CN113151813A - Conductive film repairing method - Google Patents
Conductive film repairing method Download PDFInfo
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- CN113151813A CN113151813A CN202010015177.4A CN202010015177A CN113151813A CN 113151813 A CN113151813 A CN 113151813A CN 202010015177 A CN202010015177 A CN 202010015177A CN 113151813 A CN113151813 A CN 113151813A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
- C23C18/405—Formaldehyde
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/28—Sensitising or activating
- C23C18/285—Sensitising or activating with tin based compound or composition
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
A conductive film repairing method comprises the following steps: providing a conductive film to be repaired, wherein the conductive film comprises a base film, a structural layer and a conductive grid, the structural layer is positioned on the base film, the structural layer is provided with a pattern groove, and the conductive grid is formed by filling a metal material in the pattern groove; sensitizing the conductive film; placing the sensitized conductive film in chemical copper plating solution; adding reducing liquid under the condition of stirring; and standing, and forming a deposited copper layer on the surface of the conductive grid, wherein the deposited copper layer also fills gaps with poor circuit in the conductive grid. The surface of the conductive film is sensitized and chemically plated with copper, silver or gold in the conductive grid plays a role in catalysis in the process, the reduction reaction rate near the conductive grid is high, the bad open circuit of the conductive grid can be repaired in batches, the success rate is high, the efficiency is high, and automatic repair can be realized.
Description
Technical Field
The invention relates to the technical field of conductive films, in particular to a conductive film repairing method.
Background
The transparent conductive film has high transmittance and good conductivity, and is widely applied to the fields of touch screens, electromagnetic shielding, photovoltaic devices and the like, along with the development of scientific technology, more and more electronic devices develop towards flexibility and light weight, and the demand on the transparent conductive film is increasing day by day. Among them, ITO (Indium tin oxide) conductive films and silver nanowire conductive films are currently widely used transparent conductive films.
In order to increase the flexibility of the conductive film and reduce the cost, the UV imprinting method is increasingly used in the manufacture of the transparent conductive film. In the UV imprinting method, a pattern groove is printed on a UV layer by adopting a mould through a roll-to-roll imprinting process, then conductive ink is filled in the pattern groove, and a conductive grid is formed by sintering, wherein the conductive ink usually adopts copper nano slurry or silver nano slurry.
However, in the UV imprinting method, the conductive ink filling is not uniform or the conductive ink is not uniformly filled or the conductive ink is sintered to cause micro-deformation of the base film, which may cause one or more open circuits in the conductive mesh. Such open defects account for a large percentage of production defects, and therefore a method for successfully repairing the open conductive film defects is highly desired.
Disclosure of Invention
The invention aims to provide a method for repairing a conductive film, which is used for repairing the poor disconnection of the conductive film, has high reliability and efficiency and can realize automatic repair.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a conductive film repairing method comprises the following steps:
providing a conductive film to be repaired, wherein the conductive film comprises a base film, a structural layer and a conductive grid, the structural layer is positioned on the base film, the structural layer is provided with a pattern groove, and the conductive grid is formed by filling a metal material in the pattern groove;
sensitizing the conductive film;
placing the sensitized conductive film in chemical copper plating solution;
adding reducing liquid under the condition of stirring;
and standing, and forming a deposited copper layer on the surface of the conductive grid, wherein the deposited copper layer also fills gaps with poor circuit in the conductive grid.
Preferably, the step of sensitizing the conductive film is to spray a sensitizing solution to one side of the conductive film, where the conductive grid is arranged, and clean the conductive film with pure water after spraying for 3-5 min; the sensitizing solution comprises stannous chloride with the mass fraction of 1% -5% and hydrogen chloride with the mass fraction of 4% -8%, and the PH value of the chemical copper plating solution is 10-12.
Preferably, the electroless copper plating solution includes a main salt, a complexing agent, and a PH adjuster.
Preferably, the main salt is selected from one or more of copper sulfate, copper chloride and copper nitrate; the complexing agent is selected from one or more of potassium sodium tartrate, sodium citrate, EDTA disodium and triethanolamine; the pH regulator is selected from one or more of sodium hydroxide or potassium hydroxide.
