CN111885841B - Preparation method of flexible stretchable conductive circuit - Google Patents
Preparation method of flexible stretchable conductive circuit Download PDFInfo
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- CN111885841B CN111885841B CN202010757888.9A CN202010757888A CN111885841B CN 111885841 B CN111885841 B CN 111885841B CN 202010757888 A CN202010757888 A CN 202010757888A CN 111885841 B CN111885841 B CN 111885841B
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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
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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
- H05K3/1283—After-treatment of the printed patterns, e.g. sintering or curing methods
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Abstract
The invention discloses a preparation method of a flexible stretchable conductive circuit, which comprises the following steps of firstly, mixing a dispersing agent, a raw material A and deionized water to obtain a precursor solution containing a conductive reinforcing phase; preparing a metal salt solution and an elastomer film, soaking a semi-permeable membrane by adopting a precursor solution containing a conductive enhanced phase, flatly paving the semi-permeable membrane on the surface of a metal foil, filling the metal salt solution into a test tube of a piezoelectric microdroplet on-demand injection system, repeatedly printing and depositing for 3-5 times on the semi-permeable membrane to form a conductive circuit, and taking down the metal foil; and then separating the conductive circuit from the semi-permeable membrane, moving the conductive circuit to the elastomer film to obtain a film-based conductive circuit, bonding the conductive wire, pouring an elastomer solution on the surface of the film-based conductive circuit, and curing at a proper temperature to obtain the packaged flexible stretchable conductive circuit. The problems that the existing flexible conductive circuit has high requirements on raw material selection, high preparation cost and complex process are solved.
Description
Technical Field
The invention belongs to the technical field of flexible electronic devices, and relates to a preparation method of a flexible stretchable conductive circuit.
Background
The flexible electronics refers to various micro-nano electronic devices manufactured on a flexible substrate, has unique flexibility and ductility, is easy to manufacture in batches at low cost, and has wide application prospects in the fields of wearable electronics, flexible display, man-machine interaction and the like. The conductive circuit is used as a key part for realizing interconnection between electronic elements in the field of flexible electronics, needs to have good flexibility, and can still meet the requirement of normal use when bearing large-amplitude deformation.
The traditional preparation of the flexible conductive circuit mainly adopts the technologies of ink-jet printing, silk-screen printing, nano-imprinting and the like, and directly prints a conductive material on a flexible substrate with a treated surface, thereby preparing the flexible conductive circuit. However, the above production method has problems that the requirement for selecting raw materials is high, the method for treating the surface of the flexible substrate is limited, and the process is complicated.
Disclosure of Invention
The invention aims to provide a preparation method of a flexible stretchable conductive circuit, which solves the problems of high requirement on raw material selection, high preparation cost and complex process of the conventional flexible conductive circuit.
The invention adopts a technical scheme that a preparation method of a flexible stretchable conducting circuit is implemented according to the following steps:
step 1, preparing a precursor solution containing a conductive enhanced phase
Adding the raw material A and a dispersing agent into deionized water, heating until the raw material A and the dispersing agent are completely dissolved, and filtering to obtain a precursor solution containing a conductive enhanced phase for later use;
Dissolving the raw material B in deionized water, stirring uniformly to fully dissolve the raw material B, and filtering to obtain a metal salt solution for later use;
step 4, soaking the semi-permeable membrane by adopting a precursor solution containing a conductive enhanced phase, flatly paving the semi-permeable membrane on the surface of the metal foil, and removing bubbles to completely attach the semi-permeable membrane; and loading the metal salt solution into a test tube of a piezoelectric droplet on-demand jetting system;
the controller controls the two-dimensional motion control platform to move relative to the test tube according to a set path, simultaneously controls the metal salt solution in the test tube to be sprayed out and deposited on the semipermeable membrane, forms a conductive circuit on the semipermeable membrane after repeated printing and deposition for 3-5 times, and takes down the metal foil;
step 6, washing the printed and deposited semipermeable membrane for 2-4 times by using deionized water, and separating the conductive circuit from the semipermeable membrane; moving the conducting circuit to the elastomer film, and placing the elastomer film in a constant-temperature heating furnace for heating treatment to obtain a film-based conducting circuit;
step 7, bonding the film-based conductive circuit and the lead by using conductive silver paste, leading out, and then placing in a constant-temperature heating furnace for heating treatment;
and 8, pouring the elastomer solution on the surface of the film-based conductive circuit, and curing at a proper temperature to obtain the packaged flexible stretchable conductive circuit.
