CN103617830A - A producing method of a metallic conductive film - Google Patents
A producing method of a metallic conductive film Download PDFInfo
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- CN103617830A CN103617830A CN201310513245.XA CN201310513245A CN103617830A CN 103617830 A CN103617830 A CN 103617830A CN 201310513245 A CN201310513245 A CN 201310513245A CN 103617830 A CN103617830 A CN 103617830A
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Abstract
The invention relates to the field of electronic material and discloses a producing method of a metallic film, and especially a producing method of a metallic conductive film. The producing method of a metallic conductive film is capable of increasing the adhesiveness between the metallic conductive film and a substrate and simultaneously maintaining the high conductivity and the long-term reliability of the metallic film. The producing method of a metallic conductive film comprises: S1, dissolving alginic acid and N substances containing basic groups in first solvent, wherein the N is an integer more than or equal to 1; S2, uniformly mixing dispersion liquid containing metal nano wires or dispersion liquid containing particles with the dissolved alginic acid and the N substances containing basic groups in order to obtain first solution; and S3, forming a film on the substrate with the first solution in order to obtain the metallic conductive film.
Description
Technical field
The present invention relates to field of electronic materials, particularly a kind of preparation method of conductive metal film.
Background technology
Nano silver wire transparent conductive film, has good electric conductivity, and in visible-range, has high transmission rate, is widely used in the fields such as flat panel display, thin-film solar cells, transducer, touch-screen and extending electronics.
But the adhesiveness of nano silver wire transparent conductive film and substrate is poor, when the adhesive tape that sticks to nano silver wire conductive film surface is uncovered, nano silver wire conductive film almost all can come off from substrate.At present, one of method that solves adhesion issues between nano silver wire conductive film and substrate is in the dispersion liquid of nano silver wire, to add the agent of polymer gluing, polymer gluing agent film forming together with nano silver wire, after solvent seasoning, the agent of polymer gluing is tightly sticked together nano silver wire and substrate.Another kind method is the nano silver wire surface coverage one layer of polymeric after film forming, and the method also can strengthen the adhesion between nano silver wire conductive film and substrate.But, because nano silver wire is peripheral, itself wrap up one deck stabilizer polyvinylpyrrolidone, in first method, the agent of polymer gluing is attached to behind nano silver wire periphery, silver line Contact resistance will sharply increase, in second method, owing to covering the polymer insulation of silver surface itself, also seriously reduced the conductivity of nano silver wire conductive film; Secondly, if realize large-scale commercial application, it will be very necessary and important that product keeps long-term reliability, therefore the physics and chemistry character for the polymer of the polymer gluing agent adding or covering has harsh requirement: certain film forming, inviscid after dry, be not easy the moisture absorption, can resist solvent, long-term stable existence in air is little etc. to Conductivity.Yet because of the needs of film-forming process, nano silver wire General Decentralized is in lower boiling ethanol or isopropyl alcohol, and the polymer gluing agent therefore adding must can be dispersed or dissolved in these solvents.But its ability of resisting solvent and wet environment of material that can be dissolved in picture ethanol or these polar solvents of isopropyl alcohol is often poor, the reliability of this polymer gluing agent is poor.Therefore, the reliability of its nano silver wire electrically conducting transparent laminated film of preparing is also poor.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of conductive metal film, can improve the adhesiveness between conductive metal film and substrate, and keep higher conductivity and long-term reliability simultaneously.
For solving the problems of the technologies described above, embodiments of the present invention provide a kind of preparation method of conductive metal film, comprise the following steps:
S1, the material by alginic acid and N kind containing basic group dissolve in the first solvent, and described N is more than or equal to 1 integer;
S2, the dispersion liquid that contains metal nanometer line or the dispersion liquid that contains particle are mixed with the material of N kind containing basic group with the described alginic acid of dissolving, obtain the first solution;
S3, by described the first solution film forming in substrate, dry, obtain conductive metal film.
