due to nanometer after sintering There are gap between grain, electric conductivity, mechanical property can not show a candle to continuous block metal material, greatly limit the hair of the technology Exhibition and application.
Graphene is a kind of new material with superior electrical, mechanics, thermal property found 21 century, it is both most Thin material, and most tough material, 200 times more taller than best steel of fracture strength.It has good bullet again simultaneously Property, stretch range can reach the 20% of own dimensions.It is that current nature is most thin, the highest material of intensity, and price is low It is honest and clean.Graphene and nano metal powder are mixed with circuit, there are gap, enhancing electricity between nano particle after being sintered with filling The electric conductivity on road, mechanical property are to solve one of the method that pure nano metal ink prepares flexible circuit problem at present.
But the introducing of graphene brings and writes inconvenient (graphene is easy to block traditional writing nib), sintering temperature Spend the problems such as high, sintering time is long, circuitous resistance rate is big after sintering.Therefore, it is necessary to develop a kind of novel nano silver/graphite The writing of the compound ink of alkene and sintering method, to prepare the flexible circuit of high intensity, low-resistivity.
Invention content
First technical problem to be solved by this invention be propose it is a kind of realize high intensity, low-resistivity flexible circuit The ultrasonic sintering method of heat of the compound ink of nano silver/graphene of preparation.
Boundary technical problem to be solved by this invention is to provide a kind of heat for realizing the compound ink of nano silver/graphene The device of ultrasonic sintering method.
In order to solve above-mentioned first technical problem, the heat ultrasound of the compound ink of nano silver/graphene provided by the invention Sintering method includes the following steps:
(1), the compound ink of nano silver/graphene is configured:Absolute ethyl alcohol, polyethylene glycol and glycerine are passed through into ultrasonic vibration It mixes, forms the mixed organic solvents that viscosity is 0.01~100 Pa Sec;Then by churned mechanically mode by nanometer Silver powder and graphene by nano Silver quality percentage are 96~99.9%, graphene mass percent is 4%~0.1% dispersion In mixed organic solvents, configuration quality percentage be 0.01%~90% the compound ink of nano silver/graphene;Then it will mix It is filling in Glue dripping head to close the uniform compound ink of nano silver/graphene, prepares circuit and writes;
(2), the writing of the compound ink of nano silver/graphene:By air pressure by highly viscous nano silver/graphene composite ink Water is extruded from packing element, is scribbled by Glue dripping head and is formed the flexible base board with conducting channel on flexible substrates;
Finally by the printed flexible base board with conducting channel be placed in drying oven with 55 DEG C~65 DEG C dry 2 hours~ 4 hours, to remove volatilizable organic solvent;It then takes out to carry the flexible base board of conducting channel, carries out the burning of next step Knot;
(3), the ultrasonic sintering process of the heat of the compound ink of nano silver/graphene is:By the flexibility with conducting channel of drying Substrate is placed between two layers of PDMS protection plastics, and the thickness of PDMS is 100~500 microns, is then placed on flexible base board and adds In thermal station;By ultrasonic transducer end pressure on flexible substrates, on flexible base board apply pressure reach desirable value 3~ 30MPa;It is 60~160 DEG C that warm table carries out heating temperature to flexible base board;Then, in 3~30MPa, 60~160 DEG C of condition Under, hot pressing pre-sintering is carried out, sintering time is 1~10 minute, next, under conditions of 3~30MPa, 60~160 DEG C, is opened Ultrasonic vibration is opened, heat ultrasound sintering is carried out, sintering time is 1~10 minute, by ultrasound, the effect of pressure and temperature, is realized Solid-state diffusion between nano silver/graphene forms flexible circuit, prepares with excellent conductive performance and mechanical deflection performance Flexible circuit.
It is 99.5% that nano silver powder and graphene, which press nano Silver quality percentage, in above-mentioned steps (1), graphene quality Percentage is 0.5%.
By the absolute ethyl alcohol, polyethylene glycol and glycerine with percent by volume 50 in above-mentioned steps (1):45:5 pass through Ultrasonic vibration mixes.
Flexible base board described in above-mentioned steps (1) is filter paper, rubber or printing paper.
The thickness of PDMS described in above-mentioned steps (3) is 300 microns.
Reach desirable value 15MPa to applying pressure on flexible circuit board sample described in above-mentioned steps (3), it is described It is 120 DEG C that warm table carries out heating temperature to flexible circuit board sample.
Carry out hot pressing pre-sintering described in above-mentioned steps (3), sintering time are 4 minutes;Described in progress heat ultrasound Sintering, sintering time are 4 minutes.
The supersonic frequency used in heat ultrasound sintering described in above-mentioned steps (3) is 20-120kHz;Power is 100- 3000W。