The invention is also characterized in that:
the dispersant is polyvinylpyrrolidone; the raw material A is ascorbic acid, citric acid or oxalic acid; the mass volume concentration of the precursor solution containing the conductive reinforcing phase is 21-48% w/v.
The raw material B is silver nitrate, silver chloride or copper nitrate, the mass volume concentration of the metal salt solution is 40-80% w/v.
The elastomer solution is polydimethylsilane or polybutylene adipate/terephthalate.
In the steps 3 and 8, the curing temperature of the polydimethylsilane is 80 ℃, and the curing time is 40-60 min; or the curing temperature of the poly (butylene adipate/terephthalate) is 23 ℃, and the curing time is 3-6 h.
The semipermeable membrane is cellophane or polylactic acid/cellophane composite membrane with thickness of 25g/m 2 、30g/m 2 、40g/m 2 Or 45g/m 2 (ii) a The metal foil is copper foil, zinc foil or tin foil.
The motion parameters of the two-dimensional motion control platform are as follows: the pulse amplitude is 200V, the pulse width is 10 mus, the pulse frequency is 1Hz, and the dot pitch is 0.075mm.
In step 6, the temperature of the heating treatment is 80-100 ℃, and the time is 10-15 min.
In step 7, the temperature of the heating treatment is 100-110 ℃, and the time is 20-30 min.
The invention has the beneficial effects that:
the invention relates to a preparation method of a flexible stretchable conductive circuit, which takes a semipermeable membrane with a smooth surface, no capillary holes and a deposition layer which is not easy to be fixed as a bottom plate, adopts a droplet-on-demand spraying technology to spray solution droplets on the surface of the semipermeable membrane according to a preset track, deposits a silver layer with excellent conductive performance through chemical reaction to serve as the conductive circuit, and simultaneously combines a transfer printing technology, selects a high-flexibility elastic material as a flexible substrate and a packaging layer, and prepares the flexible conductive circuit capable of bearing large-amplitude deformation (stretching, bending, winding and the like); the preparation method of the flexible stretchable conductive circuit can accurately control patterning of the conductive circuit, has wide raw material selection range, low cost and simple and feasible processing technology, solves the problems of high requirement on raw material selection, high preparation cost and complex process of the conventional flexible conductive circuit, can be widely used for preparing the flexible stretchable conductive circuit, and provides a convenient and feasible scheme for the flexible electronic industry.
Drawings
FIG. 1 is a flow chart of a method of making a flexible stretchable conductive circuit of the present invention;
FIG. 2 is a graph illustrating resistance and stretch ratio of a flexible and stretchable conductive trace according to the present invention.