Embodiment of the present invention in terms of existing technologies, utilize alginic acid and improve conductive metal film and substrate adhesion containing the material of basic group, wherein containing the substance of basic group, improve the dissolubility of alginic acid, alginic acid can be directly applied in the dispersion liquid of metal nanometer line or particle, make the technique of wet method film forming become possibility.Meanwhile, along with the volatilization of alkaline matter after film forming is removed, alginic acid dissolubility sharply declines, and makes it after film forming, possess outstanding opposing solvent and moist ability, has improved the long-term reliability of metal nanometer line conductive film.In addition, utilize its conductivity of transparent conductive film that this method obtains along with adhering raising, sharply not reduce.
In addition, when described N kind comprises Dopaminergics material containing the material of basic group, after described S1, before described S2, described method is further comprising the steps of:
S4, in being dissolved with described alginic acid and described N kind described the first solvent containing the material of basic group, add the poor solvent of alginic acid described in M kind, described M is more than or equal to 1 integer, and the addition of the poor solvent of described alginic acid is greater than the content of water in described the first solution;
The poor solvent of S5, described alginic acid is separated out the complex compound of described alginic acid and the formation of described Dopaminergics material, and the described alginic acid of described dissolving and N kind are the complex compound that described alginic acid and described Dopaminergics material form containing the material of basic group.
By adding the poor solvent of alginic acid, can separate out the complex compound that alginic acid and Dopaminergics material form.
Accompanying drawing explanation
Fig. 1 is preparation method's the schematic flow sheet of the conductive metal film of first embodiment of the invention;
Fig. 2 is preparation method's the schematic flow sheet of the conductive metal film of second embodiment of the invention;
Fig. 3 is structure of matter phenogram in technique;
Fig. 4 is the nano silver wire transparent conductive film under scanning electron microscopy;
Fig. 5 is the hot and humid reliability test result schematic diagram of nano silver wire transparent conductive film.
Embodiment
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with accompanying drawing, the embodiments of the present invention are explained in detail.Yet, persons of ordinary skill in the art may appreciate that in each execution mode of the present invention, in order to make reader understand the application better, many ins and outs have been proposed.But, even without these ins and outs and the many variations based on following execution mode and modification, also can realize each claim of the application technical scheme required for protection.
First embodiment of the invention provides a kind of preparation method of conductive metal film, as shown in Figure 1, comprises the following steps:
Alginic acid is the polysaccharide being formed by monose aldehydic acid linear polymerization, and monomer is β-D-sweet dew aldehydic acid (M) and α-L-guluronic acid (G).M and G unit are with M-M, and the compound mode of G-G or M-G is connected and is become block copolymer by Isosorbide-5-Nitrae glycosidic bond.The empirical formula of alginic acid is (C
6h
8o
6)
n, molecular weight ranges from 10,000 to 600,000 is not etc.The finished product of alginic acid is pale yellow powder, almost tasteless, insoluble in water, methyl alcohol, ethanol, acetone, chloroform, has good film forming, dry rear inviscid.The bad dissolubility of alginic acid makes it after film forming, possess outstanding opposing solvent and moist ability, be conducive to improve the long-term reliability of product, because containing a large amount of carboxyls in structure, while using as adhesive, its impact on metallic film conductivity is likely less simultaneously.
In example, the described material containing basic group can be ammoniacal liquor.In the first solvent, contain a certain amount of water and ethanol.At room temperature alginic acid, ammoniacal liquor, water and ethanol are mixed, obtain the clear solution of alginic acid.
The dispersion liquid that step 102, utilization contain metal nanometer line or the dispersion liquid that contains particle mix with the alginic acid of dissolving, obtain the first solution.
Example, what step 101 obtained is the clear solution of alginic acid, this solution is added to the dispersion liquid that contains metal nanometer line, obtains the first solution.In the first solution, the mass ratio of the clear solution of metal nanometer line or particle and alginic acid is to be more than or equal to 1 and be less than or equal to 100 number, preferably 5～20, and N is more than or equal to 1 integer.
Particularly, can first use the mode of spraying by the first solution film forming in PETG (PET) substrate, prepared film is carried out to performance characterization.In addition, can also utilize the mode of blade coating, printing or spin coating to the first solution film forming in substrate.Wherein substrate not being limited, can be the substrate of rigidity or flexible material, can be the substrate of organic or inorganic material, can also be the substrate of transparent or opaque material.