Preferably, the chemical copper plating solution comprises 1.2-2% by mass of copper sulfate and 1.0-1.8% by mass of potassium sodium tartrate.
Preferably, the reducing solution comprises one or more of formaldehyde, hypophosphite and dimethylamine borane.
Preferably, the step of adding the reducing solution under the stirring condition is to stir the chemical copper plating solution, add a formaldehyde solution, and mix to obtain a mixed chemical solution with the formaldehyde mass fraction of 1.0-1.8%.
Preferably, the metal material is selected from one or more of silver, gold, silver alloy, gold alloy.
Preferably, the standing step is performed for 10-120 min at 30-60 ℃.
Preferably, in the standing step, the thickness of the deposited copper layer is controlled to be 1-3 μm.
Compared with the prior art, the invention has the advantages and beneficial effects that:
the invention provides a conductive film repairing method, which is characterized in that the surface of a conductive film is sensitized and chemically plated with copper, silver or gold in a conductive grid plays a role in catalysis in the process, the reduction reaction rate near the conductive grid is higher, copper generated by final reduction is deposited on the surface of the conductive grid, gaps with poor circuit breaking are filled, the poor circuit breaking of the conductive grid can be repaired in batches, the success rate is high, the efficiency is high, the process is simple and reliable, automatic repairing can be realized, the resistivity uniformity of the conductive film after repairing is excellent, and the reliability of repairing is high.
Drawings
Fig. 1 is a flowchart illustrating steps of a method for repairing a conductive film according to an embodiment of the present invention;
fig. 2 is a process flow diagram of a method for repairing a conductive film according to an embodiment of the invention.
Detailed Description
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Referring to fig. 1 and fig. 2, fig. 1 is a flow chart illustrating steps of a method for repairing a conductive film according to an embodiment of the present invention, and fig. 2 is a process flow chart illustrating the method for repairing the conductive film.
The method for repairing a conductive film provided by the embodiment comprises the following steps:
s1: providing a conductive film to be repaired, and pretreating the conductive film; the conductive film comprises a base film 11, a structural layer 12 and a conductive grid 13, wherein the structural layer 12 is positioned on the base film 11 and is provided with a pattern groove, the conductive grid 13 is made by filling a metal material in the pattern groove, and one or more open circuits exist in the conductive grid 13 in the conductive film to be repaired;
s2: sensitizing the conductive film;
s3: placing the sensitized conductive film in chemical copper plating solution, and adding reducing solution under the stirring condition;
s4: standing, forming a deposited copper layer 31 on the surface of the conductive grid 13, wherein the deposited copper layer 31 is also filled in the gap with poor circuit in the conductive grid 13;
s5: and taking out the repaired conductive film, washing the conductive film for 60s by pure water, and drying the conductive film in a drying mode including but not limited to air drying or airing.
Further, in the conductive film provided in step S1, the base film 11 includes, for example, a PET material, the structural layer 12 is formed by a UV light curing layer or a thermosetting layer, and the structural layer 12 is formed with a pattern groove on a side away from the substrate by mold stamping or other patterning. The cross section of the pattern groove is, for example, rectangular, trapezoidal or trapezoid-like, the conductive grid 13 is a continuous grid arranged uniformly or non-uniformly, and the shape of the grid is, for example, one of square, rectangle, diamond, pentagon, hexagon, random grid or a combination of at least two of the above. The metal material is selected from one or more of silver, gold, silver alloy and gold alloy, and specifically, the conductive grid 13 is formed by filling conductive ink, such as silver nano-paste or gold nano-paste or silver alloy nano-paste or gold alloy nano-paste, in the pattern groove and then sintering the pattern groove. Preferably, the metal material is silver. The depth of the pattern groove is 3-8 mu m, the width of the pattern groove is 3-8 mu m, and the thickness of the conductive grid 13 is 2-4 mu m.
The step of pretreating the conductive film specifically comprises: the conductive film is laid in a tank 20, the side provided with the structural layer 12 and the conductive grid 13 faces upwards, and the pure water is used for washing for 30 s.