In the figure, 1, a semi-permeable membrane, 2, a precursor solution containing a conductive reinforcing phase, 3, a metal salt solution, 4, a conductive circuit, 5, a metal foil, 7, an elastomer film, 8, a lead and 9, an elastomer solution.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a preparation method of a flexible stretchable conductive circuit, which is implemented according to the following steps as shown in figure 1:
step 1, preparing precursor solution 2 containing conductive enhanced phase
Adding the raw material A and a dispersing agent into deionized water, heating until the raw material A and the dispersing agent are completely dissolved, and filtering to obtain a precursor solution 2 containing a conductive enhanced phase for later use;
the dispersant is polyvinylpyrrolidone; the raw material A is ascorbic acid, citric acid or oxalic acid; the mass volume concentration of the conductive reinforcing phase-containing precursor solution 2 is 21-48% by weight;
Dissolving the raw material B in deionized water, stirring uniformly to fully dissolve the raw material B, and filtering to obtain a metal salt solution 3 for later use;
wherein the raw material B is silver nitrate, silver chloride or copper nitrate, the mass volume concentration of the metal salt solution 3 is 40-80% by weight;
the elastomer solution 9 is polydimethylsilane or poly adipic acid/butylene terephthalate; the curing temperature of the polydimethylsilane is 80 ℃, and the curing time is 40-60 min; or the curing temperature of the poly (butylene adipate)/terephthalate is 23 ℃, and the curing time is 3 h-6 min;
step 4, soaking the semi-permeable membrane 1 by adopting a precursor solution 2 containing a conductive enhanced phase, flatly paving the semi-permeable membrane on the surface of the metal foil 5, and removing bubbles to completely attach the semi-permeable membrane; and the metal salt solution 3 is filled into a test tube of a piezoelectric type microdroplet on-demand spraying system;
wherein the semipermeable membrane 1 is cellophane or polylactic acid/cellophane composite membrane with thickness of 25g/m 2 、30g/m 2 、40g/m 2 Or 45g/m 2 (ii) a The metal foil 5 is a copper foil, a zinc foil or a tin foil;
the controller controls the two-dimensional motion control platform to move relative to the test tube according to a set path, simultaneously controls the metal salt solution 3 in the test tube to be sprayed out and deposited on the semipermeable membrane 1, forms a conductive circuit 4 on the semipermeable membrane 1 after repeated printing and deposition for 3-5 times, and takes down the metal foil 5;
the motion parameters of the two-dimensional motion control platform are as follows: the pulse amplitude is 200V, the pulse width is 10 mus, the pulse frequency is 1Hz, and the dot pitch is 0.075mm;
step 6, washing the printed and deposited semi-permeable membrane 1 for 2-4 times by using deionized water, and separating the conductive circuit 4 from the semi-permeable membrane 1; moving the conductive circuit 4 to the elastomer film 7, and placing the elastomer film in a constant-temperature heating furnace for heating treatment to obtain a film-based conductive circuit;
wherein the temperature of the heating treatment is 80-100 ℃, and the time is 10-15 min;
step 7, bonding the film-based conductive circuit and the lead 8 by conductive silver paste, leading out, and then placing in a constant-temperature heating furnace for heating treatment;
wherein the temperature of the heating treatment is 100-110 ℃, and the time is 20-30 min;
the elastomer solution 9 is polydimethylsilane or poly adipic acid/butylene terephthalate; the curing temperature of the polydimethylsilane is 80 ℃, and the curing time is 40-60 min; or the curing temperature of the poly (butylene adipate/terephthalate) is 23 ℃, and the curing time is 3 h-6 min.