In addition, utilize spraying, blade coating, the mode of printing or spin coating is by the first solution in substrate during film forming, and technological temperature is controlled at below 100 degree.
Conductive metal film comprises nano silver wire transparent conductive film.
Embodiment of the present invention in terms of existing technologies, utilize alginic acid and improve conductive metal film and substrate adhesion containing the material of basic group, wherein containing the substance of basic group, improve the dissolubility of alginic acid, alginic acid can be directly applied in the dispersion liquid of metal nanometer line or particle, make the technique of wet method film forming become possibility.Meanwhile, along with the volatilization of alkaline matter after film forming is removed, alginic acid dissolubility sharply declines, and makes it after film forming, possess outstanding opposing solvent and moist ability, has improved the long-term reliability of metal nanometer line conductive film.In addition, utilize its conductivity of transparent conductive film that this method obtains along with adhering raising, sharply not reduce.
The second execution mode of the present invention relates to a kind of preparation method of conductive metal film.The second execution mode has been done further improvement on the first execution mode basis, as shown in Figure 2, main improvements are: when described N kind comprises Dopaminergics material containing the material of basic group, after step 101 is carried out, before step 102 carries out, first carry out following steps:
The poor solvent of step 105, alginic acid is separated out the complex compound of alginic acid and the formation of Dopaminergics material.
Example, the first solvent can be ammoniacal liquor.Step 101 is specially: at room temperature, in mass ratio for 8:1 takes alginic acid and Dopaminergics material, add ammoniacal liquor, alginic acid and Dopaminergics material are all dissolved.It should be noted that, Dopaminergics material is meeting polymerization reaction take place in ammoniacal liquor, generates poly-Dopaminergics material, and alginic acid and Dopaminergics material and poly-Dopaminergics material all complex reaction can occur, and generate the complex compound of alginic acid and poly-Dopaminergics material.
After execution of step 101, then perform step 104 and step 105.Step 104 and step 105 are mainly that the solution of the complex compound of alginic acid and poly-Dopaminergics material and ammoniacal liquor formation is carried out to separating-purifying, extract the complex compound of alginic acid and poly-Dopaminergics material.Present embodiment adopts the method for co-precipitation to extract the complex compound of alginic acid and the formation of poly-Dopaminergics material in the first solution.Concrete, step 104 comprises: the poor solvent that adds one or more alginic acids in the complex compound of alginic acid and poly-Dopaminergics material and the solution of ammoniacal liquor formation, the addition of the poor solvent of alginic acid is greater than the content of water in the first solution, the poor solvent of alginic acid can be organic solvent, as ethanol, isopropyl alcohol, acetone.Example, the poor solvent of alginic acid can be ethanol.Then perform step 105, step 105 comprises: after a few hours, when ethanol is separated out the complex compound of alginic acid and Dopaminergics material, adopt the complex compound of the separated alginic acid of centrifugal separation and poly-Dopaminergics material.For separated as far as possible thoroughly, can carry out in triplicate separation.It should be noted that, when separation, can artificially in the first solution, leave a small amount of ammoniacal liquor.
By adding the poor solvent of alginic acid, can separate out the complex compound that alginic acid and Dopaminergics material form.
Then perform step 102.Step 102 specifically comprises: the complex compound of the dispersion liquid that contains metal nanometer line or the dispersion liquid that contains particle and alginic acid and poly-Dopaminergics material is disperseed, obtain the first solution.When not moisture in dispersion liquid, first need to add a kind of solvent to dissolve the complex compound of alginic acid and poly-Dopaminergics material, this solvent is the solvent that contains water, and then utilize metal nanometer line or particle dispersion to mix with the complex solution of alginic acid and Dopaminergics material, obtain the second solution.The preferred low boiling point organic solvent of solvent adding in step 102, preferably low boiling point solvent is mainly the consideration of the technique based in step 103, because last film forming procedure is solvent will be removed, and the high boiling solvent seasoning time is long, in film forming, can affect because of the aggravation of solvent blockage effect the quality of film forming.Example, when the second solvent is ethanol, step 102 specifically comprises: the complex compound water of the alginic acid that first step 105 can be obtained and poly-Dopaminergics material and the mixed solvent of ethanol dissolve, and obtain complex compound solvent soln, wherein the about 1:1 of the mass ratio of water and ethanol; Then complex solution is joined in the dispersion liquid of metal nanometer line, obtain the first solution, wherein the mass ratio of metal nanometer line and alginic acid can be 8.While containing water in dispersion liquid, do not need to add solvent to dissolve the complex compound of alginic acid and poly-Dopaminergics material, can directly complex compound be dissolved in the dispersion liquid of metal nanometer line, obtain the first solution.