The supersonic frequency used in heat ultrasound sintering described in above-mentioned steps (3) is 35kHz;Power is 500W.
In order to solve above-mentioned second technical problem, the heat provided by the invention for realizing the compound ink of nano silver/graphene The device of ultrasonic sintering method, including the writing system of the compound ink of nano silver/graphene and the compound ink of nano silver/graphene The ultrasonic sintering system of heat, the structure of the writing system of the compound ink of nano silver/graphene is:Pedestal is write to be equipped with Column and upper and lower translation platform and writing movements translation stage are write, the writing column and upper and lower translation platform are equipped with to write and fix Holder, the writing fixing bracket, which is equipped with, writes force snesor and packing element, and the upper end of the packing element passes through tracheae and sky Air pressure force controller connects, and the lower end of the packing element is connected with Glue dripping head;The writing movements translation stage, write column and Upper and lower translation platform writes force snesor and air pressure controller and writes control computer using communication connection;Described receives The structure of the ultrasonic sintering system of heat of the rice compound ink of silver/graphite alkene is:It is sintered pedestal and is equipped with sintering column and upper and lower translation Platform and sintering motion translation platform, the sintering column and upper and lower translation platform are equipped with and are sintered to fix holder, and the sintering is solid Fixed rack is equipped with sintering force snesor and energy converter, the energy converter are connect with ultrasonic generator, the energy converter Front end is equipped with amplitude transformer, and the front end of the amplitude transformer is equipped with tool heads;The sintering motion translation platform is equipped with warm table; The sintering column and upper and lower translation platform, sintering motion translation platform, warm table, sintering force snesor and ultrasonic generator and burning Control computer is tied using communication connection.
Using the ultrasonic sintering method of the heat of the compound ink of nano silver/graphene of above-mentioned technical proposal and its device, prepare Flexible circuit have good conductive property.As sintering time increases, the flexibility of the compound ink preparation of nano silver/graphene The average resistivity of circuit is since 1.6 Ω | and it is continuously decreased m, at 16 minutes, reaches lower resistivity, be fine silver resistance 1.87 times of rate, are further added by sintering time later, and resistivity is not decreased obviously;And prepared by the pure nano silver conductive ink of tradition For flexible circuit in identical sintering time, flexible circuit prepared by resistivity ink all more compound than nano silver/graphene is big.Explanation Flexible circuit prepared by the method for the present invention has preferable electric conductivity.
1) using flexible circuit prepared by the above method has good mechanical resistance bending performance.Mechanical resistance bending performance Test method is:The both ends for holding flexible circuit, the bending being repeated, and every 300 times, sample is averaged after measurement bending Resistance passes through the mechanical resistance bending performance for changing energy judgement sample of resistance.As bending number increases to 3000 times from 0, this The average resistance of flexible circuit prepared by the compound ink of invention nano silver/graphene only increases to 0.6 ohm from 0.51;And it passes The resistance that pure nano silver conductive ink of uniting prepares circuit then increases to 0.92 ohm from 0.7.Illustrate prepared by the method for the present invention Flexible circuit has preferable mechanical deflection performance.
Advantageous effect using the present invention has:
1, graphene has excellent electric conductivity and larger specific surface area, and the graphene film in conductive ink can be by phase Together, even if there is gap between nano-Ag particles, the bridge joint of graphene film can form excellent electricity to adjacent nano-Ag particles bridge joint Channel, hence it is evident that electric conductivity, the mechanical property for improving circuit make up the harmful effect that pore belt is come.
2, nano silver and graphene can equably, with different mass percents be dispersed in mixed organic solvents, mixing Organic solvent has good hydrophily, and can change hybrid conductive ink viscosity as needed, therefore, can be in different substrates On, with different nano silvers and graphene mass percent, write various required circuits.
3, hybrid conductive ink is write using dispensing method, it can be big by adjusting Glue dripping head bore, ink viscosity, air pressure It is small, to adjust the width and thickness of prepared flexible circuit.
4, the dispenser system controlled by computer can use common modeling software (such as PorE, CAD) to establish circuit pattern mould Type is printed after importing model, realizes prepared by required variously-shaped circuit.