In step S2, the sensitizing treatment of the conductive film is specifically performed by spraying a sensitizing solution on the side of the conductive film where the conductive grid 13 is provided, and cleaning the conductive film with pure water after spraying for 3-5 min; the sensitizing solution comprises stannous chloride with the mass fraction of 1-5% and hydrogen chloride with the mass fraction of 4-8%, so that the reducing capacity of the surface of the conductive film is enhanced, and more preferably, the mass fraction of the stannous chloride is 1-3%. In particular, stannous produces a sparingly soluble product Sn (OH) upon washing with water due to hydrolysis1～5Cl0～5The sparingly soluble product is deposited by condensation, so that a reducing liquid film 14 having a reducing action is formed on the surface of the conductive film. The mass fraction of stannous chloride is lower than 1 percent and/or the pH value of the sensitizing solution is lower, so that the deposition amount of slightly soluble products is insufficient, the density of metal crystal nuclei generated by subsequent reduction is lower, and the copper deposition rate is further causedToo low. The mass fraction of stannous chloride higher than 5% and/or the high PH of the sensitizing solution may cause excessive stannous chloride to be adsorbed on the surface of the conductive mesh 13, which may reduce the bonding force of the plating layer and may not be favorable for controlling the thickness of the deposited copper layer 31.
In step S3, the electroless copper plating solution includes a main salt, a complexing agent, and a PH adjuster, wherein the main salt is one or more selected from copper sulfate, copper chloride, and copper nitrate; the complexing agent is one or more selected from potassium sodium tartrate, sodium citrate, EDTA disodium and triethanolamine; the PH regulator is selected from one or more of sodium hydroxide and potassium hydroxide, and is used for regulating the PH value of the chemical copper plating solution to 10-12. Preferably, the electroless copper plating solution comprises 1.2-2% by mass of copper sulfate, 1.0-1.8% by mass of potassium sodium tartrate and 1.2-2% by mass of sodium hydroxide. More preferably, the electroless copper plating solution comprises 1.2 to 1.4 mass% of copper sulfate, 1.0 to 1.2 mass% of sodium potassium tartrate and 1.2 to 1.4 mass% of sodium hydroxide. The mass fraction of copper sulfate is less than 1.2% and/or the mass fraction of potassium sodium tartrate is less than 1.0%, which may result in slow reduction reaction rate, insufficient thickness of the deposited copper layer 31, unreliable repair of broken wire, or long repair period, which is not favorable for automatic repair. A copper sulfate mass fraction higher than 2% and/or a potassium sodium tartrate mass fraction higher than 1.8% may result in an excessively fast reduction reaction rate, insufficient density of the deposited copper layer 31, influence on uniformity of conductivity, and be disadvantageous in controlling the thickness of the deposited copper layer 31.
In step S3, the reducing solution is a solution containing a reducing agent, where the reducing agent includes one or more of formaldehyde, hypophosphite, and dimethylamine borane, for example: the step of adding the reducing solution under the stirring condition is specifically to stir the chemical copper plating solution, add the formaldehyde solution and mix to prepare a mixed chemical solution 30 with the formaldehyde mass fraction of 1.0-1.8%, and immerse the conductive film to be repaired in the mixed chemical solution 30 in the tank body 20. The formaldehyde solution used for preparing the mixed chemical solution 30 is, for example, a formaldehyde solution with a mass fraction of 37-42%. More preferably, the mass fraction of formaldehyde is 1% to 1.2%. The mass fraction of formaldehyde less than 1% leads to a slow reduction reaction rate, which results in insufficient thickness of the deposited copper layer 31, unreliable repair of poor wire breakage, or long repair cycle, which is not conducive to automated repair. A mass fraction of formaldehyde higher than 1.8% may result in too fast a reduction reaction, insufficient density of the deposited copper layer 31, influence on uniformity of conductivity, and be disadvantageous in controlling the thickness of the deposited copper layer 31.