It should be noted that when step 105 is separated, residual ammoniacal liquor makes the second solution be alkalescent.Although final complex compound dissolubility is strengthened, or need certain alkalescence to guarantee its dissolubility in solvent.
Finally perform step 103.The manner of execution of step 103 is identical with the first execution mode, and therefore not to repeat here in the present invention.
Be below some experimental analysis data that the present invention does the conductive metal film preparing, wherein, Fig. 3 is to structure of matter phenogram in technique.Wherein, abscissa represents wave number, and unit is centimetre/mono-, and ordinate represents light transmittance, 301 performance characterizations that are alginic acid, and 302 performance characterizations for poly-Dopaminergics material, 303 is the performance characterization of alginic acid and poly-Dopaminergics material.Fig. 4 is the nano silver wire transparent conductive film under scanning electron microscopy, wherein scheming a is fine silver nano wire transparent conductive film, as seen from the figure, fine silver nano wire is piled up loose, and fine silver nano wire does not have bending, is straight substantially, figure b is for take the nano silver wire transparent conductive film that alginic acid is binding agent, nano silver wire is piled up tight ，Xian lap-joint and is out of shape as seen, and conductive effect can be better like this.Fig. 5 is the hot and humid reliability test result of nano silver wire transparent conductive film, and condition is 85 ℃ (degrees Celsius)/85%RH(relative humidity).Wherein, abscissa represents the reliability test time, and unit is sky, and ordinate represents sheet resistance, and unit is the every side of ohm.As seen from Figure 5, under hot and humid condition, nano silver wire transparent conductive film sheet resistance is without large variation.By every experiment, show, prepared metal nanometer line conductive film, sheet resistance during light transmittance 89% is 16.3 Ω/ (the every side of ohm).The sample that the sheet resistance value of take is 34.2 Ω/ carries out the test of adhesive tape adhesion, and its value is only increased to 42.4 Ω/, and after 100 adhesive tape adhesion tests, sheet resistance is still less than 100 Ω/, and the metal nanometer line that adhesion is purer significantly improves; Hot and humid experiment shows, the transparent conductive film of preparation possesses stable long-term reliability; Be placed in acetone or water a few hours, prepared conductive film still has adhesiveness, possesses good solvent resistance energy.
Embodiment of the present invention in terms of existing technologies, utilize alginic acid and improve conductive metal film and substrate adhesion containing the material of basic group, wherein containing the substance of basic group, improve the dissolubility of alginic acid, alginic acid can be directly applied in the dispersion liquid of metal nanometer line or particle, make the technique of wet method film forming become possibility.Meanwhile, along with the volatilization of alkaline matter after film forming is removed, alginic acid dissolubility sharply declines, and makes it after film forming, possess outstanding opposing solvent and moist ability, has improved the long-term reliability of metal nanometer line conductive film.In addition, utilize its conductivity of the transparent conductive film arriving of this method along with adhering raising, sharply not reduce.
Persons of ordinary skill in the art may appreciate that the respective embodiments described above are to realize specific embodiments of the invention, and in actual applications, can to it, do various changes in the form and details, and without departing from the spirit and scope of the present invention.
Claims (10)
1. a preparation method for conductive metal film, is characterized in that, comprises the following steps:
S1, the material by alginic acid and N kind containing basic group dissolve in the first solvent, and described N is more than or equal to 1 integer;
S2, the dispersion liquid that contains metal nanometer line or the dispersion liquid that contains particle are mixed with the material of N kind containing basic group with the described alginic acid of dissolving, obtain the first solution;
S3, by described the first solution film forming in substrate, dry, obtain conductive metal film.