5, using ultrasonic wave added hot pressed sintering, the gap between nano-Ag particles is reduced, increases the compactness of sample, is improved soft The conductive capability of property circuit.
6, quick (8 points of nano silver/graphene circuit be can be achieved under 120 DEG C, the low temperature and lower pressure of 15MPa Clock) sintering.
In conclusion the present invention be it is a kind of realize high intensity, low-resistivity flexible circuit prepare nano silver/graphene The ultrasonic sintering method of heat and its device of compound ink.
Description of the drawings
Fig. 1 is the structural schematic diagram of the writing system of the compound ink of nano silver/graphene of the present invention.
Fig. 2 is the structural schematic diagram of the ultrasonic sintering system of heat of the compound ink of nano silver/graphene of the present invention.
Fig. 3 is the photo of paper substrate nano silver/graphene flexible circuit prepared by the method for the present invention.
Fig. 4 is influence diagram of the sintering time to flexible circuit conductive performance.
Fig. 5 is the bend resistance the performance test results figure of flexible circuit.
Specific implementation mode
The invention will be further described below in conjunction with the accompanying drawings.
Referring to Fig. 1 and Fig. 2, the heat ultrasonic sintering method provided by the invention for realizing the compound ink of nano silver/graphene Device includes the heat ultrasound sintering system of the writing system of the compound ink of nano silver/graphene and the compound ink of nano silver/graphene System, the structure of the writing system of the compound ink of nano silver/graphene are:It writes pedestal 11 and is equipped with writing column and upper and lower translation Platform 2 and writing movements translation stage 12, write column and upper and lower translation platform 2 is equipped with and writes fixing bracket 7, write fixing bracket 7 It is equipped with writing force snesor 4 and packing element 6, the upper end of packing element 6 is connect by tracheae 5 with air pressure controller 3, packing element 6 Lower end is connected with Glue dripping head 9;Equipped with the compound ink of nano silver/graphene 8 in packing element 6;Glue dripping head 9 is to just writing motion translation platform 12;Writing movements translation stage 12 writes column and upper and lower translation platform 2, writes force snesor 4 and air pressure controller 3 and book Control computer 1 is write using communication connection;The structure of the ultrasonic sintering system of heat of the compound ink of nano silver/graphene is:Sintering Pedestal 21 is equipped with sintering column and upper and lower translation platform 14 and sintering motion translation platform 20, is sintered on column and upper and lower translation platform 14 Equipped with holder 18 is sintered to fix, is sintered to fix holder 18 and is equipped with sintering force snesor 16 and energy converter 17, energy converter 17 with it is super Acoustic generator 15 connects, and the front end of energy converter 17 is equipped with amplitude transformer 23, and the front end of amplitude transformer 23 is equipped with tool heads 22;Sintering movement Translation stage 20 is equipped with warm table 19;Flexible base board 10 is placed on warm table 19, flexible base board 10 is submitted a written statement to a higher authority with flexible circuit 25;Flexible base board 10 is equipped with upper PDMS protective films 24 and lower PDMS protective films 26;Tool heads 22 are to positive warm table 19;Sintering is vertical Column and upper and lower translation platform 14, sintering motion translation platform 20, warm table 19, sintering force snesor 16 and ultrasonic generator 15 and sintering Control computer 13 is using communication connection.
Referring to Fig. 1, Fig. 2 and Fig. 3, the ultrasonic sintering method of heat of the compound ink of nano silver/graphene provided by the invention, packet Include following steps:
1) the compound ink of nano silver/graphene is configured:By absolute ethyl alcohol, polyethylene glycol and glycerine with percent by volume 50:45:5 are mixed by ultrasonic vibration, form a kind of big viscosity mixed organic solvents, by changing above-mentioned three kinds of components Percent by volume, mixed organic solvents of the viscosity from 0.01~100 Pa Sec of various viscosity can be formed;Then pass through mechanical agitation Mode by nano silver powder and graphene be 96~99.9% by nano Silver quality percentage, graphene mass percent is 4%~0.1%, preferably 99.5%:0.5% is dispersed in mixed organic solvents, is dispersed in mixed organic solvents, due to mixing The viscosity of organic solvent can be adjusted arbitrarily, therefore, can be realized multiple from nano silver/graphenes of 0.01%-90% mass percents Close the configuration of ink 8;And traditional ink proportioning, it is difficult to realize 10% or more mass percent proportioning;Then it will mix equal The compound ink 8 of even nano silver/graphene is filling in packing element 6, and packing element 6 is fixed on and is write on fixing bracket 7, prepares electricity Road book is write.