Example 1
The invention relates to a preparation method of a flexible stretchable conductive circuit, which is implemented according to the following steps:
step 1, preparing precursor solution 2 containing conductive enhanced phase
Adding the raw material A and a dispersing agent into deionized water, heating until the raw material A and the dispersing agent are completely dissolved, and filtering to obtain a precursor solution 2 containing a conductive enhanced phase for later use;
the dispersant is polyvinylpyrrolidone; the raw material A is citric acid; the mass-volume concentration of the conductive reinforcing phase-containing precursor solution 2 was 21% w/v;
Dissolving the raw material B in deionized water, stirring uniformly to fully dissolve the raw material B, and filtering to obtain a metal salt solution 3 for later use;
wherein the raw material B is silver chloride, the mass volume concentration of the metal salt solution 3 is 50 percent;
elastomer solution 9 is poly (butylene adipate/terephthalate); the curing temperature of the poly (butylene adipate/terephthalate) is 23 ℃, and the curing time is 5 hours;
step 4, soaking the semi-permeable membrane 1 by adopting a precursor solution 2 containing a conductive enhanced phase, flatly paving the semi-permeable membrane on the surface of the metal foil 5, and removing bubbles to completely attach the semi-permeable membrane; and the metal salt solution 3 is filled into a test tube of a piezoelectric type microdroplet on-demand spraying system;
wherein the semipermeable membrane 1 is cellophane with a thickness of 25g/m 2 (ii) a The metal foil 5 is a tin foil;
the controller controls the two-dimensional motion control platform to move relative to the test tube according to a set path, simultaneously controls the metal salt solution 3 in the test tube to be sprayed out and deposited on the semipermeable membrane 1, forms a conductive circuit 4 on the semipermeable membrane 1 after repeated printing and deposition for 3 times, and takes down the metal foil 5;
the motion parameters of the two-dimensional motion control platform are as follows: the pulse amplitude is 200V, the pulse width is 10 mus, the pulse frequency is 1Hz, and the dot pitch is 0.075mm;
step 6, washing the printed and deposited semi-permeable membrane 1 for 2 times by using deionized water, and separating the conductive circuit 4 from the semi-permeable membrane 1; moving the conductive circuit 4 to the elastomer film 7, and placing the elastomer film in a constant-temperature heating furnace for heating treatment to obtain a film-based conductive circuit;
wherein the heating treatment temperature is 80 deg.C, and the time is 13min;
step 7, bonding the film base conductive circuit and the lead 8 by conductive silver paste, leading out, and then placing in a constant temperature heating furnace for heating treatment;
wherein the temperature of the heating treatment is 105 ℃, and the time is 22min;
elastomer solution 9 is poly (butylene adipate/terephthalate); the curing temperature of the poly (butylene adipate/terephthalate) was 23 ℃ and the curing time was 5 hours.
Example 2
The invention relates to a preparation method of a flexible stretchable conductive circuit, which is implemented by the following steps:
step 1, preparing a precursor solution 2 containing a conductive reinforcing phase
Adding the raw material A and a dispersing agent into deionized water, heating until the raw material A and the dispersing agent are completely dissolved, and filtering to obtain a precursor solution 2 containing a conductive enhanced phase for later use;
the dispersant is polyvinylpyrrolidone; the raw material A is oxalic acid; the mass-volume concentration of the conductive reinforcing phase-containing precursor solution 2 was 39% w/v;
Dissolving the raw material B in deionized water, stirring uniformly to fully dissolve the raw material B, and filtering to obtain a metal salt solution 3 for later use;
wherein the raw material B is silver chloride, the mass volume concentration of the metal salt solution 3 is 40 percent;
elastomer solution 9 is poly (butylene adipate/terephthalate); the curing temperature of the poly (butylene adipate/terephthalate) is 23 ℃, and the curing time is 6 hours;
step 4, soaking the semi-permeable membrane 1 by adopting a precursor solution 2 containing a conductive enhanced phase, flatly paving the semi-permeable membrane on the surface of the metal foil 5, and removing bubbles to completely attach the semi-permeable membrane; and the metal salt solution 3 is filled into a test tube of a piezoelectric type microdroplet on-demand spraying system;
wherein the semipermeable membrane 1 is a polylactic acid/cellophane composite membrane with a thickness of 45g/m or less 2 (ii) a The metal foil 5 is a zinc foil;
the controller controls the two-dimensional motion control platform to move relative to the test tube according to a set path, controls the metal salt solution 3 in the test tube to be sprayed out and deposited on the semipermeable membrane 1, forms a conductive circuit 4 on the semipermeable membrane 1 after repeated printing and deposition for 4 times, and takes down the metal foil 5;
the motion parameters of the two-dimensional motion control platform are as follows: the pulse amplitude is 200V, the pulse width is 10 mus, the pulse frequency is 1Hz, and the dot pitch is 0.075mm;
step 6, washing the printed and deposited semi-permeable membrane 1 for 2 times by using deionized water, and separating the conductive circuit 4 from the semi-permeable membrane 1; moving the conducting circuit 4 to the elastomer film 7, and placing the elastomer film in a constant-temperature heating furnace for heating treatment to obtain a film-based conducting circuit;
wherein the heating treatment temperature is 85 deg.C, and the time is 15min;
step 7, bonding the film base conductive circuit and the lead 8 by conductive silver paste, leading out, and then placing in a constant temperature heating furnace for heating treatment;
wherein the temperature of the heating treatment is 105 ℃, and the time is 27min;
elastomer solution 9 is poly (butylene adipate/terephthalate); the curing temperature of the poly (butylene adipate/terephthalate) was 23 ℃ and the curing time was 6 hours.