2. the preparation method of conductive metal film according to claim 1, is characterized in that, when described N kind comprises Dopaminergics material containing the material of basic group, after described S1, before described S2, described method is further comprising the steps of:
S4, in being dissolved with described alginic acid and described N kind described the first solvent containing the material of basic group, add the poor solvent of alginic acid described in M kind, described M is more than or equal to 1 integer, and the addition of the poor solvent of described alginic acid is greater than the content of water in described the first solution;
The poor solvent of S5, described alginic acid is separated out the complex compound of described alginic acid and the formation of described Dopaminergics material, and the described alginic acid of described dissolving and N kind are the complex compound that described alginic acid and described Dopaminergics material form containing the material of basic group.
3. the preparation method of conductive metal film according to claim 1, is characterized in that, in described S1, the described material containing basic group contains amido, contains water or strong polar substances in described the first solvent.
4. the preparation method of conductive metal film according to claim 3, is characterized in that, the described material containing basic group is ammoniacal liquor or Dopaminergics material.
5. the preparation method of conductive metal film according to claim 2, is characterized in that, the poor solvent of described alginic acid is organic solvent.
6. the preparation method of conductive metal film according to claim 5, is characterized in that, described organic solvent is: ethanol, isopropyl alcohol, acetone.
7. the preparation method of conductive metal film according to claim 1, it is characterized in that, in described S2, the described alginic acid of described metal nanometer line or described particle and described dissolving and N kind are to be more than or equal to 1 and be less than or equal to 100 number containing the mass ratio of the material of basic group.
8. the preparation method of conductive metal film according to claim 1, is characterized in that, in described S3, utilizes the mode of spraying, blade coating, printing or spin coating by described the first solution film forming in substrate.
9. the preparation method of conductive metal film according to claim 8, is characterized in that, in described S3, utilizes spraying, blade coating, and the mode of printing or spin coating is by described the first solution in substrate during film forming, and technological temperature is controlled at below 100 degree.
10. the preparation method of conductive metal film according to claim 1, is characterized in that, in described S3, described substrate is transparent, translucent or opaque flexibility or rigidity material.
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| CN104934094A (en) * | 2015-05-27 | 2015-09-23 | 复旦大学 | Metal nanowire composite transparent conductive film, preparation method and application thereof |
| CN105602201A (en) * | 2016-03-21 | 2016-05-25 | 西南科技大学 | Preparation method of high-strength conductive polymer nanocomposite |
| CN107154283A (en) * | 2017-04-11 | 2017-09-12 | 复旦大学 | The nano silver wire of resistance to electromigration laminated film and preparation method thereof |
| CN108892811A (en) * | 2018-06-21 | 2018-11-27 | 中国科学技术大学 | A kind of inorganic wire material-organic polymer composite material and preparation method thereof |
| CN109438139A (en) * | 2018-11-09 | 2019-03-08 | 中国农业科学院农业资源与农业区划研究所 | A kind of preparation method with the alginic acid synergistic carrier for slowing down urea conversion |
| WO2019109453A1 (en) * | 2017-12-06 | 2019-06-13 | 武汉华星光电半导体显示技术有限公司 | Nano-silver wire transparent conducting film and preparation method therefor, and touch screen |
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| CN104804206A (en) * | 2015-04-28 | 2015-07-29 | 中科院广州化学有限公司南雄材料生产基地 | Method for preparing transparent conducting thin film based on silver nanowire modification |
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| US10664077B2 (en) | 2017-12-06 | 2020-05-26 | Wuhan China Optoelectronics Semiconductor Display Technology Co., Ltd. | AgNW transparent conductive film and manufacturing method thereof and touch panel |
| CN108892811A (en) * | 2018-06-21 | 2018-11-27 | 中国科学技术大学 | A kind of inorganic wire material-organic polymer composite material and preparation method thereof |
| CN108892811B (en) * | 2018-06-21 | 2020-02-07 | 中国科学技术大学 | Inorganic material-organic polymer composite material and preparation method thereof |
| CN109438139A (en) * | 2018-11-09 | 2019-03-08 | 中国农业科学院农业资源与农业区划研究所 | A kind of preparation method with the alginic acid synergistic carrier for slowing down urea conversion |
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