2) writing of the compound ink of nano silver/graphene 8:It opens and writes control computer 1, circuit model is imported flexible Circuit writes control software, and carries out hierarchy slicing and path planning.Adjust the Glue dripping head 9 and writing movements translation stage of packing element 6 12 opposite positions reach optimum position when distance between the two reaches 1mm, and Glue dripping head 9 is fixed.Open air pressure Air pressure adjustment is reached 10psi, by air pressure by the compound ink 8 of highly viscous nano silver/graphene, from packing element by force controller 3 It is extruded in 6, writing on flexible base board 10 by the painting of Glue dripping head 9, (flexible base board 10 is filter paper, rubber or printing paper, herein preferred phase Paper) on, meanwhile, 12 movement flexible base board 10 of writing movements translation stage is controlled by writing control computer 1, in flexible base board Required various circuit patterns are formed on 10.The width of circuit can be changed by changing the diameter of Glue dripping head 9.The above method can be real The now uniform book from the compound ink of nano silver/graphene of 0.01%-90% mass percents 8 on various flexible base boards 10 It writes, and traditional ball pen head Writing method, it can only realize that 10% or more mass percent matches the book of pure silver ink It writes.
Finally by printed the flexible base board 10 with conducting channel be placed in drying oven with 60 DEG C dry 3 hours, to go Except volatilizable organic solvent;It then takes out to carry the flexible base board 10 of conducting channel, carries out the sintering of next step.
3) the ultrasonic sintering process of the heat of the compound ink of nano silver/graphene is:Flexibility by drying, with conducting channel Substrate 10 is put between PDMS protective films 24 and lower PDMS protective films 26, upper PDMS protective films 24 and lower PDMS protective films 26 Thickness is 100~500 microns, preferably 300 microns, flexible circuit can be protected not contaminated and reduce ultrasound and transmitted Then flexible base board 10 is placed on warm table 19 by the amplitude fading in journey;It is sintered the control sintering column of control computer 13 And upper and lower translation platform 14 moves down, and the tool heads 22 of 17 end of energy converter are pressed on flexible base board 10, meanwhile, sintering control The detection sintering force snesor 16 of computer 13, until the pressure applied on flexible base board 10 reaches 3~30MPa of desirable value, preferably 15MPa;At the same time, sintering control computer 13 controls warm table 19 and is heated to flexible base board 10, and temperature is 60~160 DEG C, preferably 120 degrees Celsius;Then, under conditions of 15MPa, 120 DEG C, hot pressing pre-sintering is carried out, sintering time is 1~10 point Clock, preferably 4 minutes open ultrasonic generator 15 and carry out ultrasonic vibration, carry out heat next, under conditions of 15MPa, 120 DEG C Ultrasound sintering, sintering time be 1~10 minute, preferably 4 minutes, by ultrasound, pressure and temperature effect, realize nano silver/ Solid-state diffusion between graphene forms conductive flex circuitry, prepares with excellent conductive performance and mechanical deflection performance Flexible circuit.Above-mentioned heat ultrasound sintering supersonic frequency used is 20-120kHz, preferably 35kHz;Power is 100-3000W, excellent 500W is selected, the structure that substrate is destroyed to avoid excessive power closes the integrality of circuit after the completion of sintering, while being avoided that too small Power can not provide sintering needed for energy.Sintered circuit is as shown in Figure 3.
The flexible circuit prepared using the above method is had good conductive property.Fig. 4 is sintering time to flexible circuit The affecting laws of resistivity, as shown in Figure 4:As sintering time increases, the flexible electrical of the compound ink preparation of nano silver/graphene The average resistivity on road is since 1.6 Ω | and it is continuously decreased m, at 16 minutes, reaches lower resistivity, be fine silver resistivity 1.87 times, be further added by sintering time later, resistivity is not decreased obviously;And the pure nano silver conductive ink preparation of tradition is soft Property circuit in identical sintering time, flexible circuit prepared by resistivity ink all more compound than nano silver/graphene is big.Illustrate this Flexible circuit prepared by inventive method has preferable electric conductivity.
There is good mechanical resistance bending performance using flexible circuit prepared by the above method.The survey of mechanical resistance bending performance Method for testing is:The both ends for holding flexible circuit, the bending being repeated, and every 300 times, measure the average electricity of sample after bending Resistance passes through the mechanical resistance bending performance for changing energy judgement sample of resistance.Test result such as Fig. 5, as seen from the figure:With bending time Number increases to 3000 times from 0, the average resistance of flexible circuit prepared by the compound ink of nano silver/graphene of the present invention only from 0.51 increases to 0.6 ohm;And the resistance that the pure nano silver conductive ink of tradition prepares circuit then increases to 0.92 ohm from 0.7. Illustrate that the flexible circuit prepared by the method for the present invention has preferable mechanical deflection performance.