Example 3
The invention relates to a preparation method of a flexible stretchable conductive circuit, which is implemented by the following steps:
step 1, preparing precursor solution 2 containing conductive enhanced phase
Adding the raw material A and a dispersing agent into deionized water, heating until the raw material A and the dispersing agent are completely dissolved, and filtering to obtain a precursor solution 2 containing a conductive enhanced phase for later use;
the dispersant is polyvinylpyrrolidone; the raw material A is oxalic acid; the mass-volume concentration of the conductive reinforcing phase-containing precursor solution 2 was 33% w/v;
Dissolving the raw material B in deionized water, stirring uniformly to fully dissolve the raw material B, and filtering to obtain a metal salt solution 3 for later use;
wherein the raw material B is copper nitrate, the mass volume concentration of the metal salt solution 3 is 70%;
elastomer solution 9 is polydimethylsiloxane; the curing temperature of the polydimethylsilane is 80 ℃, and the curing time is 60min;
step 4, soaking the semi-permeable membrane 1 by adopting a precursor solution 2 containing a conductive enhanced phase, flatly paving the semi-permeable membrane on the surface of the metal foil 5, and removing bubbles to completely attach the semi-permeable membrane; and the metal salt solution 3 is filled into a test tube of a piezoelectric type microdroplet on-demand spraying system;
wherein the semipermeable membrane 1 is cellophane with a thickness of 40g/m 2 (ii) a The metal foil 5 is a tin foil;
the controller controls the two-dimensional motion control platform to move relative to the test tube according to a set path, controls the metal salt solution 3 in the test tube to be sprayed out and deposited on the semipermeable membrane 1, forms a conductive circuit 4 on the semipermeable membrane 1 after repeated printing and deposition for 4 times, and takes down the metal foil 5;
the motion parameters of the two-dimensional motion control platform are as follows: the pulse amplitude is 200V, the pulse width is 10 mus, the pulse frequency is 1Hz, and the dot pitch is 0.075mm;
step 6, washing the printed and deposited semipermeable membrane 1 for 3 times by using deionized water, and separating the conductive circuit 4 from the semipermeable membrane 1; moving the conductive circuit 4 to the elastomer film 7, and placing the elastomer film in a constant-temperature heating furnace for heating treatment to obtain a film-based conductive circuit;
wherein the heating treatment temperature is 95 deg.C, and the time is 10min;
step 7, bonding the film-based conductive circuit and the lead 8 by conductive silver paste, leading out, and then placing in a constant-temperature heating furnace for heating treatment;
wherein the heating treatment temperature is 108 deg.C, and the time is 30min;
elastomer solution 9 is polydimethylsiloxane; the curing temperature of the polydimethylsilane is 80 ℃, and the curing time is 60min.