In step S4, the standing step is performed under the conditions of standing at 30-60 ℃ for 10-120 min and controlling the total thickness of the conductive grid 13 and the deposited copper layer 31 to be less than the depth of the pattern groove, and more preferably, the standing step is performed at 30-40 ℃ for 20-60 min and controlling the thickness of the deposited copper layer 31 to be 1-3 μm. The thickness of the deposited copper layer 31 can be adjusted by adjusting the concentrations of the main salt, the complexing agent, and the reducing agent in the mixed chemical solution 30, the temperature of the mixed chemical solution 30, and the standing time. During the copper plating process, the silver or gold in the conductive mesh 13 acts as a catalyst, and the cuprous oxide generated by the incomplete reaction proceeds from the catalytic reduction reaction, and preferably, the metal material forming the conductive mesh 13 includes silver, which has an excellent catalytic ability for the reduction reaction. The reduction reaction rate near the conductive grid 13 is far higher than that of the surface of the structural layer 12, and finally, copper generated by reduction is deposited on the surface of the conductive grid 13, and gaps with poor circuit breaking are filled, so that the poor circuit breaking is repaired. Experiments prove that when the thickness of the deposited copper layer 31 on the surface of the conductive grid 13 reaches 8 microns, no copper plating layer still appears on the surface of the structural layer 12.
Example 1:
the mixed chemical solution 30 of the present embodiment is composed of, by mass percent: 1.2 percent of copper sulfate, 1.0 percent of sodium potassium tartrate, 1.2 percent of sodium hydroxide and 1.0 percent of formaldehyde, controlling the temperature of the mixed chemical solution 30 to be 30-35 ℃, and standing for 1 hour.
Example 2:
the mixed chemical solution 30 of the present embodiment is composed of, by mass percent: 1.2 percent of copper sulfate, 1.0 percent of sodium potassium tartrate, 1.2 percent of sodium hydroxide and 1.0 percent of formaldehyde, controlling the temperature of the mixed chemical solution 30 to be 35-40 ℃, and standing for 1 hour.
Example 3:
the mixed chemical solution 30 of the present embodiment is composed of, by mass percent: 1.2 percent of copper sulfate, 1.0 percent of sodium potassium tartrate, 1.2 percent of sodium hydroxide and 1.3 percent of formaldehyde, controlling the temperature of the mixed chemical solution 30 to be 30-35 ℃, and standing for 1 hour.
Example 4:
the mixed chemical solution 30 of the present embodiment is composed of, by mass percent: 1.5 percent of copper sulfate, 1.2 percent of sodium potassium tartrate, 1.5 percent of sodium hydroxide and 1.3 percent of formaldehyde, controlling the temperature of the mixed chemical solution 30 to be 35-40 ℃, and standing for 1 hour.
Example 5:
the mixed chemical solution 30 of the present embodiment is composed of, by mass percent: 1.5 percent of copper sulfate, 1.2 percent of sodium potassium tartrate, 1.5 percent of sodium hydroxide and 1.3 percent of formaldehyde, controlling the temperature of the mixed chemical solution 30 to be 35-40 ℃, and standing for 30 min.
Example 6:
the mixed chemical solution 30 of the present embodiment is composed of, by mass percent: 1.5 percent of copper sulfate, 1.2 percent of sodium potassium tartrate, 1.5 percent of sodium hydroxide and 1.5 percent of formaldehyde, controlling the temperature of the mixed chemical solution 30 to be 35-40 ℃, and standing for 30 min.
Example 7:
the mixed chemical solution 30 of the present embodiment is composed of, by mass percent: 1.8 percent of copper sulfate, 1.4 percent of sodium potassium tartrate, 1.8 percent of sodium hydroxide and 1.5 percent of formaldehyde, controlling the temperature of the mixed chemical solution 30 to be 55-60 ℃, and standing for 1 hour.
Example 8:
the mixed chemical solution 30 of the present embodiment is composed of, by mass percent: 2% of copper sulfate, 1.8% of sodium potassium tartrate, 2% of sodium hydroxide and 1.8% of formaldehyde, controlling the temperature of the mixed chemical solution 30 to be 55-60 ℃, and standing for 1 hour.