Claims (10)

1. a kind of ultrasonic sintering method of the heat of compound ink of nano silver/graphene, it is characterized in that:Include the following steps:
(1), the compound ink of nano silver/graphene is configured:Absolute ethyl alcohol, polyethylene glycol and glycerine are mixed by ultrasonic vibration Together, the mixed organic solvents that viscosity is 0.01~100 Pa Sec are formed;Then by churned mechanically mode by nano-silver powder End and graphene by nano Silver quality percentage are 96~99.9%, graphene mass percent be 4%~0.1% be dispersed in it is mixed It closes in organic solvent, the compound ink of nano silver/graphene that configuration quality percentage is 0.01%~90%;Then it will mix equal The even compound ink of nano silver/graphene is filling in Glue dripping head, prepares circuit and writes;
(2), the writing of the compound ink of nano silver/graphene:By air pressure by the highly viscous compound ink of nano silver/graphene from It is extruded in packing element, is scribbled by Glue dripping head and form the flexible base board with conducting channel on flexible substrates;
Finally the flexible base board with conducting channel is placed in drying oven and is dried 2 hours~4 hours with 55 DEG C~65 DEG C, with removal Volatilizable organic solvent;It then takes out to carry the flexible base board of conducting channel, carries out the sintering of next step;
(3), the ultrasonic sintering process of the heat of the compound ink of nano silver/graphene is:By the flexible base board with conducting channel of drying, It is placed between two layers of PDMS protection plastics, the thickness of PDMS is 100~500 microns, and flexible base board is then placed on warm table On;On flexible substrates by ultrasonic transducer end pressure, reach 3~30MPa of desirable value to application pressure on flexible base board;Add The heating that thermal station is 60~160 DEG C into trip temperature to flexible base board;Then, under conditions of 3~30MPa, 60~160 DEG C, into Row hot pressing is pre-sintered, and sintering time is 1-10 minutes, next, under conditions of 3~30MPa, 60~160 DEG C, opens ultrasound Vibration, carry out heat ultrasound sintering, sintering time be 1~10 minute, by ultrasound, pressure and temperature effect, realize nano silver/ Solid-state diffusion between graphene forms flexible circuit, prepares the flexibility with excellent conductive performance and mechanical deflection performance Circuit.
2. the ultrasonic sintering method of the heat of the compound ink of nano silver/graphene according to claim 1, it is characterized in that:It is above-mentioned By the absolute ethyl alcohol, polyethylene glycol and glycerine with percent by volume 50 in step (1):45:5 are mixed by ultrasonic vibration Together.
3. the ultrasonic sintering method of the heat of the compound ink of nano silver/graphene according to claim 1 or 2, it is characterized in that:On It is filter paper, rubber or printing paper to state the flexible base board described in step (1).
4. the ultrasonic sintering method of the heat of the compound ink of nano silver/graphene according to claim 1 or 2, it is characterized in that:On It is 99.5% that nano silver powder and graphene, which are stated in step (1), by nano Silver quality percentage, and graphene mass percent is 0.5%.
5. the ultrasonic sintering method of the heat of the compound ink of nano silver/graphene according to claim 1 or 2, it is characterized in that:On State and reach desirable value 15MPa to applying pressure on flexible base board described in step (3), the warm table to flexible base board into Row heating temperature is 120 DEG C.