Example 4
The invention relates to a preparation method of a flexible stretchable conductive circuit, which is implemented by the following steps:
step 1, preparing a precursor solution 2 containing a conductive reinforcing phase
Adding the raw material A and a dispersing agent into deionized water, heating until the raw material A and the dispersing agent are completely dissolved, and filtering to obtain a precursor solution 2 containing a conductive enhanced phase for later use;
the dispersant is polyvinylpyrrolidone; the raw material A is ascorbic acid; the mass volume concentration of the conductivity enhancing phase-containing precursor solution 2 was 32%;
Dissolving the raw material B in deionized water, stirring uniformly to fully dissolve the raw material B, and filtering to obtain a metal salt solution 3 for later use;
wherein the raw material B is silver nitrate, the mass volume concentration of the metal salt solution 3 is 80% w/v;
elastomer solution 9 is polydimethylsiloxane; the curing temperature of the polydimethylsilane is 80 ℃, and the curing time is 50min;
step 4, soaking the semi-permeable membrane 1 by adopting a precursor solution 2 containing a conductive enhanced phase, flatly paving the semi-permeable membrane on the surface of the metal foil 5, and removing bubbles to completely attach the semi-permeable membrane; and the metal salt solution 3 is filled into a test tube of a piezoelectric type microdroplet on-demand spraying system;
wherein the semipermeable membrane 1 is made of cellophane and has a thickness of 30g/m 2 (ii) a The metal foil 5 is a copper foil;
the controller controls the two-dimensional motion control platform to move relative to the test tube according to a set path, simultaneously controls the metal salt solution 3 in the test tube to be sprayed out and deposited on the semipermeable membrane 1, forms a conductive circuit 4 on the semipermeable membrane 1 after repeated printing and deposition for 5 times, and takes down the metal foil 5;
the motion parameters of the two-dimensional motion control platform are as follows: the pulse amplitude is 200V, the pulse width is 10 mus, the pulse frequency is 1Hz, and the dot pitch is 0.075mm;
step 6, washing the printed and deposited semipermeable membrane 1 for 3 times by using deionized water, and separating the conductive circuit 4 from the semipermeable membrane 1; moving the conducting circuit 4 to the elastomer film 7, and placing the elastomer film in a constant-temperature heating furnace for heating treatment to obtain a film-based conducting circuit;
wherein the heating treatment temperature is 90 deg.C, and the time is 15min;
step 7, bonding the film base conductive circuit and the lead 8 by conductive silver paste, leading out, and then placing in a constant temperature heating furnace for heating treatment;
wherein the heating treatment temperature is 100 deg.C, and the time is 25min;
elastomer solution 9 is polydimethylsiloxane; the curing temperature of the polydimethylsilane is 80 ℃, and the curing time is 50min.
Example 5
The invention relates to a preparation method of a flexible stretchable conductive circuit, which is implemented according to the following steps:
step 1, preparing a precursor solution 2 containing a conductive reinforcing phase
Adding the raw material A and a dispersing agent into deionized water, heating until the raw material A and the dispersing agent are completely dissolved, and filtering to obtain a precursor solution 2 containing a conductive enhanced phase for later use;
the dispersant is polyvinylpyrrolidone; the raw material A is ascorbic acid; the mass-volume concentration of the conductive reinforcing phase-containing precursor solution 2 was 48% w/v;
Dissolving the raw material B in deionized water, stirring uniformly to fully dissolve the raw material B, and filtering to obtain a metal salt solution 3 for later use;
wherein the raw material B is silver nitrate, the mass volume concentration of the metal salt solution 3 is 60% w/v;
elastomer solution 9 is poly (butylene adipate/terephthalate); the curing temperature of the poly (butylene adipate/terephthalate) is 23 ℃, and the curing time is 3 hours;
step 4, soaking the semi-permeable membrane 1 by adopting a precursor solution 2 containing a conductive enhanced phase, flatly paving the semi-permeable membrane on the surface of the metal foil 5, and removing bubbles to completely attach the semi-permeable membrane; filling the metal salt solution 3 into a test tube of a piezoelectric type droplet on-demand jet system;