The conditions, copper deposition rates, and thickness of the deposited copper layer 31 for each of examples 1-8 are shown in Table 1.
TABLE 1 implementation conditions, copper deposition rate and thickness of the deposited copper layer for each example
The invention provides a conductive film repairing method, which is characterized in that the surface of a conductive film is sensitized and chemically plated with copper, silver or gold in a conductive grid 13 plays a role in catalysis in the process, the vicinity of the conductive grid 13 has higher reduction reaction rate, copper generated by final reduction is deposited on the surface of the conductive grid 13, gaps with poor circuit breaking are filled, the poor circuit breaking of the conductive grid 13 can be repaired in batches, the success rate is high, the efficiency is high, the process is simple and reliable, automatic repairing can be realized, the resistivity uniformity of the conductive film after repairing is excellent, and the reliability of repairing is high.
In the drawings, the size and relative sizes of layers and regions may be exaggerated for clarity. It will be understood that when an element is referred to as being "formed on," "disposed on" or "located on" another element, it can be directly on the other element or intervening elements may also be present. In contrast, when an element is referred to as being "directly formed on" or "directly disposed on" another element, there are no intervening elements present.
The technical features of the above embodiments can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the above embodiments are not described, however, as long as the combinations of the technical features are not contradictory, the scope of the present description should be considered as being described in the present specification.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. A method for repairing a conductive film, comprising the steps of:
providing a conductive film to be repaired, wherein the conductive film comprises a base film, a structural layer and a conductive grid, the structural layer is positioned on the base film, the structural layer is provided with a pattern groove, and the conductive grid is formed by filling a metal material in the pattern groove;
sensitizing the conductive film;
placing the sensitized conductive film in chemical copper plating solution;
adding reducing liquid under the condition of stirring;
and standing, and forming a deposited copper layer on the surface of the conductive grid, wherein the deposited copper layer also fills gaps with poor circuit in the conductive grid.
2. The method for repairing a conductive film according to claim 1, wherein the step of sensitizing the conductive film comprises spraying a sensitizing solution to a side of the conductive film on which the conductive mesh is provided, and washing the conductive film with pure water after spraying for 3 to 5 minutes; the sensitizing solution comprises stannous chloride with the mass fraction of 1% -5% and hydrogen chloride with the mass fraction of 4% -8%, and the PH value of the chemical copper plating solution is 10-12.
3. The method for repairing a conductive film according to claim 1, wherein the electroless copper plating solution comprises a main salt, a complexing agent, and a PH adjuster.
4. The method for repairing a conductive film according to claim 3, wherein the main salt is one or more selected from copper sulfate, copper chloride, and copper nitrate; the complexing agent is selected from one or more of potassium sodium tartrate, sodium citrate, EDTA disodium and triethanolamine; the pH regulator is selected from one or more of sodium hydroxide or potassium hydroxide.
5. The method for repairing a conductive film according to claim 4, wherein the electroless copper plating solution comprises 1.2 to 2 mass% of copper sulfate and 1.0 to 1.8 mass% of potassium sodium tartrate.
6. The method for repairing a conductive film according to claim 1, wherein the reducing solution comprises one or more of formaldehyde, hypophosphite, and dimethylamine borane.
7. The method for repairing a conductive film according to claim 1, wherein the step of adding the reducing solution under stirring is to stir the chemical copper plating solution, add a formaldehyde solution, and mix the solution to obtain a mixed chemical solution containing 1.0 to 1.8 mass% of formaldehyde.
8. The method for repairing a conductive film according to claim 1, wherein the metal material is one or more selected from the group consisting of silver, gold, a silver alloy, and a gold alloy.
9. The method for repairing a conductive film according to claim 1, wherein the leaving step is carried out at 30 to 60 ℃ for 10 to 120 min.
10. The method for repairing a conductive film according to claim 1, wherein in the step of leaving to stand, the thickness of the deposited copper layer is controlled to be 1 to 3 μm.
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| 阿孜古丽•吾拉木主编: "《科技与生活同行》", 31 March 2014, 北京出版社, pages: 39 * |
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