6. the ultrasonic sintering method of the heat of the compound ink of nano silver/graphene according to claim 1 or 2, it is characterized in that:On The thickness for stating the PDMS described in step (3) is 300 microns.
7. the ultrasonic sintering method of the heat of the compound ink of nano silver/graphene according to claim 1 or 2, it is characterized in that:On The carry out hot pressing pre-sintering described in step (3) is stated, sintering time is 4 minutes;The progress heat ultrasound sintering, sintering time It is 4 minutes.
8. the ultrasonic sintering method of the heat of the compound ink of nano silver/graphene according to claim 1 or 2, it is characterized in that:On The supersonic frequency stated used in the heat ultrasound sintering described in step (3) is 20-120kHz;Power is 100-3000W.
9. the ultrasonic sintering method of the heat of the compound ink of nano silver/graphene according to claim 1 or 2, it is characterized in that:On The supersonic frequency stated used in the heat ultrasound sintering described in step (3) is 35kHz;Power is 500W.
10. realizing the device of the ultrasonic sintering method of the heat of the compound ink of nano silver/graphene described in claim 1, feature It is:The heat ultrasound sintering system of writing system and the compound ink of nano silver/graphene including the compound ink of nano silver/graphene System, the structure of the writing system of the compound ink of nano silver/graphene are:Write pedestal (11) be equipped with write column and Upper and lower translation platform (2) and writing movements translation stage (12) are write, the writing column and writing upper and lower translation platform (2) are equipped with Fixing bracket (7) is write, the writing fixing bracket (7), which is equipped with, writes force snesor (4) and packing element (6), the glue The upper end of cylinder (6) is connect by tracheae (5) with air pressure controller (3), and the lower end of the packing element (6) is connected with Glue dripping head (9);The writing movements translation stage (12) writes column and writes upper and lower translation platform (2), writes force snesor (4) and empty Air pressure force controller (3) uses communication connection with control computer (1) is write;The compound ink of nano silver/graphene The structure of hot ultrasound sintering system is:It is sintered pedestal (21) and is equipped with sintering column and sintering upper and lower translation platform (14) and sintering fortune Dynamic translation stage (20), the sintering column and sintering upper and lower translation platform (14), which are equipped with, is sintered to fix holder (18), described It is sintered to fix holder (18) and is equipped with sintering force snesor (16) and energy converter (17), the energy converter (17) occurs with ultrasound Device (15) connects, and the front end of the energy converter (17) is equipped with amplitude transformer (23), and the front end of the amplitude transformer (23) is equipped with work Has head (22);The sintering motion translation platform (20) is equipped with warm table (19);The sintering column and sintering is flat up and down Moving stage (14), sintering motion translation platform (20), warm table (19), sintering force snesor (16) and ultrasonic generator (15) and sintering Control computer (13) is using communication connection.
CN201610576017.0A 2016-07-20 2016-07-20 A kind of the heat ultrasound sintering method and its device of the compound ink of nano silver/graphene Active CN106211606B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610576017.0A CN106211606B (en) 2016-07-20 2016-07-20 A kind of the heat ultrasound sintering method and its device of the compound ink of nano silver/graphene