wherein the semipermeable membrane 1 is a polylactic acid/cellophane composite membrane with a thickness of 30g/m 2 (ii) a The metal foil 5 is a copper foil;
the controller controls the two-dimensional motion control platform to move relative to the test tube according to a set path, controls the metal salt solution 3 in the test tube to be sprayed out and deposited on the semipermeable membrane 1, repeatedly prints and deposits for 3-5 times, forms a conductive circuit 4 on the semipermeable membrane 1, and takes down the metal foil 5;
the motion parameters of the two-dimensional motion control platform are as follows: the pulse amplitude is 200V, the pulse width is 10 mus, the pulse frequency is 1Hz, and the dot pitch is 0.075mm;
step 6, washing the printed and deposited semi-permeable membrane 1 for 4 times by using deionized water, and separating the conductive circuit 4 from the semi-permeable membrane 1; moving the conducting circuit 4 to the elastomer film 7, and placing the elastomer film in a constant-temperature heating furnace for heating treatment to obtain a film-based conducting circuit;
wherein the heating treatment temperature is 100 deg.C, and the time is 13min;
step 7, bonding the film base conductive circuit and the lead 8 by conductive silver paste, leading out, and then placing in a constant temperature heating furnace for heating treatment;
wherein the heating treatment temperature is 110 deg.C, and the time is 20min;
elastomer solution 9 is poly (butylene adipate/terephthalate); the curing temperature of the poly (butylene adipate/terephthalate) was 23 ℃ and the curing time was 3 hours.
In summary, embodiment 4 is the best embodiment of the present invention. The surface of the cellophane is smooth, has no capillary holes and is waterproof, the cellophane with the original pattern layer is soaked by adopting a precursor ascorbic acid solution added with a conductive enhanced phase polyvinylpyrrolidone (PVP), the cellophane is placed on a copper foil, then a silver nitrate solution is sprayed and printed on the cellophane, and a conductive circuit 4 deposited by silver simple substances is recovered on the surface of the cellophane through oxidation-reduction reaction. Because the contact angle of the surface of the cellophane is large, silver particles generated by redox reaction can not be firmly attached to the surface of the cellophane, the conducting circuit 4 deposited on the surface of the cellophane is washed by deionized water so as to be completely separated from the cellophane, the conducting circuit 4 obtained by separation is transferred to a prepared PDMS flexible substrate in a picking mode, and finally the PDMS solution is used for packaging.
The dispersing agent PVP is added into the precursor solution, the cohesiveness among silver particles in the conductive circuit deposited on the surface of the cellophane is increased, and the mechanical property of the conductive circuit 4 is improved, so that the loss of the silver particles in the transfer printing process is reduced, and the conductivity of the flexible and stretchable conductive circuit is improved.
The flexible stretchable conductive circuit prepared in example 4 was subjected to 0-10% -20% -30% -0 cycle stretching, and the stretching apparatus used in the test was a digital display push-pull dynamometer. As shown in fig. 2, the resistance values of the conductive lines during the 1 st, 10 th and 20 th stretching processes are plotted against the stretching ratios, and the data are shown in table 1;
TABLE 1 resistance and elongation data for flexible stretchable conductive traces
As can be seen from fig. 2, the initial resistance of the conductive line is 18.5 Ω, and the resistance gradually increases as the stretching ratio increases, and the change trend of the resistance at each stretching cycle is substantially the same. After the 20 th stretching by 30%, the resistance increment of the conductive circuit relative to the initial value is only about 80%, and good flexibility and conductive characteristics are displayed.
According to the invention, the conductive circuit 4 is stripped and printed without processing a convex structure on the flexible substrate or using external action of laser, plasma and the like; the preparation method of the flexible stretchable conductive circuit is good in universality, low in cost and simple in process. The prepared conductive circuit 4 has high flexibility, transparency and conductivity with good stability, and can be applied to the touch sensing of the surface of a three-dimensional carrier or the movable joint part of a robot.
Claims (7)
1. A preparation method of a flexible stretchable conductive circuit is characterized by comprising the following steps:
step 1, preparing precursor solution (2) containing conductive enhanced phase
Adding the raw material A and a dispersing agent into deionized water, heating until the raw material A and the dispersing agent are completely dissolved, and filtering to obtain a precursor solution (2) containing a conductive enhanced phase for later use;
step 2, preparation of Metal salt solution (3)
Dissolving the raw material B in deionized water, stirring uniformly to fully dissolve the raw material B, and filtering to obtain a metal salt solution (3) for later use;
step 3, pouring the elastomer solution (9) into a mold, and then placing the mold at a proper temperature for curing to obtain an elastomer film (7) for later use;
step 4, soaking the semi-permeable membrane (1) by adopting a precursor solution (2) containing a conductive enhanced phase, flatly paving the semi-permeable membrane on the surface of the metal foil (5), and removing bubbles to completely attach the semi-permeable membrane; and the metal salt solution (3) is filled into a test tube of a piezoelectric type microdroplet on-demand jet system;
step 5, importing a pre-designed conducting circuit graph into a computer, generating a two-dimensional motion path code, and setting motion parameters of a two-dimensional motion control platform, wherein the piezoelectric type micro-droplet on-demand jetting system and the two-dimensional motion control platform are connected with a controller;
the controller controls the two-dimensional motion control platform to move relative to the test tube according to a set path, simultaneously controls the metal salt solution (3) in the test tube to be sprayed out and deposited on the semipermeable membrane (1), forms a conductive circuit (4) on the semipermeable membrane (1) after repeated printing and deposition for 3-5 times, and takes down the metal foil (5);
step 6, washing the printed and deposited semi-permeable membrane (1) for 2-4 times by using deionized water, and separating the conductive circuit (4) from the semi-permeable membrane (1); moving the conducting circuit (4) to an elastomer film (7), and placing the elastomer film in a constant-temperature heating furnace for heating treatment to obtain a film-based conducting circuit;
step 7, bonding the film-based conductive circuit and a lead (8) by using conductive silver paste, leading out, and then placing in a constant-temperature heating furnace for heating treatment;
step 8, pouring the elastomer solution (9) on the surface of the film-based conductive circuit, and curing at a proper temperature to obtain a packaged flexible stretchable conductive circuit;
the dispersing agent is polyvinylpyrrolidone; the raw material A is ascorbic acid, citric acid or oxalic acid; the mass volume concentration of the conductive reinforcing phase-containing precursor solution (2) is 21% w/v-48%;
the raw material B is silver nitrate, silver chloride or copper nitrate, and the mass volume concentration of the metal salt solution (3) is 40% by weight w/v-80% by weight.
2. A method of making a flexible stretchable conductive trace according to claim 1, wherein the elastomer solution (9) is polydimethylsilane or polybutylene adipate/terephthalate.
3. The method for preparing a flexible and stretchable conductive circuit according to claim 2, wherein in the steps 3 and 8, the curing temperature of the polydimethylsilane is 80 ℃ and the curing time is 40-60 min; or the curing temperature of the poly (butylene adipate/terephthalate) is 23 ℃, and the curing time is 3-6 h.
4. The method for preparing a flexible and stretchable conductive circuit according to claim 1, wherein the semi-permeable membrane (1) is a cellophane or a polylactic acid/cellophane composite membrane with a thickness of 25g/m 2 、30g/m 2 、40g/m 2 Or 45g/m 2 (ii) a The metal foil (5) is a copper foil, a zinc foil or a tin foil.
5. The method of claim 1, wherein the two-dimensional motion controls a motion parameter of the platform: the pulse amplitude is 200V, the pulse width is 10 mus, the pulse frequency is 1Hz, and the dot pitch is 0.075mm.
6. The method for preparing a flexible and stretchable conductive circuit according to claim 1, wherein in the step 6, the temperature of the heating treatment is 80 ℃ to 100 ℃ for 10min to 15min.
7. The method for preparing a flexible and stretchable conductive circuit according to claim 1, wherein in the step 7, the temperature of the heating treatment is 100 ℃ to 110 ℃ for 20min to 30min.
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