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610576017.0A CN106211606B (en) 2016-07-20 2016-07-20 A kind of the heat ultrasound sintering method and its device of the compound ink of nano silver/graphene

Publications (2)

Publication Number Publication Date
CN106211606A CN106211606A (en) 2016-12-07
CN106211606B true CN106211606B (en) 2018-08-31

Family

ID=57491978

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610576017.0A Active CN106211606B (en) 2016-07-20 2016-07-20 A kind of the heat ultrasound sintering method and its device of the compound ink of nano silver/graphene

Country Status (1)

Country Link
CN (1) CN106211606B (en)

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107824393A (en) * 2017-11-23 2018-03-23 河北立德电子有限公司 A kind of point glue equipment with ultrasonic vibration and the dispensing method using its progress
US20190174633A1 (en) * 2017-12-05 2019-06-06 Illinois Tool Works Inc. Material temperature sensor for stencil printer
US10933483B2 (en) 2017-12-05 2021-03-02 Illinois Tool Works Inc. IR non-contact temperature sensing in a dispenser
EP3746300B1 (en) * 2018-02-01 2023-05-03 The Procter & Gamble Company System and method for dispensing material
US10849843B2 (en) 2018-02-01 2020-12-01 The Procter & Gamble Company Stable cosmetic ink composition
US10813857B2 (en) 2018-02-01 2020-10-27 The Procter & Gamble Company Heterogenous cosmetic ink composition for inkjet printing applications
CN110429209B (en) * 2018-08-23 2022-01-11 广东聚华印刷显示技术有限公司 Preparation method and processing equipment of metal structure based on roll-to-roll printing technology
CN109623068B (en) * 2019-01-10 2021-02-19 哈尔滨工业大学(深圳) Nano-silver connection method based on multipoint ultrasonic vibration
CN109540374B (en) * 2019-01-10 2024-03-15 中南大学 Ultrasonic sintering packaging device
CN111148363B (en) * 2019-12-31 2021-06-11 浙江理工大学 Method for preparing flexible circuit board by etching-writing nano conductive material on surface of polymer film
CN111239183B (en) * 2020-03-10 2022-03-18 嘉兴学院 Device and method for measuring dynamic thermal conductivity coefficient of silver nanoparticle conductive ink in sintering process
CN116179020B (en) * 2023-03-01 2024-04-19 哈尔滨工业大学(深圳) Preparation method of liquid metal microparticle ink conductive circuit

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2608287A1 (en) * 2011-12-22 2013-06-26 Meggitt A/S Flexible piezoelectric material, production and use thereof
CN105101658A (en) * 2015-09-09 2015-11-25 中南大学 Hot ultrasonic low-temperature sintering method and device of nano silver conductive ink

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2608287A1 (en) * 2011-12-22 2013-06-26 Meggitt A/S Flexible piezoelectric material, production and use thereof
CN105101658A (en) * 2015-09-09 2015-11-25 中南大学 Hot ultrasonic low-temperature sintering method and device of nano silver conductive ink

Also Published As

Publication number Publication date
CN106211606A (en) 2016-12-07

Similar Documents

Publication Publication Date Title
CN106211606B (en) A kind of the heat ultrasound sintering method and its device of the compound ink of nano silver/graphene
Guo et al. One‐step liquid metal transfer printing: toward fabrication of flexible electronics on wide range of substrates
Chang et al. Direct writing and repairable paper flexible electronics using nickel–liquid metal ink
CN105453001B (en) Electronic unit is bonded to patterning nano wire transparent conductor
US11059098B2 (en) Direct printing and writing using undercooled metallic core-shell particles
Ding et al. Preparing of highly conductive patterns on flexible substrates by screen printing of silver nanoparticles with different size distribution
CA2559289A1 (en) Variable watt density layered heater
KR20060012545A (en) Low sintering temperatures conductive nano-inks and a method for producing the same
CN105101658B (en) The hot ultrasonic cryogenic sintering method and device of a kind of nano silver conductive ink
US20220195222A1 (en) Systems and methods of additive printing of functional electronic circuits
Bellitti et al. Resistive sensors for smart objects: Analysis on printing techniques
Lim et al. Surface treatments for inkjet printing onto a PTFE-based substrate for high frequency applications
CN106455311B (en) A method of double-sided flex circuit is made using laser printing
CN113215855B (en) Graphene paper capable of continuously regulating and controlling wettability of various liquids and application thereof
JP2004188286A (en) Thermally conductive coat and method for forming the same
Angeli et al. Advances in printing technologies for soft robotics devices applications
Akin et al. A cold spray-based novel manufacturing route for flexible electronics
Ratnayake et al. Characterizing the conductivity of aerosol jet printed silver features on glass
CN106550548A (en) A kind of laser printing forming method of flexible circuit
CN106313787B (en) A kind of composite wire rod for 3D printing and preparation method thereof
Radivojevic et al. Optimised curing of silver ink jet based printed traces
Faller et al. Hybrid printing for the fabrication of smart sensors
Rahman et al. Fine conductive line printing of high viscosity CuO ink using near field electrospinning (NFES)
Cai et al. Laser sintering of thick-film PTC thermistor paste deposited by micro-pen direct-write technology
Khan et al. Substrate treatment evaluation and their impact on printing results for wearable electronics

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant